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HUTNICTWO, GÓRNICTWO ›
INŻYNIERIA MATERIAŁOWA › 2010-3
 

Publikacja: Properties of WE-43 magnesium alloy in high-temperature brittle range
Autor: Janusz Adamiec  

Crystallisation of the alloys, both during casting and during welding occurs always in some temperature range, called crystallisation range. The nuclei of crystallisation appear during lowering the temperature below liquidus temperature. In a pool of liquid metal the nucleuses form in partially melted crystallites and grow usually to the form of column crystals or dendritic crystals. In a certain moment of crystallisation the crystals begin to interact between each other as long as they form skeleton of continuous solid phase. Temperature in which the crystals begin to interact between each other is called the coherence temperature and the temperature when the network of solid body starts to form - rigidity temperature. Below this temperature the semi-solid body starts to possess the characteristics of solid phase, which means that it preserves the shape and possesses the mechanical properties - the resistance and ductility [1, 2÷4]. Partial tears of the structure and hot cracks of the casts and welded and padded joints are the final effect of the high-temperature brittleness phenomenon. They should be treated as irreversible failures formed in the crystallisation process, which is in the range of liquid and solid phase coexistence [1]. Hot cracks are of intercrystalline character and the main reason of their formulation is the decrease in metal plasticity in certain temperature range, called the brittle temperature range (BTR) and the strain, under the influence of which it is going to be in this particular time range. The decrease in metal ductility may be caused by the decrease in resistance of the crystalline boundaries areas, as a result of presence of liquid film or accumulation of a big amount of defects of crystal lattice in those areas. Liquid phase may appear in the last phase of solidification or as a result of partial melting of the areas of crystalline boundaries during metal heating in solid stage [3]. There are [...]

 

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POZOSTAŁE PUBLIKACJE W TYM ZESZYCIE:
(Ti, Al)N films on Ti-6Al-4V titanium alloy produced by means of vacuum arc method
 
Piotr Wieciński  Jerz y Smolik  Halina Garbacz  Hideyuki Murakami  Krz ysztof j. Kurzydłowski  
Surface engineering methods are effective way to meet the increasing demands of industry. The needs of increasing efficiency and life time of the mechanical components lead to looking for a coatings which are resist to degradation in severe environments and endurance of extremely high thermomechanical loads [1]. In recent years, the development of several industrial branches was determined by the potential of surface engineering, especially of plasma deposition methods of thin coatings [2÷4]. (Ti, Al)N coating is an example of thin PVD coatings which are known for more then 10 years. Due to their high hardness, superior resistance to abrasive and chemical wear, (Ti, Al)N coatings considerably improve the life time of the cutting and drilling tools and allow to applied higher working velocities [5÷7]. Additionally, they exhibit excellent oxidation resistance, at temperatures higher than 850°C, due to dense alumina layer which is formed on the surface [8÷10]. (Ti, Al)N phase has B1-NaCl structure, the same as for TiN phase. Since Al atoms are smaller than Ti, substitution of Ti atoms with Al atoms results in gradually decreases of TiN lattice parameters [10] and appearance of the distortions and residual stresses in crystallographic structure [11]. The hardness of the (Ti, Al)N strongly depends on the aluminium content in the coating. The hardness and Young modulus increase, with increasing aluminium content in the film up to 60÷70%. However, beyond this value mechanical properties of the coating decreases due to formation of hexagonal wurtzite phase, which is typical for AlN. According to he authors of [12, 13], (Ti, Al)N film has B1-NaCl structure when the aluminium content is below 70%. One of the PVD technique which is used for deposition of (Ti, Al)N coatings is vacuum arc method. The main advantages of this method are: high level of ionizations of the target, presence of multiple ions, high kinetic energy of ions and high [...]
 
A method for evaluation of the size of a grain on non-planar surfaces
 
JERZY CHMIELA  DAMIA N SŁOTA  JAN CWAJNA  STANIS ŁAW ROSKOSZ  
In the stereological methods [1÷3], applied to describe the grain size of polycrystalline materials, images of metallographic specimens or images of plane sections of three-dimensional model structures are used. Frequently, it becomes necessary to evaluate the grain size in finished components, for which, due to their manufacturing technology, it is impossible to make microsections without destroying the component. In such cases, the possibility to evaluate the size of grain on a non-planar surface would be an effective solution. However, the reference publications do not provide any information in this respect, while there is an urgent need for such, i.e. study in order to improve the quality control of many parts, including turbine blades produced by investment casting. PHASES OF EVALUATION OF THE GRAIN SIZE ON A NON-PLANAR SURFACE Evaluation of the grain size on a non-planar surface is a multiphase task. In the first place, the grain boundaries must be detected. This is combined with photographic documentation, including an image of orthogonal projection of a non-planar surface. Based on the image of the projection, a quantitative analysis of the structure is performed in order to determine the necessary stereological parameters and coordinates of grain boundaries points. The values of stereological parameters obtained by measuring serve as reference values for the evaluation of the grain size on a non-planar surface obtained through approximation of geometric measurements of the real surface area of the investigated component. The coordinates of grain boundaries, determined in the orthogonal projection image, provide a foundation for mapping the image of the structure on an analytical non-planar surface and for calculating stereological parameters. A detailed discussion of the particular phases of evaluation of the grain size on a non-planar surface was based on an example of a test component presented in Figure 1. The su[...]
 
A note on the kink bands in compressed Ni2MnGa single crystals
 
Maciej J. Szczerba  Bogusław Major  Marek S. Szczerba  
In the last decade Ni-Mn-Ga single crystals had been a subject of intense structural and magnetic studies, because of their enormous magnetic shape memory effect (MSM), which is observed when the alloy possesses a tetragonal or orthorhombic crystal structure [1÷3]. Large interest has been paid to the Curie temperature and to the critical temperature of martensitic transformation, where upon cooling the high temperature cubic phase is replaced by the tetragonal (orthorhombic) structure [4, 5]. Recently, there has been focused a greater interest on the mechanical properties of the Ni2MnGa type alloys of cubic phase, because of their capability to adopt large plastic strains at high temperatures [6, 7] and hence the effect of the plastic deformation on the degree of deprivation of the MSM is also studied [8]. In this context, studies of the brittle-ductile transition which is observed in the cubic Ni2MnGa single crystals at elevated temperatures are of particular significance. However, as it was very recently reported in [9], Ni-Mn-Ga single crystals of both of the cubic and tetragonal structure, subjected to the room temperature compression are still capable to accommodate locally small plastic strains, before they fracture at the strength level of about 1 GPa. It seems important to make a proposal that the brittle-ductile transition in these alloys may be strongly correlated with temperature stability of the mechanism responsible for the accommodation of these small plastic strains. In this work, deformation geometry of the discussed accommodation mechanism will be shown in detail. Basing on the experimental observations of the Ni2MnGa single crystals compressed at 475 K it will be shown that the accommodation mechanism consists of a successive nucleation and further propagation of the kink bands and it is strongly correlated with the appearance of the mechanical instabilities on the stress-strain curve. The analysis presented i[...]
 
AgSnBi consolidated by cyclic extrusion compression
 
Maria Richert  Jan Richert  Agnieszka Hotloś  Beata Leszczyńska-Madej  Marcin Maślanka  Marcin Mroczkowski  
Electrical contact materials are used in a variety of applications, such as electrical switches, contractors, circuit breakers, voltage regulators, arcing tips, switch gears and relays. Contact performance typically regards the three major functions of the switch and their respective set of dependent variables. During contact operation, a low tendency for contact welding and a low erosion rate are required. The toxic nature of lead and the increasing awareness of its adverse effect on environment and health have led to the development of lead-free alloys in recent years. A candidate lead-free electric contact alloys must fulfill some requirements: suitable melting temperature and solidification behavior, good wettability, excellent mechanical properties and very good conductivity, resistance against wear [1÷3]. The Ag-Bi-Sn alloy is a promising lead-free alloy because it is superior to other candidates with respect to melting, wettability and mechanical properties [4, 5]. Internal oxidation of Ag-Sn alloy is important to prepare Ag-SnO2 electrical contact materials [6]. This process of reaction diffusion of Ag-Sn-Cu consists of a few stages. It mainly includes three stages: the first process is the adsorption and decomposition of oxygen at the surface; the second one is oxidizing reaction to form SnO2 particles and oxide band; the third one is diffusion of Cu and CuO formation. Being pollution-free, silver tin oxide (Ag/SnO2) has been used to replace toxic Ag/CdO contact materials in last two decades. In terms of replacing cancerous Ag-CdO, as well as reducing material and process cost, an attempt has been made to synthesize Ag-Sn-Bi tertiary system as a new way of production of materials for the electric contacts [3÷5]. The purpose of this paper is to investigate hardness and microstructure of Ag-Sn-Bi contact material fabricated by powder metallurgy and then consolidation by special Cyclic Extrusion Compression method [7]. [...]
 
Al effect on the transport properties of nickel oxide – influence on nickel oxidation
 
Nacer Halem  Jan Kusiński  MARIO ARA ABRUDE ANU  Georgette Petot-Ervas  
Although the oxidation of dilute Ni-Al (or Cr) alloys have received considerable attention [1÷9], gaps in the understanding of the oxidation mechanism are apparent, mainly at T > 900°C. One can recall that under ideal conditions, a compact Ni1-xO scale grows, according to a parabolic law, and it is generally assumed that the rate controlling factor is the outward diffusion of Ni2+ by a vacancy mechanism. In the present investigation, we have studied the oxidation kinetic of Ni and dilute Ni-Al (0.5 wt. %) alloys and we have compared the results to those of similar studies performed in the past, with dilute Al-Ni alloys. The data were analyzed taking into account, both the transport processes in pure and Al-doped Ni1-xO samples and a fundamental analysis of transport processes through the oxidation layer. Transport properties IN TR ANSITION MET AL OXIDES These oxides are p-type semiconductors [10÷19]. The prevailing defects are cationic vacancies (V&#945;&#697;) with an effective mean charge -&#945;. Their formation can be described by the following equation: &#189;O2 <=> OO + V&#945;&#697; + &#945;h- (1) If KV = [h-]&#945;[V&#945;&#697;]/(PO2)1/2 = exp(-&#916;GV/RT) (2) is the equilibrium constant of Eq. 1, then it follows from the electroneutrality condition that in the undoped oxide: [h-] = &#945;[V&#945;&#697;] = AKV 1/(&#945;+1) (PO2)1/2(&#945;+1) (3) where OO is an oxygen ion in a normal site, h- an electron hole, &#916;GV (= &#916;HV - T&#916;SV = -RT lnKV) the standard free enthalpy of formation of one mole of cationic vacancy, A = &#945;1/(&#945;+1) and the square brackets indicate molar fractions. Electrical conductivity of undoped and Al (0.11 at. %)-doped Ni1-xO single crystals The electrical conductivity (&#963;) of p-type semiconducting oxides in equilibrium with the surrounding atmosphere is controlled by the hole concentration (Eqs. 2, 3): &#963; = &#963;0 exp(-&#916;H&#963;/RT) = e &#956; p (4) where e is [...]
 
Al/SiC composites produced by direct extrusion using the KOBO method
 
Jarosław Woźniak  Marek Kostecki  Włodzimierz Bochniak  Andrzej Olszyna  
The constantly increasing interest in metal-ceramic composites has been inspired by the unique properties of these materials. Their high strength properties, good wear resistance, ability to work at elevated temperatures, and low density make them very attractive for the automobile, spacecraft, aircraft and electronic industries. The amount of these composites used in the industry increased from 3.6×103 tons in 2005 to 4.9×103 tons in 2010 [1, 2]. The Al/SiC composites are increasingly used in the automobile industry for manufacturing the components of car engines. Thanks to their advantageous properties, the Al/SiC composites supersede aluminum and its alloys. They are used for the manufacture of pistons, connecting-rods, and brake plates. The methods, most often reported in the literature, employed for producing rods of Al/SiC composites are the extrusion techniques. In these methods, the material prepared for the extrusion process is a mixture of appropriate powders, which is consolidated or capsuled. The consolidation is performed using various techniques such as e.g. hot-pressing or melt-pressing [3÷5]. A method which permits avoiding the hot-pressing or sintering operations is the KOBO method, in which a solid material or a powder mixture is extruded in a press with a reversely rotating die. Thanks to the rotation of the die, the deformation path of the material varies during the process. The KOBO method is particularly advantageous since it permits reducing the extrusion forces necessary for the composite material to be fully consolidated [6, 7]. Experimental The matrix material for the Al/SiC was prepared from a commercial Al powder with a purity of 99.7% and an average particle size of 6.74 &#956;m (delivered by the Bend-Lutz Co). The reinforcing phase was made of a SiC powder with a purity of 99.8% and an average particle size of 0.42 &#956;m (Alfa Aesar Co). The size of the particles of the powders was selected so[...]
 
Analysis of the possibilities of increasing resistance to plastic deformation of new biopolymers by means of modification through radiation
 
JERZY CYBO  JOANNA MASZYBROCKA  JERZY KANSY  ADRIAN BARYLSKI  
Operational durability of the polymer-metal kinematic systems used in technology and endoprosthesoplasty depends to a considerable degree on the resistance of polyethylene to plastic deformation and wear [1÷6]. In about 90% of applications, conventional and the cheapest polymer-metal couples are still used in alloplastic procedures. In one of such cases, a ca. fivefold reduction of susceptibility to permanent deformation and tribological wear was obtained for the polyethylene Chirulen 1120. The effect was a result of a combined application of small plastic deformation (ef. &#8776; 0.2, initiating the transitions) and electron beam irradiation [7÷9]. Those factors modified the morphology of the polymer. As a result, in operational conditions, the thickness of the deformed upper layer of polyethylene reduced, its degree of crystallinity and reorientation of the lamellar phase were modified, the degree of structure order increased, and in consequence, the operational durability improved. The reference literature of the last decade shows, however, that in order to increase resistance to wear and ageing, what should be aimed at is to ensure a very high molecular weight and an appropriate proportion of crystalline and amorphous phases [10÷13]. In the shaping of the properties, a more and more significant role of irradiation with an electron beam is being recognized. Doses higher than 25 kGy are conducive to decomposition of long macrochains, spatial arrangement of the structure and UHMWPE crosslinking. A growing dose, to as much as 150 kGy, causes a very significant increase of resistance to wear [14, 15]. According to the presented information from the reference literature, two grades of polyethylene have been recently introduced to production. Polymers GUR 1020 and GUR 1050 have replaced Chirulen 1120 of a molecular weight of ca. 106 g/mole. New materials weigh many times more: 5&#183;106 and 9.2&#183;106 g/mole, and are intended e[...]
 
Analysis of the stress distribution in the nanogrid coatings based on digital representation of the structure
 
KONRA D PERZYŃSKI  ŁUKASZ MAJOR  MAGDALENA KOPERNIK  Łukasz MADEJ  MACIEJ Pietrzyk  
The multilayered coatings have various demanding applications, were reliability of the product is crucial. The artificial heart chamber and its constructional elements, e.g. the aortic valves, is one of such examples. The tribology rules used in the deposition of coatings on the substrates are relatively simple. The goal is to obtain as many coating layers as possible. In the standard deposition process the first coating is hard, the second is soft, and they repeat periodically. But this approach is not sufficient and cannot be adapted for specific applications, such as the heart chamber. In that case the outer coating has to be biocompatible and permanent natural tissuecoating connection has to be created. The shape of the chamber and its elements is quite complicated and many crucial points with the stress concentration occur. On the other hand, the material of the chamber cannot be deformed irreversibly. Thus, the requirements for the substrate-coating-tissue system are strict and the standard modeling methods of the multicoating system, which represents the flat boundaries between subsequent coatings, should not be used. It is due to the fact that the capabilities of these methods to correctly predict the fatigue and cracking phenomena of the analyzed specimens are not sufficient. The example of a multilayered specimen with the flat boundaries is presented in Figure 1. In reality the boundaries between coatings have irregular shapes. New numerical models, that can correctly describe the geometry of the boundaries among layers, have to be developed to account for these irregularities. Application of the digital material representation is one of the possible solutions [1, 2]. DIGITAL REPRESENTATION OF THE NANOGRIDS MATERIALS Various methods can be used to deposit the nanogrid materials [3]. Development of a correct numerical model to support the expe[...]
 
Analysis of titanium sheet bending process
 
Janina Adamus  Piotr lacki  Maciej Motyka  ZYGMUNT NITKIEWICZ  
Titanium and its alloys are exceptional structural materials, far outstripping other in many aspects. Thanks to low specific gravity and high mechanical strength titanium materials are used whenever the construction weight and its strength are essential, e.g. in the aircraft and aerospace industries, for sporting equipment and in medicine [1, 2]. Furthermore, the value of the elastic modulus of titanium alloys is approximately half the corresponding value for steel. Thus, titanium alloys are excellent materials for various types of springs [3, 4]. Good corrosion resistance in most corrosive environments warrant the application of titanium elements in chemical and marine industries, desalination and desulfurization systems, in sewage treatment plants, geothermal systems etc. Apart from technical applications titanium and its alloys are often used in medicine and jewellery because of a good biocompability. Titanium as a material with the unique mechanical and physical properties is used whenever common structural materials such as aluminium and steel fail. Unfortunately, the application of titanium and its alloys is difficult because of high production and processing costs and the fact that titanium alloys fall into group of materials which hardly deform, especially in sheet-metal forming processes. During the forming of titanium sheets it is necessary to overcome many technological barriers, which are not reflected in the technical literature. Bending is one of the most commonly used forming methods of the titanium elements. It comes down to a stable change in material curvature by bending or straightening. Bending can be done on press brakes or stamping presses using bending tools, as a roll bending, roll form profiling etc. During bending of the titanium elements it is necessary to take the following into consideration: -- titanium, especially its alloys, is characterized by [...]
 
Anisotropy of Portevin-Le Chatelier effect in Al-Mg-Mn sheet alloy described by acoustic emission
 
Joanna Zdunek  Jan Powiec  Ja rosław Mizera  Wojciech l. Spychalski  Krzy sztof j. Kurzydłowski  
The Portevin-Le Chatelier (PLC) effect which was found to occur in many metal alloys, in particular in aluminium alloys, during tensile testing at certain temperature range is typical of plastic deformation instability. It appears as a serration on the stress-strain curves. Traditionally the PLC bands are examined by indirect methods, for example by using an extensometer or a strain gauge [1, 2]. The PLC effect is basically understood to be a material property since it is primary known to arise from the underlying microstructural processes that govern the plastic deformation kinetics of metallic solids solution, such as the dynamic interaction between the gliding dislocations and the mobile solute atoms [3]. There have also been reports which analyze the PLC effect in terms of microbanding [4], planar slip [5], test temperature, strain rate and grain size [6, 7]. Aluminium alloys are known to exhibit an anisotropy of mechanical properties usually correlated with the crystallographic texture. Cheng and Morris [7] reported on the relation between the occurrence of the PLC effect and the anisotropy of mechanical properties in the Al-Mg alloy. They attributed the intensi[...]
 
Application of EFTEM and FIB electron tomography to 3D visualization and metrology of nanoparticles in Inconel 718 superalloy
 
Adam KRUK  GRZEGORZ CEMPURA  BEATA DUBIEL  Aleksandra Czyrska-Filemonowicz  
Inconel 718 (IN718) is one of the most common precipitation-hardened Ni-base superalloys. It belongs to a class of Ni-Fe superalloys, containing a relatively high content of Fe as well as Ti and Al to provide &#947;&#8242;, Ni3(Ti, Al) precipitates. It also contains Nb which leads to precipitation of the tetragonal Ni3Nb phase (&#947;") [1]. A disadvantage is that the &#947;" precipitates have a worse thermal stability than &#947;&#8242; leading to a faster coarsening rate and to a gradual transformation to an orthorhombic phase of Ni3Nb (&#948;) above about 800°C. This limits the use of the alloy to below about 650°C. The &#947;" phase occurs in the form of as elongated, oriented particles (disc-shaped) within the &#947; matrix, while the &#947;&#8242; precipitates are spherical [1, 2]. Transmission electron microscopy (TEM) images give valuable information about the microstructure and chemical composition of materials. However, they &#8220;only" provide a 2D projection of a 3D object. Electron tomography was developed to reconstruct objects in three dimensions (3D) from a tilt series of TEM images. This technique is well accepted in the life sciences as a method used to study viruses or cells. The resolution in the reconstructions, however, is limited to a few nanometers. Electron tomography techniques have recently been adopted by researchers in materials science [2]. In practice, however, the resolution is still of the order of one to two nanometers because of the limited stability of the sample holders and the presence of dynamic diffraction in crystalline solids. Electron tomography is a technique that uses a transmission electron microscope (TEM) to determine a 3D structure from any given asymmetric object [3]. This process can be simply broken down into 4 steps. First, a series of 2D projection images of the specimen are recorded and systematically tilted to different angles in the microscope. Second, these individual im[...]
 
Ball milling amorphization and consolidation of NiTiZrNb and NiNbTiZrCoCu alloys
 
Jan Dutkiewicz  Lidia Lityńska-Dobrzyńska  Wojciech Maziarz  Tomasz Czeppe  Anna Góral  Justyna Grzonka  
Amorphous nickel rich alloys have been obtained in recent years by rapid quenching from the liquid state or by mechanical alloying in a planetary mill [1÷9]. One advantage of the latter method is that it makes it possible to obtain new materials from powders of different elements, which are immiscible in the liquid state. Binary NiTi alloys subjected to ball milling or severe plastic deformation can be obtained amorphous [1÷3]. The tendency to form an amorphous structure depends on the relative values of the deformation temperature and martensite start (Ms) temperature. Lowering of the deformation temperature in the range below the martensite finish temperature facilitates amorphization [3]. Mechanical alloying of Ni60Nb20Zr20 alloy [4] involves two consecutive amorphization reactions, leading first to the amorphization reaction between Ni and Zr layers and on further milling consequently a Ni-Nb amorphous phase forms. The resulting two amorphous phases homogenize at longer milling times. Multicomponent nickel base alloys can be obtained as bulk glass at composition of Ni50Co10Nb20Ti10Zr10 (at. %) alloys with reported large supercooled liquid region of more than 40 K formed by copper-mold casting. The alloys with 5 and 10 at. % cobalt possess the highest glass-forming ability [5]. Mechanically alloyed Ni57Zr20Ti18Al5 alloy powders synthesized by high-energy ball milling have shown a complete amorphization after 5 h of milling, even broader supercooled region of 56°C and crystallization temperature above 500°C [6]. Substitution of aluminum by silicon [7] also allowed to obtain amorphous Ni57Zr20Ti20Si3 powders by mechanical alloying of pure Ni, Zr, Ti, Si, and ceramic powder mixture; the metallic alloy amorphized after 5 hours milling indicating a good glass forming ability. In [8] Amorphous Ni59Zr20Ti16Sn5 alloys were fabricated by melt spinning and by mechanical alloying (MA) techniques. Differences in crystallization temperat[...]
 
Blood permeability testing of chitosan sealed polyester vascular prosthesis
 
MACIEJ GAWLIKOWSKI  KAROLINA GORKA  ROMAN KUSTOSZ  ADAM JAROSZ  ANTONI NIEKRASZEWICZ  MAGDALENA KUCHARSKA  
The aim of the investigation was to determine blood permeability through the vascular grafts sealed with chitosan. The measurement method of water permeability of vascular grafts is specified in appropriate standard [1]. However the standard&#8217;s procedure does not reflect real prosthesis&#8217; work conditions, particularly when it is applied as an element of heart assist system [2]. In respect of this it was intended to perform testing according to distinct procedure giving more complete representation of vascular prosthesis&#8217; properties and taking into consideration mechanical extensibility of woven fabric during work with pulsatile pressure load. MATERIALS AND METHODS Vascular grafts The material of the investigation were BARD 004187 style 6010 vascular prosthesis of 16mm internal diameter [3]. Graft samples marked as 10 and 20 were sealed with layers based on chitosan. &#8220;10" and &#8220;20" runs was sealed with material of relative molecular mass respectively about 130 kD and 100 kD. Reference samples, marked as 0REF were not modified in any way. For testing purposes sample sets together with mounting elements and soft ring seals were prepared (Fig. 1). In such a set active graft&#8217;s length (intended for contact with blood) was 70 mm and active graft&#8217;s wall area was 35 cm2. Operating medium As an operating medium the blood collected from animals with CPDA-1 [4] anticoagulant was used. Transport of biological material to the laboratory was performed in temperature of 10°C. Time elapsed from blood collecting to beginning of the investigation was about 1.5 h. Biological material&#8217;s stability was determined by biochemical tests (hematocrit level, degree of hemolysis) [5] on the spot of drawing, directly before and during investigation. Testing methodology Vascular prosthesis&#8217; samples were divided in three groups: a, b and c. In "a" group the grafts were subjected to the test without prelimin[...]
 
Capabilities of Al2O3 nanolayer formation on carbon fibers by CVD method
 
ANITA OLSZÓWKA-MYALSKA  AGNIESZKA BOTOR-PROBIERZ  
Carbon fibers are characterized as materials with low oxidation resistance in an oxidative environment and chemical reactivity limits their application in metal-matrix composites. To widen the application of carbon fibers in a metal composite some form of coating is needed which may improve their oxidation resistance at high temperatures and to give the possibility of the fiber/matrix interfacial reaction control [1÷4]. In fact, several techniques such as chemical vapor deposition (CVD), physical vapor deposition (PVD), the solgel method and other modern techniques can be used to provide coating for carbon fibers. Alumina coating in comparison with other coatings seems to be very attractive, simply because of the low precursor material price. The most frequent technique used to obtain oxide coatings like alumina, silica, zirconia and titania is the sol-gel method. In the case of an organometallic solution application, fibers are passed through a solution and the coating is formed by hydrolysis of the organometallic compounds. The oxide coating homogeneity and thickness can be controlled by the appropriate selection of the solution concentration, immersion time and temperature [1, 3÷7]. Alumina coatings obtained on the carbon fibers by sol-gel method only partially prevent the oxidation of carbon because of the presence of pores [3]. However some authors [6] report that the porous alumina coatings obtained on fibers by sol-gel act not only as diffusion barriers (improving the oxidation resistance of carbon fiber and preventing harmful CF/Al interfacial reactions), but also promote wettability and relieve thermal stress concentration between the carbon fibers and the aluminum matrix. The other technique used to obtain thin al[...]
 
Catalytic activity of Ni3Al foils in decomposition of selected chemical compounds
 
Paweł Jóźwik  Zbigniew Bojar  Piotr Winiarek  
Alloys based on the Ni3Al intermetallic phase, as compared to competitive group of nickel-based superalloys, exhibit high strength for high deformation velocity at elevated temperature, high resistance to oxidation and carburization at elevated temperature, and much better fatigue strength (they crack more slowly than other intermetallic phase-based alloys). However, common application of these alloys meets, quite a few technological drawbacks mainly related to insufficient plasticity and a tendency to brittle cracking [1, 2]. Additionally, Ni3Al-based alloys can be used in the form of honeycomb structures, which have an advantage in lightweight, highstiffness and high-strength over bulk Ni-based superalloys. Thus far, we have successfully fabricated Ni3Al thin foils by cold rolling of commonly casted ingots without any additional treatment. The proposed technology allows to obtain foils with thickness even below 50 &#956;m and with micro- and nanograined structure [3, 4]. Methanol is expected to become an alternative energy source (a fuel) in the near future. It can be easily synthesized from biomass, natural gas, coal etc., which are more abundant resources than crude oil [8, 9]. Hexane, as the second analyzed compound in this field of research, is a component of many products related to the petroleum and gasoline industries. Nevertheless, as an effect of these applications, increasing amount of this compound is released to the atmosphere and possibility of hexane deactivations is important for environmental pollution reducing. Above mentioned mechanical properties of Ni3Al thin foils, and their additional good catalytic properties without any coating, allow to build microscale power sources and microreactors for air purification (e.g. MEMS, MECS) [3, 4]. The main purpose of this work was an assessment of catalytic effects observed while thermodecomposition reactions of methanol and hexane run over Ni3Al foil surface. Preli[...]
 
Catalytic behaviours and electrical conduction changes in BaCeO3 ceramics synthesized by sol-gel method
 
ARAB MADJID  Franciso Wendell B. Lopez  Carlson Pereira de Souza  Agnieszka Kopia  Bakiz Bahcine  JEAN RAYMOND GAVARRI  
BaCeO3 (BCO) ceramics and related perovskite type compounds were intensively studied because of their high temperature potential applications (e.g. for fuel cell and electrocatalysis technologies) [1÷3]. They were regarded as very promising candidates as solid electrolytes in electrochemical devices such as solid oxide fuel cells (SOFCs) and gas sensors [4÷6]. These perovskite type structures were highly interesting mainly because of their high ionic conductivity. More recently, we found that BaCeO3 exhibited heterogeneous photocatalytic activities for water splitting [7÷10]. Doped barium cerate materials were also investigated as proton conductors in humidified reducing atmosphere at intermediate temperature: these perovskite type materials were also considered as promising electrolytes for SOFCs [11÷14]. The microstructure and the presence of carbon dioxide in the ambient atmosphere were also considered as potential parameters that could condition the conductivity mechanisms [15]. These oxide materials were also found to present high interest as catalysts for oxidation reaction because of their high capacity of oxygen conduction. Recently solid gas interaction analyses between BCO and methane CH4 in air-CH4 flows were published [16, 17]. However, in our knowledge, the solid gas interactions between BaCeO3 and carbon monoxide CO were never studied. In this work, we first study the conversion of CO in air-CO gas mixtures interacting with barium cerate powder, and then we determine the high temperature electrical conductivity of compacted pellets of barium cerate. We report a new synthesis method allowing preparing BaCeO3 perovskite ceramics at moderate temperature (1100°C). Characterizations are achieved using X-ray diffraction and transmission electron microscopy. The catalytic properties are investigated from analyses of emitted gases from Fourier Transform infrared spectroscopy (FTIR). The electrical properties are studied [...]
 
Characterisation of nanocomposite nc-WC/a-C and nc-WC/a-C:H coatings on oxygen hardened Ti-6Al-4V alloy
 
TOMASZ MOSKALEWICZ  BOGDAN WENDLER  Aleksandra Czyrska -Filemonowicz  
Titanium and its alloys are often applied in aeronautics, chemical, petrochemical, marine industries and medicine as structure materials due to their high specific strength and excellent corrosion resistance [1, 2]. However, titanium alloys are characterized by poor tribological properties especially in sliding situations. These include high and unstable friction coefficients, severe adhesive wear, susceptibility to fretting wear and a strong tendency to gall when in rubbing contact with itself and other surface [3]. Deposition of a low friction and wear resistant coatings by different surface engineering methods is one of the most prospective means to improve the tribological properties of the titanium alloys. Nanocomposite coatings were found to be a prospective for improvement of tribological properties of materials. Hard and soft phase were often mixed in order to get a compromise between mechanical and tribological properties [4]. In this field, many nanocrystalline metal carbide particles (nc-MeC, where Me = transition metal) have been used as a hard phase and amorphous carbon, hydrogen-free (a-C) or hydrogenated (a-C:H) have been used as a second phase [4÷8]. Carbon-based nanocomposites, where nanocrystalline phase is embedded into a-C matrix, are considered as a new class of protective material and found wide range of engineering applications, such as cutting and machining tools, bearing, pumps, machine and engine parts [9, 10]. These coatings exhibited high hardness, toughness, good wear resistance and very low friction in ambient air due to the lubricious a-C matrix [11÷13]. However, when such coatings are deposited on &#8216;soft&#8217; substrates, like commercially pure titanium or Ti-6Al-4V alloy, when the applied load is high enough the softer substrate can undergo plastic deformation [14]. Therefore, in a present study nanocomposite coatings were deposited on a &#8216;hard&#8217; substrate - oxygen hardened Ti-[...]
 
Characteristics of surface layers produced on austenitic-ferritic stainless steel by low temperature glow discharge nitriding
 
Bartosz Gołębiowski  Tadeusz Zakroczymski  Robert Sobiecki  Wiesław Świątnicki  
Austenitic-ferritic stainless steels are characterized by high strength, better than those of standard austenitic stainless steels, good ductility, high resistance to stress corrosion, low thermal expansion and good weldability. Moreover, thanks to the presence of austenite which is resistant to hydrogen corrosion [1], the resistance to the hydrogen-induced damage of austenitic-ferritic steels is better that that of single-phase ferritic steels. It has been shown, that duplex steels are however romoted to the hydrogen embrittlement [2]. Numerous advantages of these steels make them attractive for many potential applications, e.g. in the food, chemical, petrochemical and paper industries where they can be used for the manufacture of components intended for exploitation in aggressive environments, such as boilers, pressure vessels, installations in the food industry and mining, pipelines transporting natural gas or oil in contact with seawater. These conditions may favour the penetration of hydrogen into the steel, and thereby promote hydrogen corrosion. A method of reducing hydrogen penetration into steel is to produce a nitrided layer on the surface [3, 4]. A phase with especially advantageous properties in this respect is the S-phase (known as expanded austenite &#947;N [5]), which can increase the resistance to frictional wear and significantly reduce the penetration of hydrogen [3, 6], without altering the high corrosion resistance of the steel. The presence of the S-phase formed during the low-temperature nitriding is manifested in the diffraction spectra as a shift of the diffraction peaks, (which accompan[...]
 
Characterization of friction stir welds of 6013 and 6013/2017A aluminium alloy sheets
 
Krzysztof Mroczka  Jan Dutkiewicz  Adam Pietras  
The Friction Stir Welding (FSW) takes place due to rotation and movement of FSW tool. A tool moves the welded materials along its edges. As a result of the FSW process good quality of a weld is obtained below the melting point. The FSW weld consists of particular zones: the weld nugget (area in the centre), thermomechanically affected zone and heat affected zone. The weld nugget is frequently surrounded by rings known as an onion microstructure (rings) especially within the FSW welds of the aluminium alloys of 6XXX series. The microstructure and properties of the particular zones depend strongly on the welding parameters [1] and the type of the welding tool pin and shoulder. For example, a grain size within the weld nugget was found to depend strongly on the linear velocity of the tool [2]. The various studies of the aluminium alloys that underwent friction stir welding show various dislocation densities within welds&#8217; nuggets [3]. The hardness in the region of the weld can change in many ways [4, 5]. The welds formed by FSW between the aluminium alloy sheets and especially between the 6XXX series alloys are much better than those formed by a high-temperature welding methods like Gas Metal Arc Welding especially due to lower temperature of welding [6]. The FSW technology is applied presently for welding of the aluminium and magnesium alloys as well as copper, steel, composites and dissimilar materials [7÷10]. The alloys of the 6XXX series are often applied in the constructions and transportation industry. The 6013 aluminium alloy has broad application in the production of many car parts like vehicle structure, wheels, panels and others [11]. The mentioned alloy can be welded by the means of the FSW method similarly as other alloys of the 6XXX series [11, 12]. Uzun et al. [13] signaled the possibility of welding the alloy with steel. Therefore, the aim of the paper was to analyze the microstructures and properties of the [...]
 
Characterization of titanium nitride layer on titanium alloy
 
BARBARA SUROWSKA  JAROSŁAW BIENIAŚ  
Titanium and titanium alloys are widely used at some technical and medical applications because of their mechanical and corrosion resistance properties. The Ti6Al4V alloy is the most popular and universal alloy, for example it find a use for the aircraft parts and for implants in dentistry and orthopedics [1÷3]. This alloy is produce as cast and as forging. It belongs to the high strength materials but its wear resistance is low. Therefore various methods of surface modification are used [4÷7], e.g. plasma electrolytic oxidation (PEO), electrophoretic deposition (EPD), vacuum plasma spraying, glow discharge, plasma treatment, chemical vapor deposition (CVD). Nitriding of titanium and titanium alloys has been investigated for many years and is used effectively for protection against wear. In this paper the TiN+Ti2N+&#945;Ti(N) layer deposited by glow-discharge nitriding on the Ti6Al4V alloy is characterized. This hybrid system is destined as outer layer or intermediate layer under other ceramic in biomedical applications and as thin film for adhesive bonding to polymer composites in aircraft applications. Materials and methods The TiN/Ti2N/&#945;Ti(N) layer was deposited on the Ti6Al4V alloy (ASTM grade 5). This hybrid layer was produced by glow-discharge assisted by nitriding in pure nitrogen atmosphere at 1073 K (800°C) and 4 hPa pressure for 3 h. The process was carried out with the use of universal apparatus for different types of thermochemical treatment under glow discharge conditions at Warsaw University of Technology [7, 8]. The thickness of coating was about 40 &#956;m. The phase composition of surface layer was performed by X-ray diffraction technique (XRD). Microstructure and morphology of thin film were analyzed by scanning electron microscope (SEM) with energy dispersive X-ray spectroscopy (ED[...]
 
Comparison of structure and morphology of hydroxyapatite films obtained by sol-gel and RF PECVD methods
 
Anna Zydorczyk  Bożena Pietrzyk  Hieronim Szymanowski  Sebastian Miszczak  
In the recent years, increasing number of applications of hydroxyapatite (HAP) layers as implant coatings have been observed. Due to its chemical composition, similar to that of natural bones, HAP is highly valued by the medical environment. The HAP layer causes the implant to integrate faster into surrounding tissues [1]. Additionally, it is a layer limiting the penetration of metal ions to organism, and preventing the immune system response. A number of methods can be used to produce biocompatible coatings on metals for biomedical applications: high temperature plasma-spraying, electrophoretic deposition, laser deposition, micro-arc techniques, magnetron sputtering and sol-gel techniques [2÷9]. However, each method has its own limitations, often caused by low adhesion strength to the substrate and also by difficulties with controlling the phase composition of the coating during the deposition. In this work HAP layers were deposited by sol-gel method which provided good control of film parameters, and by a new PE RFCVD method. Experimental procedure In sol-gel method, the calcium-phosphate sol was prepared by dissolving Ca(NO3)2&#8901;4H2O and (C2H5O)3PO in ethanol. Next, the solutions were mixed and aged for 15 hours at 60°C. The HAP layers were deposited on samples of AISI 316L stainless steel and silicon wafers by dip-coating method. Samples were withdrawn from sol with constant speed of 35 mm/min and annealed in air at 500°C[...]
 
Composite layers produced on nickel substrate by the PACVD metod with the participation of trimethylaluminum
 
JERZY ROBERT SOBIECKI  RYSZARD SITEK  MICHAŁ TACI KOWSKI  TADEUSZ WIERZCHOŃ  
The PAMOCVD method (Plasma Assisted Metal Organic Chemical Vapor Deposition) is a combination of two methods of deposition from a gaseous phase, namely the MOCVD method (Metal Organic Chemical Vapor Deposition), which is widely used in electronic industry, and the PACVD method (Plasma Assisted Chemical Vapor Deposition) in which the electrical activation of gaseous atmosphere can be done by direct current (DC) or radio frequency current (RF) or microwave current (MW) [1]. The process conducted in the gaseous atmosphere, enriched with metalorganic precursors (MOCVD) and activated by a glow discharge (PACVD), permits producing layers with unique properties, namely good adherence to the substrate, advantageous performance properties (wear and corrosion resistance, heat resistance), and good mechanical properties. This combined process can produce, e.g. layers of the Ti(OCN) type [2], CrN layers [3], titanium and nickel aluminides [4], aluminum coatings [5÷10], ZrO2, or NCD and DLC coatings. The CVD method with the participation of metalorganic precursors has already been used for producing aluminum layers since the end of 1960s (20th century). The use of the reactive atmospheres enriched with vapors of metalorganic compounds permitted lowering the process temperature thanks to the low temperature of decomposition of these compounds. In the production of aluminum coatings, the most frequently used metalorganic precursors are: trimethylaluminum [(CH3)Al3] known as TMA [5÷8], [(CH3)2AlH] (di-methyl-aluminum hydride - DMAH) [5÷10], [i-C4H9)3Al] (tri-isobutyl-aluminum - TIBA) [5÷7], bis(isobuthyl)(-methylcyclopentadienyl) aluminum (III) [6], diemethylamine alane DMEAA - [AlH3N(CH3)2(C2H5)] [6, 7, 9], triimethylylamine alane - TMAA [6, 7] and triethylamine alane - TEAA [6]. Studies carried out during the last years were chiefly aimed at seeking new precursors and examining how they affect the structure and properties of the aluminum l[...]
 
Composition - property relations in low-neodymium Nd-Fe-B-Ti melt-spun alloys
 
Marzena Spyra  Elżbieta Jezierska  Daniela Derewnicka  Marcin Leonowicz  
Modification of the properties of Nd-Fe-B magnets by minor addition of other elements has been studied since their development in 1984 [1÷4]. For neodymium contents lower than that for the stechiometric Nd2Fe14B phase, beside the hard magnetic phase, the soft magnetic phases such as &#945;-Fe, Fe3B and Fe2B is present. Such alloys are called magnetic nanocomposites [5÷6]. However, deacrease of the Nd content leads to substantial drop of the coercivity. Thus, we tried to modify of the microstructure of the alloys by addition of small proportion of Ti. In this work the effect of titanium addition was studied for the alloys content of 7, 8 and 9% at. of neodymium. EXPERIMENTAL The initial ingots were prepared by arc melting of pure elements. The Nd7Fe79-xB14Tix, Nd8Fe78-xB14Tix and Nd8Fe77-xB14Tix ribbon alloys (x = 0, 2, 4 at. %) were prepared by rapid solidification of molten alloys by melt-spinning with the roll speed of 20 m/s. The overquenched ribbons were annealed at 953÷973 K for 20 minutes. The microstructure of the annealed ribbons was studied using a JEOL JEM 3010 transmission electron microscope. The phase constitution was evaluated using X-ray diffraction (XRD) (Philips PW 1140, Co). The magnetic properties were measured using a Lake- Shore 7410 vibrating sample magnetometer in maximum external field of 3 T. RESULTS AND DISCUSSION Addition of Ti for the Nd-Fe-B alloys generally resulted in increase of the onset of crystall[...]
 
Computer simulation of stresses in coatings obtained in the PVD process
 
AGATA ŚLIWA  WALDEMAR KWAŚNY  LESZEK A. DOBRZAŃSKI  
Quick development of different industry parts nowadays determines more requirements concerning engineering materials in the range of mechanical properties, wear resistance, erosion influence and high temperature influence. It is essential to understand phenomena proceeding during production, treatment and service of the engineering material so that it meets the requirements. The internal stress phenomenon, resulting from irregular heating or cooling, during plastic working treatment in the consequence of phase process at mechanical surface treatment, pouring and metal and alloy solidification and also during anti-wear coating deposition has also its impact. One has to perform various tests to acquire that, from destructive methods to the nondestructive ones, like the ultrasonic and diffraction methods [1]. The advanced surface treatment technology, especially among others PVD technology, allows to improve service properties of tools made from the conventional tool materials, which - if not subjected to such treatment - in many cases do not meet the requirements and expectations of tools users. Specifications of the PVD coatings fabrication process require performing analysis of the process parameters effect on material the substrate and also interaction between the coating and material substrate in the intermediate zone. The finite element method is commonly used currently in such branches of science, like: mechanics, biomechanics, mechatronics, materials engineering, and thermodynamics. All types of simulations shorten the design process and give the possibility to investigate the particular factors on the entire model. This is often impossible to achieve in real conditions or not justified economically. The finite element method makes it possible to understand better the relationships among various parameters and makes it possible to select the optimum solution [2]. Many analyses are performed nowadays using advanced calcul[...]
 
Crystallographic orientation of aircraft engines turbine blades made of CMSX-4 single crystal nickel superalloy
 
Arkadiusz Onyszko  Włodzimierz Bogdano wicz  Andrzej Nowotnik  Krzysztof Kubiak  Jan Sieniawski  
The aircraft engines turbine blades are considered to be so-called Flight Safety Parts (FSP). They are subject to exceptional requirements related to the production process and quality control. They feature narrow dimensional tolerances and perfect surface quality. Requirements with regard to metallurgical purity, permissible casts&#8217; gas and shrinkage porosity, crystallographic orientation, phase composition and relative volume of strengthening phases as well as heat resistance and high-temperature creep resistance are also strict. Single crystal blades of nickel superalloys belong to the group of products most difficult to produce and meeting strictest reliability requirements [1, 2]. Blades of the first turbine stages and guide vanes made of nickel and cobalt superalloys are subject to continual modification both in terms of their chemical composition, heat treatment as well as manufacturing technology. The manufacture of precise casts of single crystal blades of complex shape of the blade and locking piece is a difficult process, belonging to highly advanced technologies. This applies also to the technology of ceramic moulds exposed to especially difficult conditions, including increased time of interaction with a liquid metal. Single crystal blades feature the highest hightemperature creep resistance as compared with blades obtained in the process of directional crystallisation or conventional casts of microstructure composed of equiaxial grains [2÷5]. Single crystal superalloys&#8217; properties depend on the crystallographic direction taken for studies. Hence the assessment of single crystal casts&#8217; quality is related to determination of their crystallographic orientation, which provides the basis for mechanical properties analysis. It has been assumed on the basis of literature review, that the value of the angle of direction [001] deviation from the angle of single crystal superalloys growth cannot exceed 15°.[...]
 
Development of [FeCoTaN/TaN]n multilayer films for the simultaneous provision of wear protection and soft magnetic properties
 
Christian Klever  Stefanie Spitz  Harald Leiste  Klaus Seemann  Michael Stüber  Sven Ulrich  
Wear protection coatings produced by physical vapour deposition techniques are established in engineering applications since the early 1980ies. However, a real-time optical inspection of their current state in service is impossible in most cases due to non-accessibility. As an approach to overcome this problem, we recently started the development of wear protection films with intrinsic sensor functionality based on the implementation of a magnetoelastic ferromagnetic phase [1]. The development of soft ferromagnetic thin films is driven by the increasing trend of miniaturization in many technological applications. Thin films in which low coercivity is combined with a strong uniaxial anisotropy, a high saturation polarization, and a high electrical resistance, are interesting for the use in applications where high frequency electromagnetic fields are applied, such as microinductors and transformers with magnetic cores [2]. In particular, such thin films are generally suited for the use in remote interrogable sensor applications [3]. As an interesting material class, nanocrystalline FeCoTMN films have been developed in the past years. In such films, FeCo grains are refined by the surrounding TMN matrix which results in the reduction of the coercive fields and considerable electrical resistance. Additionally, grain growth processes upon annealing are hindered up to considerable temperatures. For the induction of a uniaxial ferromagnetic anisotropy, usually an external static magnetic field is applied, either during film growth or ex-situ with simultaneous annealing. In numerous studies, FeCoTaN films were shown to exhibit a combination of properties which is a good compromise between the above requirements [4, 5]. However, there has been no report available on the optimization or at least the determination of the mechanical properties of nanocrystalline ferromagnetic composite films suitable for applications in electromagnetic hi[...]
 
Development of Ti-based materials for alloplastic implants
 
ANDRZEJ ZIELIŃSKI  SYLWIA SOBIESZCZYK  BEATA śWIECZKO-ŻUREK  
The Ti-based biomaterials, light materials of highest corrosion resistance and biocompatibility [1], have also some disadvantages. They may slowly dissolve and result in serious illnesses if the Ti-Al-V alloy is applied [2]. The Ti alloys have Young modulus too high as compared to that of a bone [3], fatigue limit too low [4], and the bone-implant interface strength too weak [5]. The new no Al and no V alloys are developed [6]. This paper is aimed at demonstrating the previous results and current research work in this area made by Advanced Biomaterials Research Group at the Faculty of Mechanical Engineering, GUT. EARLY AND LATE REACTIONS TO METALLIC IMPLANTS The research is made on possible allergies of patients to titanium and Ti alloys. The cases of such allergies were discovered in hospital examinations, mainly for stainless steels but also a case for Ti alloy was found. The biodegradation can result from different origin: presence of bacteria [1÷3], wear of surgical tools, improper material [3, 4]. Even for Ti alloy severe degradation can occur (Fig. 1). The modelisation of change in biological environment of an implant following inflammation process and assessment of metallic ions` release by special tests and sensitive chemical techniques are performed. EFFECTS OF BACTERIA ON CORROSION One of possible determinants of early allergies and inflammation processes can be presence of bacteria [1, 4, 5]. The exposure tests in biological environments have shown that different bacteria may have different and substantial effect on corrosion resistance of titanium alloy. Especially, in presence of Staphylococcus aureus no important corrosion occurs and Enterobacter cloacae presence results in fast corrosion - Figure 2. The results are explained by a model under elaboration in which biofilm of different thickness, permeability and distance from a metal surface affects composition and pH of solution adjacent to a metal, creating c[...]
 
Directionally solidified CMSX-4 nickel based superalloys; microstructure, orientation, residual stress, microanalysis
 
BOGUSŁAW MAJOR  KRZYSZTOF KUBIAK  Jan Bonarski  Maciej Szczerba  Łukasz Major  Anna Góral  Anna Rakowska  
Single crystal nickel based superalloys still belong to the most widely used and reliable materials for the most exposed parts of gas turbine [1÷5]. Directional solidification (DS) is a technology, which enables to produce gas turbine blades and vanes with columnar crystal or single crystal structures. High temperature mechanical properties of single crystal nickel base superalloy castings are better than castings with polycrystalline structures [1]. The aims of producing of the blades as single crystals are to eliminate grain boundaries which favour creep and ensuring of [001] crystal orientation with minimum of Young&#8217;s modulus that is suitable for thermal fatigue resistance. The final structure of the castings prepared by DS is influenced by the parameters of the process, therefore it is inevitable to map and control them [5]. A large number of the alloys used rely on carefully tailored compositions and heat treatment schedules that result principally in a microstructure consisting of gamma (&#947;) matrix (FCC crystal structure) and ordered gammaprime (&#947;&#697;) (L12) phases [4]. The aim of investigations was to study microstructure in respect to its inhomogeneity in different scale, defect of microstructure in nanoscale, crystallographic orientation measured using X-ray texture technique as well as residual stress by application of X-ray method in directionally solidified CMSX-4 nickel-based superalloys produced using the facilities working at the Rzeszow University of Technology. mATERIAL AND METH ODS OF EXAMINATI ONS Materials for examination were fabricated at the vacuum metallurgy laboratory of the Faculty of Materials Science and Technology at the Rzeszow University of Technology by application of the single crystal casting system. A nickel based superalloy CMSX-4 was produced with the nominal chemical composition as follows: Cr-5.7; Co-11; Mo-0.42; W-5.2; Ta-5.6; Al-5.2; Ti-0.74; Re-3; Hf- 0.1; Ni-balance.[...]
 
DSC examinations of the Al-20 wt. % Zn sand-cast alloy inoculated with Ti-containing grain-refiners
 
DI MITRIOS TSIVOULAS  TOMASZ CZEPPE  WITOLD K. KRAJEWSKI  
Master alloys (MAs) are added to the melt during casting in order to achieve as fine and uniform equiaxed grain structures as possible upon solidification. Their action is enhanced by the presence of higher amounts of solute in the base alloy [1]. The main concern for grain refinement is to avoid the formation of columnar or mixed columnar and equiaxed grains in the cross-section of the cast ingot. The sole restriction on the grain refinement ability of the master alloys is imposed by the ingot dimensions and the cooling rate; a large ingot size and a low cooling rate lead to larger differences in grain morphology and size between the surface and centre of the ingot [2]. There are several benefits for a finer cast structure after solidification. These are, namely, fewer casting defects, easier processing in the subsequent fabrication stages, higher ductility of the ingot surface shell, which reduces surface cracking susceptibility, and higher yield stress of the final wrought products [2]. However, the grain refinement process is affected by several parameters, such as the quantity of the master alloy added in the melt, the distribution characteristics of the nucleating particles in the master alloy and in the melt, the exact compositions of the master alloy and of the base alloy, the casting speed and temperature, the ingot dimensions and the cooling rate [1]. Regarding the four master alloys of the present work, the (Al, Zn)3Ti has not been studied before, while the ZnTi4 alloy was reported to yield a larger grain size compared to the typical AlTiB and AlTiC additions [3, 4]. The latter two MAs constitute the most common refiner additions, with the AlTiB-type reported to be superior in terms of grain refinement potential compared to AlTiC-type [2÷5]. This is said to occur due to the lower number of nuclei in the latter MA-type [2]. Li et al. [6] reported that increasing the amount of Ti and C beyond the standard contents in [...]
 
Effect of Al and Iradditions on surface morphology and topography of FeCrNi coatings
 
Barbara Kucharska  
The magnetron sputtering deposition (MSD) method belongs to the basic and the most important methods of depositing coatings in vacuum conditions, PVD [1÷3]. A very valuable advantage of this method is the possibility of depositing coatings, particularly those of complex chemical composition, in a broad range of thicknesses, starting from several angstroms. This method is successfully used for depositing coatings based on steels, also heat-resistant grades, which include 310S steel. In the chemical composition of this steel are the additions of Ni (~20%) and Cr (~25%) [4÷6]. For better resistance the chemical composition are enriched by addition of high melting elements [7, 8]. The properties of magnetron coatings depend on the sputtering process parameters, which influence the microstructure and the grain size of coatings [9, 10]. The essential purpose of applying coatings is to protect the substrate or to modify the properties of surface. This function can only be fulfilled by coatings that are tight and exhibit good adhesion to the substrate [11]. These conditions are applicable in particular to coatings intended for protection against corrosion in liquid solutions, as well as in high-temperature oxidation conditions [12÷15]. Also, in corrosion protection, surface smoothness plays an important role. Low surface roughness and the absence of surface defects inhibit the build-up of aggressive ions and deposits that might initiate pit corrosion [16]. The paper presents the investigation of the surface topography of magnetron coatings based on heat-resisting steel of 310S enriched Al and Ru additions. The AFM (Atomic Force Microscope), SEM (Scanning Electron Microscope), and profilometric techniques were used in the investigation. material Coatings of the composition of 310S heat-resisting steel, deposited on a substrate of the same steel by the magnetron sputtering method, were examined. The magnetron targets were two discs, eac[...]
 
Effect of annealing on the structure and properties of Ni46.4Mn28.5Ga25.1 single crystal
 
RafaŁ Wróblewski  Krzysztof Sielicki  Marcin Leonowicz  
Ferromagnetic Heusler alloys are based on the X2YZ phase. The first notice on such alloys comes from Friedrich Heusler et al. who characterized the Cu2MnAl alloy in 1903 [1]. That alloy showed ferromagnetic properties although none of the components was ferromagnetic. In 1934 Bradley and Rodgers reported on the effect of heat treatment of Cu2MnAl alloy [2]. Main conclusion coming from this work is that the ferromagnetism of the Heusler-based alloys depends not only on the chemical composition but also on the positions of neighbouring atoms. The Ni2MnGa-type alloys due to their magnetic field induced strain (MFIS), up to 10%, attract attention of the scientists and engineers. Over ten years of studies, since the first report, the magnetic shape memory effect (MSME) [3] has brought many publications on the structure and properties of the Ni2MnGa alloys. Especially structure of the martensite, its type and forming conditions is an object of great interest of many researchers. Various heat treatment procedures were proposed. For example Gaitzsch et al. have found that annealing at 803 K for 24 h leads in the Ni50Mn30Ga20 alloy to formation of the 7M martensite [4]. In our previous work we studied the effect of annealing temperature and the cooling rate on the structure of the polycrystalline Ni50Mn29Ga21 alloy [5]. It was found that the final structure strongly depends on the conditions of heat treatment and the 7M martensite can be produced by annealing [...]
 
Effect of chemical composition variation on mechanical properties of 6xxx aluminum alloys
 
Grażna Mrówka-Nowotnik  Jan Sieniawski  
The 6xxx-group contains magnesium and silicon as major addition elements. These multiphase alloys belong to the group of commercial aluminum alloys, in which relative volume, chemical composition and morphology of structural constituents exert significant influence on their useful properties [1÷4]. In the technical 6xxx aluminium alloys contents of Si and Mg are in the range of 0.5÷1.2 wt. %, usually with a Si/Mg ratio larger than one. Besides the intentional additions, transition metals such as Fe and Mn are always present. If Si content in Al alloys exceed the amount that is necessary to form Mg2Si phase, the remaining Si is present in other phases, such as Al-Fe-Si and Al-Fe-Si-Mn particles [1, 5÷13]. The aluminium alloys of 6xxx group have been studied extensively because of their technological importance and their exceptional increase in strength obtained by precipitation hardening. The 6xxx aluminium alloys are mostly used in extruded products, as well as for construction and automotive purposes. The ease with which these alloys can be shaped, their low density, their very good corrosion and surface properties and good weldability are factors that together with a low price these make them commercially very attractive. The precipitation of the metastable precursors of the equilibrium &#946;(Mg2Si) phase occurs in one or more sequences which are quite complex. The precipitation sequence for 6xxx alloys, which is generally accepted in the literature [1, 7], is: SSSS &#8594; atomic clusters &#8594;GP zones &#8594; &#946;&#8243;&#8594; &#946;&#697;&#8594; &#946; (stable) Some authors [8] consider the GP zones as GP1 zones while the &#946;&#8243; is called a GP2 zone. The most effective hardening phase for this types of materials is &#946;&#8243;. The medium strength AlMgSi aluminium alloys are commonly processed by extrusion. Their extradubility depends to a large extent on chemical composition, casting condition and heat tre[...]
 
Effect of nanostructure on the Ti Grade2 properties
 
Halina Garbacz  
Titanium is the metal of choice for the fabrication of dental and orthopedic implants due to its excellent biocompatibility and high corrosion resistance to physiological environment. However, commercially pure titanium exhibit low strength and wear resistance, which is related to low hardness. Mechanical properties of the bulk material can be ameliorated by several hardening mechanisms, e.g. solid solution (alloying), dispersion strengthening, grain refinement. Ti6Al4V represents one of the most common &#945;+&#946; alloys [1]. However, its drawback could arise from the alloying elements with toxic effects. Vanadium ions are classified as toxic [2], inhibit enzymes or can interact with intercellular components [3]. To overcome these concerns, the toxic V was substituted by inert Nb to create the alloy Ti6Al7Nb [4] similar to or with even slightly better properties than Ti6Al4V. High strength of metallic implants without using alloying elements can be achieved by grain refinement of titanium as the Hall-Petch relation predicts, what was experimentally proven [5÷7]. Severe plastic deformation (SPD) processing aims to get microstructural refinement to a level not achievable with traditional processing [8÷10]. Hydrostatic extrusion is one of the SPD methods, which allows to obtain a significant grain refinement, down to the nanometric scale. This method is developed in collaboration between the Warsaw University of Technology and Institute of High Pressure Physics, Polish Academy of Sciences in Warsaw. In comparison to the standard SPD methods, the hydrostatic extrusion (HE), as a method of grain refinement, usually requires a significant smaller total strain [11]. A number of commercially pure metals and alloys have been processed by HE at ambient temperature to evaluate the potential of this method for achieving grain size refinement. For pure metals, the highest degree of grain size refinement was achieved in the case of titan[...]
 
Effect of rapid solidification on the structure and mechanical properties of Al-4Fe-4Ni alloy
 
Anna Kula  Ludwik Blaz  Makoto Sugamata  Grzegorz Wloch  
Aluminum alloys are widely used in constructions of light components at aerospace and automotive industry. In order to improve the performance of these materials, especially at elevated temperatures, novel alloying systems and adequate production processes, are extensively studied. Among several technologies, the rapid solidification processes (RS) have been received considerable attention as an effective way to design modern materials with excellent combination of the strength, sufficient ductility and other useful properties [1, 2]. RS materials are characterized by specific features, such as refined grain size, increased solid solubility of some elements in the alloy matrix, which often result in the suppression of some precipitates formation and modification of their morphology. RS process is a relatively attractive technique for Al-based alloys containing rare earth metals such as Ce, Y and transition metals such as Mn, V, Cr, Ni and others. Low solubility of these alloying elements has restricted the content of alloying elements to low values at traditional metallurgy processes, as the formation of coarse intermetallics (30 &#956;m in diameter or larger) deteriorate mechanical properties [3]. Hence, RS processes are particularly convenient for the structure refining and modification of the microstructure in those alloying systems. It has been reported that the strength of aluminum-transition metal alloys at room and elevated temperature is improved by uniform dispersion of fine intermetallic compounds formed under rapid solidification and high cooling rates [4÷7]. The objective of the present study is to analyze the influence of rapid solidification process on the microstructure and mechanical properties of the Al-4Fe-4Ni alloy on the basis of experiments performed on both RS-material and s[...]
 
Effect of selected parameters of the melt-spinning process on the thickness and magnetic properties of Nd-Fe-Al ribbons
 
Waldemar Kaszuwara  Bartosz Michalski  Jerzy Latuch  Janusz Rębiś  
The Nd-Fe-Al alloys, first described by Inoue [1] in 1996, are inferior to Nd-Fe-B magnets as far as the magnetic properties are concerned, but their great advantage is that they do not need additional annealing (performed after melt-spinning) to achieve their possibly good magnetic properties. These properties depend on the cooling rate of the melted material, and the best values achieve at the quenching rates at which the ribbons have a thickness of the order of tenths of millimeter. Magnets of this size could be used directly, without further treatment, in electromechanical micro-devices or in the MEMS technique [2]. In the application range so defined, the melt-spinning processed Nd-Fe-Al alloys can compete with Nd-Fe-B alloys, since the basic technology of Nd-Fe-B magnets does not permit producing easily components with a thickness of the order of tenths of millimeter. The thickness and properties of the Ne-Fe-Al ribbons can be modified by controlling the melt-spinning process parameters, such as the rotational speed of the wheel, the shape and size of the crucible opening, the temperature of the melted material, and the pressure of the ejecting gas [3]. It has been demonstrated thus far that rapid cooling (at a wheel rotational speed of 20÷30 m/s) promotes an increase of the share of an amorphous phase and gives ribbons with poor magnetic properties. When cooled at lower rates, the material contains a greater proportion of crystalline phases and has substantially better magnetic properties [3, 4]. The microstructure of the Nd-Fe-Al alloys has been described in many publications [5, 6], but there is no consistency in the interpretation of the results. At present, we can say that the Nd-Fe-Al alloys with the best properties contain very small amounts of the amorphous phase and that their structure is multi-phase and built on a nanometric level [7]. The aim of the present study was to examine the possibility of producing [...]
 
Electrical studies of phase stabilities in the Ce2O(CO3)2·H2O/CeO2 and LaOHCO3/La2O3 systems
 
Bahci ne Bakiz  MADJ ID ARAB  FRÉDÉRIC GU INNETON  LAMIA BOURJA  ABDE LJALIL BEN LHACHEMI  JEAN-RAYMOND GAVARRI  
To develop new selective sensing devices for gas detection, working in environmental conditions, we are investigating materials susceptible to interact successively with H2O (vapor), CO2 gas and finally with a specific gas such as methane CH4, carbon monoxide CO. One possible solution for improving the selectivity should be to use oxide phases highly sensitive to carbonatation or hydration, presenting successive phases stable at increasing temperatures [1÷6]. Two systems are presently investigated to determine their relative reactivities with CO2 and H2O: the La2O3-H2O-CO2 and CeO2-H2OCO 2 rare earth based systems. The lanthanum based system presents a series of phases LaOHCO3, La2O2CO3 and La2O3 stable in three different temperature ranges [7÷15]. It also presents a high interest because of the strong capacity of hydration of the oxide phase La2O3. In addition, we have recently shown that these La2O3, LaOHCO3 and La2O2CO3 phases might present interesting catalytic activities, in presence of methane-air (CH4-air) and carbon monoxide-air (COair) flows at various temperatures [16]. The cerium system seems to behave differently with one stable Ce2O(CO3)2&#183;H2O phase (with 3+ valence for cerium ion) and the CeO2 oxide (ceria) stable under air with 4+ valence for cerium ion [17, 18]. In the present study, we focus our attention on the decarbonatation kinetics of the carbonate phases and on the carbonatation kinetics of the oxide phases: the main objective of these analyses should be to determine their electrical sensitivities during gas solid interactions with CO2. These correlations between phase changes and electrical responses are not known, and they could deliver interesting informations to develop miniaturized electrical devices including microsensor or microabsorber systems. Exp erim ental detail s Elaboration The initial samples were first synthesized following the same approach. A first step consisted in preparing two c[...]
 
Electrodeposition of nanocrystalline Ni-Mo coatings from citrate electrolyte solution
 
EWA BELTOWSKA-LEHMAN  AGNIESZKA BIGOS  PAULINA INDYKA  LESZEK TARKOWSKI  MARCIN KOT  JERZY MORGIEL  
Alloys containing molybdenum, e.g. Ni-Mo, are characterized by high hardness, high wear, thermal and corrosion resistance as well as good catalytic properties for hydrogen evolution in alkaline solutions. They also offer an important alternative to hard chromium coatings as chromates are known to be highly toxic and according to EU directive they should be eliminated from manufacturing process, e.g. in automotive and aviation industries [1]. However, these alloys are difficult to prepare by conventional thermal methods due to the large differences in their melting points (Ni - 1455°C, Mo - 2620°C) and their limited mutual solubility [2]. Several techniques have been proposed for the Ni-Mo alloy preparation: mechanical alloying, plasma sputtering, gas condensation and electrocrystallization. Electroplating is a relatively simple, low cost and low temperature method suitable for mass production, where the substrates of complex shape can be uniformly plated by coatings with high rate. However, it is known that molybdenum in a metallic state cannot be separately electrodeposited from an aqueous solution of its salts, but it can readily be co-deposited with iron-group metals such as nickel, forming an alloy. The phenomenon is called induced co-deposition [3]. The mechanism is still not clearly understood, although a few hypotheses are presented in literature [3÷6]. The electrodeposition of Ni-Mo alloys have been extensively investigated [7÷11]. A great number of galvanic baths were studied, e.g.: sulphate, sulpho- salicylate, acetate, tartrate, pyrophosphate, amonia and citrate. Most deposits obtained from these baths were poor quality, porous or cracked and electrodeposition process was not efficient, however pyrophosphate and citrate electrolytes are the most promising. In the present work the correlation of electrodeposition conditions from citrate solution with the coating properties was determined. The surface morphology as a f[...]
 
FEM simulation of superplastic forming of a spherical cap made of Ti-6Al-4V
 
PIOTR LACKI  JANINA ADAMUS  MACIEJ MOTYKA  
The phenomenon known as superplasticity has been observed for a wide range of materials including metallic alloys such as: titanium, and aluminium alloys, ceramics, composites and minerals [6÷8, 11, 12]. Superplastic forming (SPF) is a technological process that enables large deformation with no loss of material continuity. Slip along grain boundaries is considered to be the main mechanism of superplastic forming. Depending on the kind of material and process parameters it is possible to obtain elongation of up to several hundred percent. Superplastic forming is used for the materials with poor formability in conventional conditions or if their degree of deformation is insufficient. Superplastic forming is particularly well suited for forming of Ti-6Al-4V titanium alloy. Ti-6Al-4V titanium alloy is one of the most commonly materials associated with superplastic forming. It is used for light and highly strong structural elements in aircraft industry. Superplastic forming processes in aircraft industry applications require fine-grained equiaxed microstructure of Ti&#8209;6Al&#8209;4V alloy. In practice, superplasticity conditions are summarised as a grain size less than 10 &#956;m, low strain rate of less than 10-3 s-1 and forming temperatures of T &#8805; 0.5 Tm, where Tm is the melting point of the material [13]. Materials for superplastic forming process need to be specially prepared by hot metal forming and heat treatment [5, 6]. A design of superplastic forming is much more difficult than conventional forming processes because of the larger amount of parameters that have to be taken into consideration and controlled in narrow range of tolerance. Strain rate is the key parameter and it requires special attention. This parameter decides whether the necking and rupture occur in the drawn-part. Titanium alloys exhibit high dependence of yield stress on temperature and strain rate [8÷10]. The current design methods of superplasti[...]
 
Fluidized Bed Atmospheric Diffusion Treatment (F-A/D-T) – scopes and limitations
 
Józef Jasiński  Leopold Jeziorski  Jarosław Jasiński  
Fluidized Bed Atmospheric Diffusion Treatment of the alloys and metallic materials during tools and machine parts volumetric heat treatment gives possibility to the surface layer diffusive saturation of metallic materials with an interstitial elements. Formation of the Cr, Zn, Ti, W, Nb coatings and layers using fluidization method is also known. Technically fluidization effect was used 60 years ago in the United Kingdom for the precipitation hardening of the aluminium alloys [1]. In Poland the interest for fluid heat treatment started in the 1970 [2]. Researches using fluidization technology were guided mainly by the two units, Institute of Precision Mechanics - - Warsaw and Materials Science Institute - Czestochowa Univeristy of Technology. The experiments performed initially by the Institute of Precision Mechanics were focused mainly on the tools low-temperature nitriding and oxidizing [3], while Materials Science Institute in Czestochowa researches were interested in carburizing and carbonitriding mechanisms and kinetics of tools and machine parts in the organic and inorganic fluidized beds. Next years, differences rela[...]
 
Gas nitrided layers on precipitation hardened stainless steel
 
Paweł Kochmański  Jolanta Baranowska  
This paper presents research results of nitrided layers on Sandvik NanoflexTM stainless steel, known also as 1RK91, which belongs to precipitation-hardening stainless steel group. This is an ultra highstrength material with a combined excellent corrosion resistance. By a simple heat treatment after cold deformation, extremely high tensile strength levels (2000 MPa and 3000 MPa for wire) in combination with a good toughness (up to ca. 600 HV) could be obtained. Achievement of such good mechanical properties is caused thanks to very fine, submicroscopic precipitations as: Cu, Fe2Mo, &#414;-Ni3(Ti, Al), R-phase, described in several publications [1÷7]. Due to its special properties, this steel is suitable to manufacturing very responsible surgical tools. Heat treatment of the steel consists of two steps, i.e. solutioning (ca. 1050÷1100°C), and precipitation hardening by ageing at temperature typically 475°C for 4 hours. This range of hardening temperature overlaps with temperature of nitriding process, therefore thermo-chemical and heat treatment could be conducted simultaneously under condition of sufficient corrosion resistance of the layers manufactured at this temperature. Although limited studies have been conducted to investigate the plasma and gaseous nitriding response of 17-4 PH stainless steels [8÷12], very little work has been done concerning the nitriding behaviour of Nanoflex steel [13, 14]. Sun and Bell have studied layers obtained on 17-4 PH with the plasma nitriding at temperatures between 350 and 450°C [7]. They observed in layers nitrided at temperatures lower than 425°C &#8220;white" and featureless morphology after etching. The resultant XRD patterns for these layers are typical of an amorphous like structure, without any distinct reflection peaks. Frandsen with others [14] successfully nitrided Nanoflex steel using gaseous process at temperature below 425°C for long duration time (16÷20.5 h). Obtained by them [...]
 
Grain imaging and measurement on cross-section of turbine blade using EBSD and optical methods
 
Agnieszka Szczotok  Bartosz Chmiela  Maria Sozańska  
Turbine blades are termed Flight Safety Parts (FSP). Imaging and measurement of grain in case of the blades is very important, because grain size, shape and distribution strongly affect the mechanical properties of the blades. The size and shape of primary grain are basic structural criteria for quality evaluation of precision cast products from nickel-based superalloys. The evaluation of fine-grained product is of great importance to metallurgists. This work which has traditionally been carried out using light microscopy can be performed by means of the electron backscattered diffraction (EBSD) technique used in the scanning electron microscope (SEM). EBSD is nowadays capable of undertaking such a study. EBSD has been known for many years (the diffraction of electrons was first observed in 1928 by Kikuchi [1]), but only widely applied in the last 10 years. EBSD is now a fast, automated technique which is utilized to determine microtexture (texture on the scale of the microstructure), microstructure quantification, grain and phase boundary characterization, phase identification and strain determination [2÷4]. EBSD is based on acquisition and analysis of Kikuchi diffraction patterns from the subsurface of a specimen in an SEM. In EBSD a stationary electron beam strikes a tilted crystalline sample and the diffracted electrons form a pattern on a fluorescent screen. The diffraction pattern can be used to measure the crystal orientation, as well as boundary misorientations, discriminate between different materials, and provide information about local crystalline perfection. When the beam is scanned in a grid across a polycrystalline sample and the crystal orientation is measured at each point, the resulting map reveals the constituent grain morphology, orientations and boundaries. Electron backscatter diffraction technique to measure grain-specific orientations and misorientations was first recorded more than 20 years ago [5] and[...]
 
High and low voltage anodic etching of microand nanocrystalline Ti-based biomaterials
 
GRZEGORZ ADAMEK  JAROSŁAW JAKUBOWICZ  
Titanium based materials are commonly used as biomaterials due to their excellent biocompatibility and mechanical properties. In respect to biomedical applications, usually we are interesting in pure Ti, Ti-6Al-4V and other alloys as well as Ti-ceramic biocomposites [1÷8]. To improve biocompatibility, osseointegration or corrosion resistance, the implant surface improvement is required, which provide sufficiently high roughness. The rough surface of the implant for hard tissue applications can be prepared mainly by mechanical [9] or electrochemical [10, 11] methods. In the electrochemical process, the material is an anode immersed in the electrolyte, so the process is called anodic oxidation. The anodic etching can be made at broad potential range, which results in different oxide type. The etching usually proceeds in H3PO4 or CH3COOH electrolytes with small HF or NH4F content. These small additions, usually in the range of 0.1÷2%, result in increasing current density followed to enhanced surface dissolution. Additionally, the etching rate can be substantially improved by decreasing grain size. For nanostructure materials, the large volume fraction of the grain boundaries states an easy way for the electrolyte penetration. Atoms, which lie on the grain boundaries are firstly removed and additionally small nanograins are easily released from the alloy, resulting in pores formation. That material has lower density than microcrystalline counterpart and the etched surface is comparable in morphology to the metallic foams. Due to large pores, this material is attractive for strong fixation with bones. experimental data In this work, the electrochemical etching was applied to the surface modification of the microcrystalline Ti, as well as micro- and nanocrystalline Ti-6Al-4V alloys. The microcrystalline materials were bought in Godfellow and, nanocrystalline one was prepared by 48 h mechanical alloying in SPEX 8000 [...]
 
Influence of a high-temperature hydrogen treatment on a microstructure and surface fracture in Ti-6Al-4V alloy
 
Maria Sozańska  
Hydrogen is a unique alloying element in titanium alloys because, unlike other elements, it can easily be added and removed without melting. Titanium and its alloys show the absorbability of almost 60 at. % of hydrogen at 600°C. The limit hydrogen of solubility in Ti&#945; is very low and does not exceed 0.05 at. % at room temperature. The limit hydrogen of solubility in Ti&#946; is much higher and its maximum value is 48 at. %. Since the beginning of the titanium industry, a great deal of attention has been paid to control the hydrogen content at titanium products - above 0.2 ppm. The presence of hydrogen in titanium alloys usually results in degradation of their microstructure and properties, as well promote some undesirable effects such as hydrogen corrosion and hydrogen embrittlement [1]. Treated usually as a component that has a degrading effect, hydrogen can also be an alloying component with positive temporary influence on microstructure and properties of titanium alloys, in particular the two-phase ones [2÷4]. In the presented work, the results of investigation of division of lamellar microstructure by hydrogen action are presented and discussed in detail. The cyclic heat treatment operation with the hydrogen atmosphere is tested. MAterial and EXPERIMENTAL Details Two-phase Ti-6Al-4V alloy with: Al - 6.2 wt. %, V - 4.3 wt. %, Fe - 0.3 wt. % and Ti - in balance was investigated. The alloy was annealed at 1100°C for 1 hour and slowly cooled in the furnace. Principles of high-temperature hydrogen treatment with cyclic operation in Ti-6Al-4V alloy In titanium alloys, hydrogen most often appears as[...]
 
Influence of boron on the surface microstructure of sintered AISI 316L austenitic stainless steel
 
Jan Kazior  Tadeusz Pieczonka  
Boron is one of the most suitable element investigated with the aim to activate sintering of stainless steels powders, whose properties are strongly influenced by residual open porosity. Due to it high affinity for oxygen, boron reduces the surface oxide of the powders. Furthermore, boron is &#945;-stabilizer element and it forms different types of borides (depending on the composition of the base material) which react with the matrix producing eutectic liquids at lower temperatures than those usually adopted for the sintering of stainless steel, what in consequences increases density [1÷7]. However there are many factors, beside chemical composition, which influence liquid phase sintering: particle size, green density, sintering atmosphere, temperature, time of isothermal holding and heating rate. Their combined effect makes it more difficult to envisage and control this process. For small components the control of the heating rate is sufficient to ensure uniform densification, but for complex components the densification variation are influenced first of all by the amount of liquid, which is related to the mutual solubility of the base and additive. As far as boron is concerned, depending on its concentration and heating rate, a transient or persistent liquid phase during sintering is induced and densification variation and microstructure are changed. During persistent liquid phase sintering, both primary and secondary rearrangement occur, which promote a considerable densification. Near full density can be easily obtained, but the effect on the mechanical properties is partially (sometimes significantly) reduced by the boride particles resulting from the solidification of the eutectic liquid, which remain as an almost continuous network surrounding the ferrous based grains. Whilst hardness and strength are increased, ductility and toughness are lower than it could be expected, since this network constitutes a low energy path[...]
 
Influence of casting parameters on thermal properties of bulk metallic glass Cu48Zr36Ag11Ti5
 
Piotr Błyskun  Jerzy Latuch  TADEUSZ KULIK  
Bulk metallic glasses take their structure straight from the liquid. In opposition to the crystal metallic alloys they possess neither a crystalline structure nor its defects, such as vacancies, dislocations or grain boundaries [1]. This causes an extraordinary properties of this group of materials. As regards to their properties, metallic glasses differ significantly among each other, because of their sensitivity to even the slightest change of chemical composition. However, it is possible to describe same general features. Bulk metallic glasses exhibit high compressive strength (from 2 to 5 GPa) [2, 3] and relatively low Young&#8217;s modulus (70÷90 GPa) [4], what gives rise to an ability of accumulating a large amount of elastic energy. Moreover, they have very high wear resistance [5] that comes not only from the hardness [6], but also from very high surface smoothness [7]. These materials also exhibit very attractive formability. A characteristic temperature area of very high viscosity appears during heating before crystallization of the amorphous structure. This area is defined as &#916;Tx and is called a supercooled liquid region. It appears between the onset temperature of crystallization - Tx and the glass transition temperature - Tg: &#916;Tx = Tx - Tg. In this temperature region metallic glass is very susceptible for plastic deformation (that may reach 106%) and many little parts can be put together to produce one complex detail [5]. What is important, the amorphous structure is not lost after heating for short time [8÷10]. In addition, the parameter &#916;Tx is often being used to describe glass forming ability of a bulk glassy alloy. It means that alloys with higher value of &#916;Tx exhibit better glass forming ability. For this reason, the research effort is focused to find optimal manufacturing parameters of the glass with the widest supercooled liquid region. A lack of long range ordering (characteristic for amo[...]
 
Influence of initial heat treatment on the structure and creep resistance of austenitic Fe-Ni alloy
 
Kazimierz j. Ducki  Marek Hetmańczyk  
Austenitic Fe-Ni alloys precipitation-strengthened with intermetallic phases of type &#947;&#8242; (Ni3(Al, Ti)) obtain their optimum properties after multi-stage heat treatment consisting of solution treatment (or annealing) and various ageing variants. Most frequently for such type of alloys, solution heat treatment from a temperature 980÷1010°C and single-stage ageing at temperature of 710÷730°C during 16÷20 h are applied [1÷4]. For some Fe-Ni alloys after solution, it is recommended to apply two-stage ageing, which consists of carrying out a controlled cooling cycle between two isothermal soaking processes [5, 6]. In the presented paper, investigation was initiated concerning the effect of initial heat treatment on the structure, mechanical properties and creep resistance of an austenitic Fe-Ni alloy precipitationstrengthened with an intermetallic phase of the &#947;&#8242; type. MATERIAL AND PROCEDURE The examinations were performed on rolled bars, 16 mm in diameter, of an austenitic Fe-Ni alloy of A-286 type. The chemical composition of the material is given in Table 1. Specimens of Fe-Ni alloy were subjected to tests after two variants of heat treatment, i.e. solution heat treatment and single-stage ageing and solution heat treatment followed by two-stage ageing. Parameters of heat treatment for the investigated Fe-Ni alloy were determined based on previously carried out studies [7, 8]. For the investigated alloy after solution heat treatment in the conditions 980°C/2 h/water, two variants of specimens ageing were used for comparison, i.e.: -- single-stage ageing (variant A): 715°C/16 h/air, -- two-stage ageing (variant B) : 720°C/8 h + cooling in the furnace up to a temperature of 650°C + 650°C/8 h/air. A schematic course of heat treatment of specimens made of the investigated alloy is presented in Figure 1. A static tensile test was carried out using a strength testing machine MTS-810. The examinations were carried [...]
 
Influence of manufacture conditions on the properties of CMSX-4 single crystal castings
 
Krzysztof Kubiak  Arkadiusz Onyszko  Jan Sieniawski  Włodzimierz Bogdanowicz  Andrzej Nowotnik  
Single crystal turbine blades of the first turbine stages were casted of nickel and cobalt superalloys. Beginning of their production requires significant capital expenditure. It also causes many technological difficulties. Thus, it is essential to have suitable set of casting equipments, vacuum furnaces for the heat treatment and last but not least all the processing know-how. Therefore, only a few foundries are capable to manufacture such turbine blades. Mass production of these single crystal parts of an aircraft engines so far has not been implemented in Poland. The studies performed allow to realize a production technology for single crystal turbine blades casting in Research and Development Laboratory for Aerospace Materials of Rzeszów University of Technology. In practice, precise single crystal casts are obtained via directional crystallization with the use of a block starter and spiral grains selector in a ceramic mould. In the process of monocrystallization the ceramic mould is withdrawn from the heating zone of the furnace to grow the blade. The grains in the cast&#8217;s starter grow in a columnar way against their spiral selector. Only one grain survives during competitive growth in the spiral grain selector. The phenomenon of grains growth &#8216;competition&#8217; is the basis for this process [1÷3]. A single crystal grain nucleus growing from the spiral selectors is the beginning of the single crystal crystallisation consisting in dendrites growth in three orthogonal crystallographic orientations [001]. The direction of [001] axis is parallel to single crystal&#8217;s growth axis [4÷10]. Intensive examinations of quality assessment methods were carried out in recent years for single crystal casts of a second generation[...]
 
Influence of sintering temperature on morphology of dense bioceramics based on hydroxyapatite derived from porcine bones
 
Anna Maria Janus  ROMAN MAJOR  MAREK FARYNA  
Hydroxyapatite (HAp - Ca10(PO4)6(OH)2) is the major constituent of mineral phase of human bone. It characterizes itself with high biocompatibility and has been used in medicine and stomatology for more than 20 years [1]. Hydroxyapatite can be obtained either by synthesis or by extraction from natural sources. Commercially available hydroxyapatite materials are listed in Table 1. Hydroxyapatite derived from porcine bones has not been commercialized yet, thus its development seems to be an attractive field of research. Biocompatibility of hydroxyapatite of porcine origin has been proved under in vitro and in vivo conditions [2, 3]. Heat treatment significantly influences chemical composition of the regarded hydroxyapatite derived from the animal bone. Such observation is proved by the other investigators [4, 5]. The information, found in literature and concerning influence of the sintering conditions on the dense bioceramics biocompatibility, however, do not cover all possible sintering conditions [5÷8]. The aim of the presented work was to examine the influence of the temperature of sintering process on the hydroxyapatite morphology. The properties of the investigated materials were afterwards subject of in vitro biocompatibility investigation. MATERIALS AND METHODS Hydroxyapatite of porcine origin was obtained from long porcine bones. Preparation procedure comprised bones boiling in distilled water for 24 h, mechanical removal of tissue and spongy parts residues, leaching out of organic matter with 4 M sodium hydroxide solution during 48 h at 100°C, rinsing with distilled water in order to remove NaOH, drying at 120°C to constant mass, milling, sieving and calcination at 450°C in atmosphere of air for complete removal of organic matter. As reference material HA BIOCER synthetic hydroxyapatite from Chema-Elektromet (Pola[...]
 
Influence of Sn, Fe and Ag addition on amorphization and thermal stability of mechanically alloyed CuTiZrNi alloys
 
DARIUSZ OLESZA K  SYLWIA DĄBROWSKA  TADEUSZ KULI K  
There have been many works on the development of new alloy systems showing enhanced glass forming ability, enabling the formation of bulk metallic glasses (BMG). Over the past decade, BMGs have gained considerable attention due to their properties (high yield strength, hardness and elastic strain limit, relatively high fracture toughness, fatigue resistance and corrosion resistance) and potential as new structural materials [1÷3]. Nowadays Cu based bulk metallic glasses are considered as potential engineering materials due to their good mechanical properties [4]. Various Cu based alloys have been reported to show the enhanced glass forming ability, enabling the preparation of bulk alloys by conventional casting methods [5]. These alloys usually belong to the CuTiZrNi system, sometimes Hf, Al or Y are also added. Recently, the influence of Fe, Si, Pb and Sn addition on the glass forming ability and crystallization of CuTiZrNi BMGs has been studied [6]. Another possibility of fabrication of bulk amorphous alloys is consolidation of amorphous powders obtained by melt atomisation or by mechanical alloying technique. Hot pressing, extrusion or spark plasma sintering of amorphous powders in the temperature range between glass transition temperature and onset crystallization temperature allow the fabrication of bulk amorphous samples. There are few reports only on the mechanical alloying of the CuTiZrNi powder mixtures [7÷9], showing the amorphization possibility in this system. The starting point for many studies is Cu47Ti34Zr11Ni8 alloy elaborated by W. L. Johnson [10]. In the present work, the influence of chemical composition on the amorphization and thermal stability of mechanically alloyed CuTiZrNi elemental powder mixtures was studied. The basic Cu47Ti34Zr11Ni8 composition was modified by replacing Ni by Sn and replacing Zr by Ag [...]
 
Influence of strain rate and deformation temperature on the microstructure of Inconel X750 superalloy
 
Andrzej Nowotnik  Jan Sieniawski  Grażyna Mrówka-Nowotnik  Arkadiusz Onyszko  
A fundamental feature of plastic deformation is the homogeneity of strain distribution. It is commonly accepted that at low temperatures and high strains, flow localization may develop and affect the material ductility. On the other hand, hot-deformation at intermediate temperatures may also result in localized plastic flow and non- -homogenous deformation. Flow localization, as a result of substructure instability and collective motion of a large number of dislocations characterizes coarse slip or shear banding, Luders bands and the Portevin-LeChatelier effect. Kink bands and mechanical twins may also be considered as a individual form of flow localization. Coarse slip is usually used to describe the localized flow within individual grains, whereas shear bands traverse many grains very often without any significant relation to the position of easy glide systems plane. In pure metals and single phase alloys, shear bands have been found to be preferential sites for the nucleation of both static and dynamic recrystallization. It is widely believed that in age hardenable alloys, shear bands and dislocation substructure produce preferred sites for nucleation of precipitates, thus enhancing the nucleation. These same features also are believed to enhance the particle growth rate during hot deformation as a result of higher vacancy concentration produced by intensive straining as well as increased dislocation pipe diffusion. The study of processes which are associated with dynamic aging of supersaturated solid solution during hot deformation may turn out to be very complicated because of the mutual interaction between dynamic precipitation and the structure resulting from the deformation process. The contribution of flow localization to the strain hardening or flow softening and the flow stress-strain behaviour during hot deformation of precipitation hardenable alloys is still a subject of extensive research. The interaction between [...]
 
Kinetics of phase transformations during tempering of tool steels of a different chromium content
 
JERZY PACYNA  PIOTR BAŁA  JANUSZ KRAWCZYK  
During heating as-quenched martensite, the tempering (of unalloyed, medium and high carbon steels) takes place in three distinct but overlapping stages: precipitation of &#949; carbide, transformation of the retained austenite into lower bainite and precipitation of cementite. In steels containing alloying elements contributing to an effect of secondary hardening (V, Mo, W) a fourth stage (transformation) occurs: precipitation of MC and M2C-type alloy carbides, that nucleate independently [1÷4]. The first transformation occurs in the temperature range of 100÷200°C. Metastable &#949; carbide (Fe2.4C) with hexagonal crystal structure precipitates from the supersaturated martensite [5÷8]. Precipitation of highly dispersed &#949; carbide is believed to enhance strengthening in steel [2, 4]. The second transformation takes place during tempering in the temperature range of 200÷320°C and this is a transformation of the retained austenite. As the result of this transformation, a non-homogeneous mixture consisting of supersaturated ferrite and cementite, i.e. lower bainite forms [1, 2, 4]. Cementite is formed during the third transformation occurring during tempering in the temperature range of 200÷420°C. This results in further decarbonization of the matrix and dissolution of metastable &#949; carbides allowing for the recovery of the steel matrix [4, 7]. The mechanism of the nucleation of cementite is, however, not fully understood yet. According to Ref. [4] precipitating cementite nucleates independently or in situ on &#949; carbide particles. Whereas according to Ref. [5] cementite nucleates independently, mainly on grain boundaries of former austenite or on subgrain boundaries of the newly formed cell structure. Above 400°C diffusion of alloying elements such as V, Mo and W takes place. Then, the cementite gradually dissolves to make the nucleation of MC and M2C carbides coherent with the alloy matrix possible. This leads to an [...]
 
Kinetics of phase transformations of undercooled austenite in tool steels of a different chromium content
 
JANUSZ KRAWCZYK  JERZY PACYNA  PIOTR BAŁA  TERESA SKRZYPEK  ADAM KOKOSZA  
The chemical composition and microstructure of hypereutectoid steel influences its most important properties, such as: heat fatigue resistance, resistance to oxidation and mechanical properties [1], which in consequence determines functionality qualities of tools produced of this steel. Depending on the material used certain surface defects can generate, which eliminate tools from further exploitation [2]. A retained austenite can also play a significant role. Retained austenite being a metastable phase, appears to be the main reason for spalling of indigenous rolls [2]. Hypereutectoid cementite and changes in a matrix influence tribological properties [3, 4]. Spectroscopic methods can be used for the analysis of such changes, e.g. for characteristics of cementite precipitates [5]. Possibilities of applying hypereutectoid steels for tools production can also be determined by means of the CCT diagrams. E.g. the effect of hot deformation on phase transformation kinetics of undercooled austenite was considered in the reference [6]. The knowledge mentioned above, allows to design hypereutectoid steels (e.g. of a bainitic matrix) or to estimate possible effects when elements made of this steel (intended to be of a pearlitic matrix) enter into a bainitic zone at cooling [7]. The chemical composition analysis of this type of steel requires also a broad estimation of alloy carbides being formed in it [8], including the role of a continuous network of secondary cementite [9, 10]. Thus, a carbon content in those steels can be optimised with regard to the mechanical properties [11] and its influence on the microstructure of a steel matrix can be determined [12]. An interlamellar distance in pearlite substantially influences functional qualities of steel [13]. The austenitizing temperature [14] and the cooling rate [15] are decisive when considering the steel microstructure. Vanadium carbides, especially their influence on grain sizes, are[...]
 
Laser welding of DP steel - characterization of microstructure of steel and welded joint
 
Marek Stanisław WĘGLOWSKI  Sebastian STANO  Władysław OSUCH  Grzegorz MICHTA  
Increasing demands on weight reduction, safety and cost have led to a rapid development in car body engineering. A number of new materials are being investigated, especially steels of greater strength. Advanced High Strength Steels (AHSS) are being intensively explored by the automotive industry [1]. The combination of excellent structural properties and good formability makes AHSS such as DP (Dual Phase) steel attractive candidates for light-weight vehicles. Dual Phase steels, so called because they consist essentially of a dispersion of martensite in a ferrite matrix, are produced by intercritically annealing and cooling with rate appropriate to achieve the desired structure [2]. Apart from the chemical composition, the microstructure and mechanical properties from the practical point of view the most important property is weldability of automotive steels [3]. Traditionally, resistance welding and fusion welding have been used in the automotive industry. However, the most prospective welding process in this branch of industry is laser welding. The main advantages of laser welding are small distortions of the sheets caused by a small width of HAZ, high welding speed and flexibility of this process [3]. Kang et al. [4] have shown results of laser welding of DP 600 steel 1.4 mm in thickness. They have performed hardness measurements, microstructure examination, mechanical properties and formability tests. The results have shown that the maximum hardness in the heat affected zone (HAZ) exceeds 350 HV. The maximum hardness was mainly the result of bainite, ferrite and small amounts of martensite phase. In another studies [5], High Strength Low Alloy (HSLA) and DP980 (980 MPa) sheet steels, 1.2 mm in thickness, were welded with a 4 kW diode laser. For the DP steel weld formability was much lower than that of corresponding base metal, due to the formation of soft zones in the outer region of the HAZ of the welds. Results of DP 600 [...]
 
Laws of substructure anisotropy of textured metal materials
 
YURIY PERLOVICH  MARGARITA ISAENKOVA  VLADIMIR FESENKO  
Any metal material with a developed crystallographic texture shows the substructure anisotropy, i.e. different values of substructure parameters, measured along different directions. Usually such measurements are realizable by methods of X-ray diffractometry. Among substructure parameters, influencing the pattern of X-ray diffraction and, in particular, profiles of X-ray lines, there are interplanar spacings of the crystalline lattice, coherent domain size, lattice distortion, dislocation density. However, it is evident for specialists in X-ray analysis, that the above simplest definition of substructure anisotropy needs an additional clarification concerning the term &#8220;different directions". Since all X-ray measurements of substructure parameters use concrete X-ray lines (hkl), which are reflections from the corresponding crystallographic planes {hkl}, these measurements characterize the substructure as it is seen only along crystallographic axes <hkl>. Therefore, the definition of substructure anisotropy as applied to a textured polycrystal means, that we compare substructure parameters, measured along crystallographic axes of the same type <hkl> parallel to different directions (&#968;, &#966;) in the system of external coordinates. In the particular case these axes can belong to the same grain, then measured substructure parameters characterize the substructure anisotropy, developed in grains with a concrete orientation under deformation. When considering the substructure anisotropy of material, references to orientations (&#968;, &#966;)i of axis <hkl> are sufficient for its characterization, whereas the description of substructure non-uniformity of textured material requires to split the distribution of axes <hkl> into sets, belonging to grains with different orientations, characterized with Euler angles. At the same time the concept of substructure anisotropy is close to the concept of substructure non-uniformity in [...]
 
Low cycle fatigue behavior and microstructure of 3rd generation TiAl-based alloy
 
Grzegorz Cempura  Heinz-Josef Penkalla  Florian Schubert  Aleksandra Czyrska-Filemonowicz  
Continuous effort over the last decades is emphasized to develop structural materials that could supply appropriate mechanical properties at the highest possible temperatures. The increase of operational temperature is particularly important to achieve higher thermal efficiency, improvement of acceleration, thrust to weight ratio and lower fuel usage of modern jet engines, stationary gas turbines and other high temperature machines[1]. For a gas turbine, increase of 150°C in the turbine entry, could improve its efficiency of about 5% [2]. In power engineering and aeronautics Ti based alloys are used among others for compressor discs and fan blades. Ti fan blades are used in the low-pressure compressor but application of conventional Ti alloys limits temperature in the high pressure compressor up to about 550°C because their insufficient oxidation resistance [3, 4]. There is a need to develop the lightweight alloys which could be used at the temperatures higher than 600°C. Intermetallic bases alloys have a great potential for application as a structural material for HT applications, because of low density, high strength and good oxidation resistance. Their strongly ordered structure and directional bonding is manifested by their high melting point and Young modulus. However, a large number of ordered phases are too brittle for structural applications. Ti-Al intermetallic based alloys, especially third generation with the density of about 4 g/cm3 have very promising mechanical properties. The TiAl alloys may be processed in a similar way like other metals and alloys: with use of conventional manufacturing processes like ingot melting, casting, precision casting, forging, and machining on almost conventional equipment [5]. Third generation of TiAl alloys was developed to be the alternative to nickel-based superalloys in the temperature range up to about 700°C. Due to addition of 5÷10 at. % Nb those alloys have strength and weigh[...]
 
Low friction MoS2(Ti, W) coatings deposited by magnetron sputtering
 
Wojciech Paw lak  Bogdan Wendler  Piotr Nolbrzak  Marcin Makówka  Katarzyna Włodarczyk  Adam Rylski  
Self-lubrication of graphite or of some metal dichalcogenides (such as MoS2 or WS2) is a very desired property in many technical applications. The phenomenon of self-lubrication in these materials is a result of a very big anisotropy of the crystallographic structure of these materials. In case of the MoS2-based material the basal planes of MoS2 elementary cells consist of hexagonal, strong covalent- -bonded planes of metal atoms between two planes of sulfur atoms. In a perpendicular direction exist weak Van der Waals interactions between the neighbouring planes built from sulfur atoms, what brings about a low shear strength [1, 2]. Limitation of use of grease and oils in friction couples becomes more and more important due to difficulties with smearing at high loads and to high costs of recycling of used oils. Nowadays, coatings&#8217; engineering is able to tailor the most outward areas of mating machine elements to working conditions. Coatings based on MoS2 have been largely used in numerous applications, such as, for example, ceramic tools for dry machining of stainless steel [3÷6], inserts for dry high speed milling of steel and grey cast iron [7, 8], ejector pins used for plastic moulds [4], punches for piercing and fine blanking of stainless steel [6], in a variety of engine components such as fuel injection systems, tappets, pistons, piston rings and bearings [5] and recently also as coatings for gears [9, 10] or for elements of friction simulator working in real space environment in a lunar orbiter [11]. On the other hand, pure MoS2 coatings exhibit relatively high wear during sliding in humid atmospheres or temperatures higher than 400÷500°C due to heavy oxidation [2]. Many attempts have been made to extend the range of convenient working conditions. Firstly, by incorporating different metals atoms into MoS2 matrix, as, for example: Au, Ni, Pb, Ti, Ta, Cr, Ce, Re, Mo, Cr, Zr, W, Si [2, 12÷14]. Secondly, by using comp[...]
 
Low temperature deformation twinning in channel-die compressed aluminium single crystals evidenced by Acoustic Emission
 
Zdzisław Jasieński  Andrzej Pawełek  Andrzej Piątkowski  
It is commonly believed that twinning is the most efficient source of acoustic emission [1÷5] due to fast release of great amount of elastic energy. It is connected with the fact, that the velocity of twinning dislocations is higher from this of slip dislocations [4], which results in the increase of contribution of accelerating effects in the recorded AE impulses. Very often acoustic emission induced by twinning contains also an audible range. Hence, more or less loud characteristic knocks during deformation can be heard. One of the first AE investigations concerned the tensile test of titanium and its alloys [1], in which it was established, that the AE activity in Ti was bound with twinning from the beginning, while in Ti alloys the AE impulses from twinning appeared after a high degree of deformation. During compression of the &#947;-TiAl alloy, AE sources were identified as generally coming from slip, twinning and the appearance and development of microcracks. It was reported that &#8220;the detailed mechanisms by which moving dislocations create elastic waves are not fully understood" [3]. Moreover, the problem of twinning in Al has still remained controversial. In available literature authors did not find any data on this subject. It is believed quite commonly, that at least in simple uniaxial strain state - like in a tensile test - twins do not appear in Al. The aim of this work is to demonstrate, that there are numerous proofs that in a complex strain state, which occurs in the channel die compression of single Al crystals at temperature of liquid nitrogen the twinning processes do occur. MATERI ALS AND MET HODS The single crystals of Al and Ag (for comparison) were produced with the Bridgman method, of which samples of dimensions 10×10×10 mm of orientations {112}<111> and {531}<231> for Al and {112}<111> for Ag were cut out. The single crystals were subjected to tests of channel-die compression at temperature of liq[...]
 
Magnetic properties of Fe60Co5Zr10Mo5B20 bulk amorphous and partially crystallized soft magnetic alloy
 
MARCIN NABIAŁEK  MICHAŁ SZOTA  MARCIN DOSPIAL  JAROSŁAW JĘDRYKA  
Currently the search for materials with interesting properties is the subject of considerable attention of electro-machine industry. The bulk amorphous and nanocrystalline materials (obtained on their base, across controlled thermal crystallization process) can be rate to such a group of alloys. Production of bulk amorphous alloys is complicated and requires following few principles during alloy composition. Such a principles were posted by Inoue et. al [1, 2]. Inoue showed that alloy composition should consist at least four types of atoms, base atoms radius should to vary by 12% and heat of mixing among basic components should have negative value. Multi-component alloy composition lead to complicated microstructure, where short range exchange interaction are energetically more valuable then long range one. Variation in radius of base atoms leads to large density, which results from higher compaction of atoms in liquid then in crystalline state. Furthermore, transition from liquid into crystalline state is connected with growth of volume of the sample during solidification process. Negative heat of mixing causes growth of energetic barrier between liquid and solid state during solidification process. Increase of smelted material viscosity lead to decrease of atom movement in alloy volume and block crystallization process. Some of the bulk amorphous alloys based on iron or cobalt display good soft magnetic properties [3, 4]. Improvement of these features can be achieved by nanocrystalization [5, 6]. Several methods like classical crystallization based on long-lasting (under crystallization temperature) heat treatment [7÷9] or unconventional based on impulse (over crystallization temperature) heat treatment [10] of a bulk amorphous alloys lead to nanocrystallization. These methods are expensive and time-consuming. Production of as cast bulk nanocrystalline alloy can be viable alternative. In this work the properties of Fe60Co5Zr1[...]
 
Manufacturing powder bearings modified with solid lubricant nanoparticles for high temperature applications
 
HANNA WIŚ niewska-WEINERT  VOL F Leshchynsky  MI KHAIL IGNATIEV  TOMASZ RYBAK  
With the rapid development of industries and advanced technologies, more and more mechanical devices are required to work in high temperature, for example, the various devices used in aviation and electrical industries, the engine sliding components, and the mechanical devices in the nuclear industry. The conventional grease lubricating systems used in the high temperature do not meet the present requirements, so it is urgent to develop materials with excellent self-lubricating property from the room temperature to about 1000°C. Sliney and co-workers prepared several high temperature self-lubricating sintered materials [1÷4], three typical materials among which are PS101 (30% Ni-Cr, 30% Ag, 25% CaF, 15% glass), PS200 (80% Ni-Co-Cr3C2, 10% Ag, 10% BaF2/CaF2), and PS300(80% Ni-Cr-Cr2O3, 10% Ag, 10% BaF2/CaF2). These materials show good self-lubricating properties (friction coefficient about 0.1÷0.3) in a wide temperature range. New advanced materials are generally considered as essential for the development of novel solid lubricants giving access to high temperature applications [5]. The nanoparticle solid lubricant materials have been identified as being of potentially outmost importance for many industrial high temperature applications, as a consequence of their original two-dimensional lamellar structure and superior friction properties. These materials have been identified as strong candidates for high temperature tribology applications because of their atomic-scale structure involving strong covalent bonds and non-compact space filling. Detailed analysis of nanoparticles mechanical behaviour during sliding is essential to gain understanding of the complex physical nature of these nanostructures during friction process. The shape, strength, fracture and interparticle friction properties of such nanostructures are of great importance. The nanoparticle ensemble behavior is believed to be identified by continuum mechanics metho[...]
 
Mechanical alloying of Astaloy CrL powders with silicon
 
Marek Hebda  Jan kazior  
It is well known that in the competition between wrought and Powder Metallurgy (PM) steels, sintered materials are at an extreme unbeneficial due to the deleterious effect of porosity on mechanical properties such as tensile strength, ductility and impact toughness. Furthermore, the increased alloy level in powder mixture is disadvantage due to their negative effect on compressibility. For this reason it is very important to try to explore non traditional strengthening mechanism for sintered steels [1]. Recently it was discover that bainitic-austenitic dual phase steels containing silicon are known to posses high toughness thanks to the presence of a finely dispersed retained austenite in a carbide free bainitic matrix. The absence of carbides in retained austenite is due to the effect of silicon on the bainitic transformation. Such a microstructure is expected to improve the mechanical properties of porous sintered steels. High strength bainitic steels have not been as successful in practice as quenched and tempered martensitic steels, because the coarse cementite particles in bainite are unbeneficial. However, the precipitation of cementite during bainitic transformation can be suppressed by alloying the steel with about 1.5 wt. % Si, which has very low solubility in cementite and greatly retards its growth from austenite [2]. The addition of silicon to steel enables the production of a distinctive microstructure consisting of a mixture of bainitic ferrite, carbon enriched retained austenite, and some martensite [3], thereby stabilizing it down to ambient temperature. The amount of retained austenite present in microstructure depends on the composition, cooling rate, austenite morphology and annealing temperature and time. The silicon suppresses the precipitation of brittle cementite, and hence should lead to an improvement in toughness. However, the full benefit of this carbide free bainitic microstructure has frequently no[...]
 
Mechanical and acoustic emission behavior in channel-die compressed Mg9Li alloys before and after treatment by HPT method
 
Andrzej Pawełek  Stanislav Kudela  Andrzej Piątkowski  Zdzisaw Jasieński  Zbigniew Ranachowski  Stanislav Kudela  
The Mg-Li alloys and the composites based on these materials have been still attractive candidates for light and tough construction materials for the application in automobile (e.g. car engine housings), aviation and space industries. The alloys can occur in three different phase areas. The alloys containing up to 4 wt. % Li consist of &#945; phase of hexagonal lattice A3 (hcp), while these with above 12 wt. % Li are in the form of &#946; phase, which is cubic A2 (bcc). The alloys of Li content from 4 up to 12 wt. % are two-phase and occur as the mixture of &#945;+&#946; phases. The mechanical properties of the &#945; phase are worse than these of the &#946; phase, which reveals very good plasticity [1]. The methods of intensive deformation have recently been more frequently applied [2÷4] in order to obtain ultra fine-grained refinement which ensures high strength and plasticity as well as prospects for the superplastic flow of the material in conditions of relatively low temperatures [2]. The AE technique has been still helpful in the examinations of deformation mechanisms, particularly regarding the mentioned materials of ultra fine-grained (nonocrystalline) morphology obtained after processing with intensive strain methods [2, 3, 7, 8]. The aim of the research was to describe and explain the correlations between the proceeding of the generated AE signals and the mechanisms of plastic (or possible superplastic) deformation in the Mg-Li alloys subjected to compression tests in the channel-die before and after the application of HPT technique. EXPERI MENT AL MET HODS The Mg-9Li alloys were produced within the cooperation with the Institute of Materials and Machine Mechanics, Slovak Academy of Sciences, Bratislava, Slovakia. The material was obtained by melting magnesium and lithium of 99.99 and 99.5 % purity, respectively in a Ba[...]
 
Mechanical and tribological properties of electrodeposited Ni-Mo coatings
 
MARCIN kOT  EWA BEŁTOWSKA-LEHMAN  AGNIESZKA BIGOS  PAULINA INDYKA  JERZY MORGIEL  WIESŁAW RAKOWSKI  
Hard chromium coatings are widely used in aerospace, automotive, hydraulic and machinery industry to reduce friction, wear and corrosion. Electrodeposition is a frequently used technique to deposit such a coatings because is simple, low cost and low temperature. Main advantage is to possibility of relatively uniform deposition on large, complex shape elements. Nowadays hard chromium that dominates within this group coatings were characterize by good mechanical and corrosion resistance but the deposition process is toxic and carcinogenic. Many environmental friendly materials are proposed to replace electroplated chromium coatings, and one of them are nickel based alloys coatings - Ni-P [1], Ni-Mo [2], Ni-W [3] and nanocomposite coatings like Ni-P-Al2O3 [4], Ni-W-SiC [5]. Pure Ni coatings are not hard and wear resistant, but their properties could be significantly improved by alloying and reducing the grain size to nanocrystalline structure. It is reported that Ni-Mo deposits have a good corrosion resistance but there is a lack of tribological studies. For coating-substrate systems wear is not only determined by hardness as showed classical theories of friction [6]. Increase of hardness is usually associated with rise of stiffness and frequently cause change of deformation mechanisms from plastic to brittle fracture. Many studies indicate than wear depends on quotient of hardness H and modulus of elasticity E [7] which is called plasticity index. This value can be used to quantitatively assess the load that may be carried on by the coating in the elastic stress regime. Wear at the elastic state, when abrasive wear dominates is significantly lower than under plastic deformation. The value of the contact force that caused plastic deformation of the coating can be calculated from Hertz theory [8]: P R R pl E l ind = 0 68 3 &#8901; &#8901; 3 2 2 . &#960; (1) where Eind is the reduced modulus of elasticity of coating and the [...]
 
MgH2 and intermetallic hydride nanocomposites synthesized by mechanical ball milling
 
TOMASZ CZUJKO  ZBIGNIE W ZARAŃSKI  
One of the obstacles to the implementation of the Hydrogen Economy into automotive industry is a lack of viable hydrogen storage system. Relatively promising is hydrogen storage system based on solid state hydrides with high hydrogen capacities exceeding 6 wt. %. However, a number of high capacity hydrides have high desorption temperatures which are incompatible with the waste heat generated by an automotive PEM (Proton Exchange Membrane) fuel cell. The search for materials that match the DOE criteria for hydrogen storage materials to be used in automobile applications has been largely focused on hydride composites in the past ten years [1÷5]. Very recently, it has been shown [4, 5] that the hydrogen desorption temperature of the composite constituent with the higher desorption temperature in the systems, substantially decreases linearly with increasing volume fraction of the constituent having lower desorption temperature. In the present work the composite approach is applied to the MgH2 + FeTi and MgH2 + LaNi5 systems. The composites with various volume fractions of both constituents were processed by controlled reactive milling (CRM) in a magneto-mill (under hydrogen atmosphere). Hydrogen desorption was tested using a Differential Scanning Calorimeter (DSC) and Temperature Programmed Desorption (TPD) analysis. The aim of this work is to analyze the influence of intermetallic additives on magnesium hydrogen decomposition process in MgH2 + FeTi and MgH2 + LaNi5 composites. experimental As-received commercial MgH2 powder (Sigma-Aldrich; ~98 wt. % purity; the remaining Mg), LaNi5 (Alfa Aesar, hydrogen storage grade) and cast FeTi intermetallic powder, were mixed to MgH2 + X wt. % FeTi and MgH2 + X wt. % LaNi5 (where X = 10, 30 and 50) compositions. As a reference MgH2 without additives was used. The FeTi intermetallic powder was obtained by melting pre-compressed Fe and Ti powders mixture and grinding the obtained ingot. Gr[...]
 
MgH2 based composites with LiAlH4 and LiNH2 complex hydrides
 
ZBIGNIE W ZARAŃS KI  TOMASZ CZUJKO  Iwona MaLKA  
The investigation of materials that could match the requirements for hydrogen storage system to be used in automobile applications has been mostly focused on complex hydrides in the past few years. Especially, since the work of Chen et al. [1], Luo [2] and Vajo et al. [3] on mixtures of LiNH2/LiH, LiNH2/MgH2 and LiBH4/MgH2, there have been many publications dedicated to complex hydrides that are thermodynamically destabilized by ball milling with other hydrides [4÷7]. The advantage of such reactions is that the relatively large enthalpies of complex hydrides can be decreased by providing an alternate reaction pathway that liberates hydrogen. It has also been observed that new phases could be formed during the high-energy ball milling of different ratios of known hydrides [2, 3]. Very recently, it has been shown [4, 5] that the hydrogen desorption temperature of the composite constituent with the higher desorption temperature in the systems, substantially decreases linearly with increasing volume fraction of the constituent having lower desorption temperature. In the present work the composite approach is applied to the MgH2 + LiAlH4 and MgH2 + LiNH2 systems. The composites with various volume fractions of both constituents were processed by controlled mechanical milling (CMM) in a magneto-mill (under protective argon atmosphere). Hydrogen desorption was tested using a Differential Scanning Calorimeter (DSC) analysis. The aim of this work is to analyze the influence of intermetallic additives on magnesium hydrogen decomposition process in LiAlH4 and LiNH2 composites. experimental As-received commercial MgH2 powder (Sigma-Aldrich; ~98 wt. % purity; the rema[...]
 
Microstructural analysis of as-cast single-crystalline CMSX-4 gas turbine blade
 
Beata Dubiel  Wiktoria Ratuszek  Aleksandra Czyrska-Filemonowicz  
Turbine blades are critical components in both aircraft and stationary gas turbines. They must be capable to withstand extreme conditions of temperature and stress during operation. The demand for increase of the operating temperature above 1000°C resulted in a development of directionally solidified single crystal (SC) superalloys for gas turbine blades [1÷3]. Single crystal solidification was achieved by application of helical grain selector between the casting and chill plate, enabling selection of a single grain, which fills the whole mould by dendritic growth. Although such superalloys are called &#8220;single crystals", they consist of two phases: &#947; solid solution matrix and about 70% volume fraction of &#947;&#697; precipitates. Segregation of chemical elements, which occurs during solidification, leads to the differences in the microstructure inside dendrite arms and between them. Dendritic regions consist of &#947;&#697; precipitates surrounded by narrow &#947; channels, while interdendritic spaces contain coarse irregular &#947;-&#947;&#697; eutectic islands [3÷6]. Casting of turbine blades in single crystal form is very complicated and requires definition of optimum parameters of technological process. Beside the careful inspection of the presence of casting defects, the quality control of as-cast blades involves checking of the deviation from the desired crystallographic orientation, which should be less than 15° [1]. However, to check in more detail if the solidification parameters of the casting are properly chosen, the assessment of the microstructure in microand nanoscale should be performed. The present paper reports the results of the analysis of the crystallographic orientation and microstructure of trial casting of CMSX-4 single crystal gas turbine blade performed within the project on &#8220;Dire[...]
 
Microstructural evaluation of CMSX-4 superalloy single crystal castings of various geometry
 
Anna Szular  Arkadiusz Onyszko  Maciej Motyka  Zenon Lipiński  
The turbine blades and combustion chamber belong to critical parts of aircraft jet engines. They work under extreme conditions: very aggressive corrosion environment, high mechanical and thermal stresses. Therefore the creep resistance is very important criterion for selection of critical parts materials and methods of their production [1]. Advances in turbine blade manufacturing were mainly caused by implementation of directional crystallization in casting process. This method enabled obtaining columnar grains in castings, elongated in the main axis direction. This kind of microstructure with no transverse grain boundaries provides higher creep resistance of castings. It was found that much better properties characterize single crystal castings. Casting process of single crystal blades is analogous to casting process of blades having columnar grains. The difference is in the beginning of crystallization process - only one grain properly oriented is selected for further growth [2÷5]. The main parameters controlling single crystal casting quality are temperature gradient and withdrawal rate of mould (vw). Too high cooling rate causes crystallization of grains in front of interface between liquid and solid phases. Whereas too slow mould removal from the heating zone leads to excessive microstructural segregation and defects formation in castings. It is considered that higher temperature gradient (in the accepted range) contributes to improvement of casting quality. The most often applied values of temperature gradient are in the range of 3÷6.5°C/mm and withdrawal rate of about 5 mm/min [6÷12]. Microstructure of most nickel superalloys is mainly composed of gamma (&#947;) and gamma prime (&#947;&#8242;) phases. The &#947;&#8242; phase (Ni3(Al, Ti)) - primary strengthening phase - is coherent with the matrix - &#947; phase. The close match in matrix lattice parameter (~0÷1%) combined with the chemical compatibility allows the &#94[...]
 
Microstructure and hardness of magnetron sputtering (Cr, Si)N coatings with up to 30 at. % Si
 
Justyna Grzonka  Ryszard Mania  SŁA WOMIR ZIMO WSKI  Jerzy Morgiel  
TiN coatings extending the cutting tools lifetime were praised for their very good adhesion and hardness exceeding those of high speed steel or even cemented carbides [1, 2]. However, their limited high temperature resistance for oxidation during high speed machining turned interest toward those sandwiched with CrN or multi-layer coatings like TiN/VN or TiN/NbN [3, 4]. The hardness of the latter exceeds those characteristic for individual layers due to coherency strains, while vanadium or niobium nitrides prevent them from premature oxidation [3, 4]. In most cases the TiN is deposited first to gain advantage of its excellent adhesion to most steel substrates. Unfortunately the deposition process of multilayer coatings is a complicated one and in consequence rarely economically acceptable. Therefore, as an alternative, a nanocomposite crystalline-amorphous TiN/Si3N4 coatings were proposed by Veprek et al. [5]. The idea of nanocrystalline-amorphous composites is based on development of shear resistant nanocrystallites of transition-metal nitrides or carbides surrounded by amorphous nitride [5, 6]. The TiN/Si3N4 coatings obtained up to date show large scatter of hardness from ~20 to ~60 GPa being generally well below expectations [7÷11]. The CrN/Si3N4 coatings showed also only moderate hardness increase from 16 characteristic for CrN up to max. ~34 GPa [2]. Even as higher gains were expected from the nanocomposite model rising CrN based coating hardness up to the level characteristic for TiN seems interesting from practical point of view. The further development of these interesting nanocomposite coatings might be achieved only through simultaneous hardness measurements and detail experimental ver[...]
 
Microstructure and kinetics of intermetallic phases growth in Ag/In/Ag joint obtained as the result of diffusion soldering
 
Przemysław Skrzyniarz  Joanna Wojewoda-Budka  Robert Filipek  Paweł Zięba  
Environment protection and improving the quality of joints are two main bases of the present development of modern technologies of different materials joining. The environment protection trend came into being in the 1990&#8217;s in the USA and later it also spread over Europe and Japan. The main aim is working out soldering materials able to replace the Sn-Pb solders commonly used so far. This can be obtained by eliminating cadmium and lead which are the components of soft solder used in conventional soldering process. Additionally, RoHS 2002/95/EC directive of the European Parliament and Council of January 27, 2003 orders the member countries to limit the use of some hazardous substances in electrical and electronic equipment. Soon another directive was issued: WEEE 2002/96/EC - Waste Electrical and Electronic Equipment referring to the problem of the used up electrical and electronic equipment and its reusing, recycling, and other forms of recovery. It imposes the responsibility for storing and recycling hazardous substances on the manufactures. Hence, a lot of information concerning new methods of joining materials can be found in the literature. The electronic industry is a good example. Assembly line production of circuits of high integration scale with many units sensitive to high temperature and joined in a very short time enforces applying a special soldering process so that the solder area is as small as possible. Diffusion soldering meets such requirements. The joint made in this way takes up 6 times less space than in the case of conventional soldering and it can work at the temperatures higher than 350°C [1, 2], and it often shows mechanical and thermal stability at temperatures 2÷3 times higher than the joining temperature. Moreover, the surfaces to be joined do not require special preparation, which remarkably shortens the production time [3]. The example here could be circuits on the basis of SiC and semiconduct[...]
 
Microstructure and magnetic properties of the Cu-1% Co single crystal
 
Joanna Czub  BEATA DUBIEL  WALDEMAR Tokarz  ALEKSANDRA Czyrska-Filemonowicz  
The Cu-Co alloys has been found to be ideal candidates to study the giant magnetoresistance phenomenon (GMR), originally observed in thin magnetic films [1], that have focused great research interest. Such materials can be applied in micro-switching devices and detection heads in magnetic recording. The GMR phenomenon, a big change of the electrical resistivity caused by external magnetic field, is attributed to the spin-dependent scattering that takes place in the interfaces between magnetic particles and the metallic matrix in which they are embedded [2÷5]. The films made of the alloys based on non-magnetic elements (Cu, Ag) with precipitated ferromagnetic particles (Fe, Co) appear to posses GMR properties [6, 7]. However, besides the GMR phenomenon, such alloys provide a unique opportunity to study their basic properties, such their microstructures and magnetic properties. The purpose of this work is to present the results of the transmission electron microscopy (TEM) analysis which provides the real size distribution of Co particles in the Cu-1% Co single crystal. We report also the results of the magnetic measurements in connection with the real distribution of Co particles which allows us to explain the relation between the size of the Co particle and the magnetic properties. EXPERIMENTAL DETAILS In the present study the Cu-1% Co (wt. %) single crystal of the origin reported in [8] was used. The investigations were performed on a sample aged at 600°C for 24 hours. The samples for TEM and magnetic investigations were cut out from the single crystal. TEM investigations were performed using a JEOL JEM-2010 ARP microscope on thin foils prepared by the electropolishing method. Image analyses were carried out using the ImageJ software. The magnetic properties were measured using a standard vibrating sample magnetometer in the external[...]
 
Microstructure and mechanical properties of friction stir welded Sc-modified Al-Zn-Mg-Cu alloy
 
Mateusz Kopyściański  Stanisław Dymek  Carter Hamilton  Marek Blicha rski  
Conventional Al-Zn-Mg-Cu (7000 series) alloys are widely used in aerospace applications due to their favorable mechanical properties. Their strength, the highest among all aluminum alloys, arises from a high density of minute precipitates produced upon aging. However, the mechanical properties degrade above 150°C due to the coarsening and/or dissolution of the strengthening phases within the microstructure. There is currently strong interest in adding zirconium and scandium to Al alloys in order to improve the overall performance of these alloys [1, 2]. Additions of scandium and zirconium to these alloys can stabilize the microstructure at elevated temperatures and can augment the mechanical properties through the formation of fine, secondary strengthening phases such as Al3(Sc, Zr) [3, 4]. Addition of Zr together with Sc improves the effectiveness of Sc as an inhibitor of recrystallization and increases the stability of the alloy during prolonged exposure to elevated temperatures [5]. What is more, the addition of Zr reduces the susceptibility of the Al3Sc precipitates to coarsening. Because the nanometer-sized Al3(Sc, Zr) particles stabilize the microstructure in elevated temperatures, the potential for enhanced properties following joining operations, such as friction stir welding (FSW), arises. Friction stir welded joints display excellent mechanical properties when compared to conventional fusion welds, and as such, the aerospace industry is embracing the FSW technology and implementing its capabilities into their manufacturing sectors [6]. Over the last fifteen years, numerous investigations have sought to characterize the principles of FSW and to model the microstructural evolution [7÷12]. The current status of FSW research pertaining to aluminum alloys has been recently well summarized by Threadgill et al. [13]. The following paper contains introductory results on the characterization of microstructure and mechanical pr[...]
 
Microstructure and mechanical properties of model Al – Li alloys treated by SPD
 
Bogusława Adamczyk-Cieśla k  Jarosław Mizera  Krzysztof Jan Kurzydłowski  
Several commercial aluminum alloys are targeted to be advanced materials for aerospace technology due to their low density, high strength and high elastic modulus, as well as excellent fatigue properties. Since the reduction of density is one of the main requirements of modern materials used in aerospace applications, the aluminium- -lithium alloys became more attractive than conventional aluminium alloys [1÷3]. Studies on Al-Li alloys intended for aerospace applications have long been carried out, and numerous papers on this subject have been published [4, 5]. Several commercial aluminium alloys have been designed to take advantage of the attributes of lithium, which is the only alloying element that increases the strength and modulus while decreasing the density of the alloy. However, the existing commercial alloys containing lithium were designed to be relatively strong, so that they also contain the usual alloying elements that ensure precipitation strengthening [6÷8]. Therefore, although the microstructure and mechanical properties of Al-Li alloys have been extensively studied before, they have still been a subject of importance in the recent years. This is connected with new properties of the materials subjected to severe plastic deformation (SPD) and with their commercial applications. The major advantage of SPD techniques is their ability to produce micrometer size subgrains within the originally coarse grains of materials and alloys [9÷12]. In the present work the evolution of microstructure and mechanical properties of three aluminum-lithium alloys were examined. The materials with an ultra fine structure produced by hydrostatic extrusion were compared with these materials in the initial state. ma [...]
 
Microstructure and mechanical properties of the Cu/SnAuCu/Cu joints
 
Joanna Wojewoda-Budka  Anna Sypień  Anna Wierzbicka-Miernik  Andrzej Piątkowski  Paweł Zięba  
The European Union regulations forced the manufactures to limit the use of certain hazardous substances such as cadmium and lead in the electrical and electronic equipment and also make them responsible for its storage and recycling [1, 2]. In a consequence the lead-free interconnection technology is one of the most active branches of the nowadays materials science. PbSn replecements are mainly the tin alloys, among which a special class are those consisted of tin and noble metals such as copper, silver and gold. They are possesing two characteristic features - the high melting point and high concenteration of Sn compared to that of eutectic PbSn. Moreover, the composition of the lead-free solders can be described as eutectic or near-eutectic, which ensures the best manufacturability. The microstructure of these solders is a mixture of tin and the intermetallic phase (IP). Since both mechanical and electrical properties of the tin are anisothropic they are also anisothropic in the case of eutectic solders. Therefore, the intermetallics may take a form of the inhomogenous structures (for example Ag3Sn in the shape large plate-like crystals). To avoid of such IP creation the concentartion of silver in SnAg solder should be less than 3% wt. and copper should not go over than 0.7% wt. in SnCu solders. In the case of SnAu solders gold must not exceed the value of 5% wt. otherwise it leads to the formation of AuSn4 phase which causes britlle &#8220;cold" joint. Ternary solders are mainly SnAgCu solders (SAC) where the amounts of silver and copper (corresponding to the eutectic composition) are 3.5&#177;0.3 and 0.9&#177;0.2 (wt. %), respectively [3÷5]. Other ternary solder is SnAuCu alloy which may be used as a joining material for the joints in so-called noble electronics. They are applied in devices with the highest degree of reliability, such as biomedical devices. It should be noted that such products after their exploitation und[...]
 
Microstructure and properties of ball milled and hot compacted powder of 7055 aluminium alloy
 
Lidia Lityńska-Dobrzyńska  Jan Dutkiewicz  Wojciech Maziarz  Anna Góral  Łukasz Rogal  Adam Kanciruk  
7xxx series (Al-Zn-Mg-Cu) aluminum alloys are widely used in the aircraft industry due to their low density, high strength and good workability [1, 2]. Their strengthening increases with the concentration of Zn and is associated with higher density of very fine precipitates of metastable &#951;&#8242;-phase enriched with Zn and Mg. The high solute (about 8 wt. % of Zn) alloy designated AA 7055 (ALCOA) evokes the highest strength aluminium alloys produced by ingot metallurgy and is applied as upper wing skin materials in commercial aircraft [3]. The 7055 composition processed using the T77 temper provides a microstructure at and near grain boundaries that is resistant to both intergranular fracture and interglanular corrosion. Aluminium based materials produced by powder metallurgy (PM) processing offer a number of interesting opportunities for high strength applications. Powder metallurgy enables to fabricate high quality parts close to final dimensions with refined microstructure as compared with these produced by the conventional ingot metallurgy [4, 5]. The ball milling applied before the compaction allows obtaining a very fine microstructure and the extension of the solid solubility limits of the elements added to the alloy [6]. It results in improved mechanical and corrosion properties of the compacted products. PM technology provides more homogenous distribution of the precipitates and reduces the particle size that makes corrosion more uniform [7]. The aim of the present investigation was to study the effect of ball milling and hot pressing on the microstructure and properties of milled and compacted 7055 aluminium alloy powder. Exp erimental details The mixtures of elemental powders of aluminum, zinc, magnesium, copper and zirconium were used as starting materials to yield (wt. %) Al - 8% Zn - 2% - Mg - 2.3% Cu - 0.2% Zr compositions corresponding to 7055 commercial aluminium alloy. The ball milling of the powder was [...]
 
Microstructure and properties of laser remelted iron base amorphous coatings
 
JAN KUSIŃSKI  SłAWOMIR KĄC  GRZEGORZ KUSISKI  
[...]
 
Microstructure investigation of thin films SnO2 produced by pulsed laser deposition
 
Agnieszka Kopia  
The domain of gas concentration measurements - that was until recently important primarily in industrial technologies - has become important in atmosphere pollution research and in issues related directly to households (emission of toxic gasses, such as CO, NOx, CH4) [1]. A sensor for detecting and measuring gas concentrations should be characterized by appropriately high sensitivity, selectivity, a short response time and stability. These requirements led to a fast development of research on semiconductor-based gas sensors (Tab. 1). They meet the majority of these requirements and their appeal is additionally due to the simplicity of their structure and low costs of production. In series production, thick-layered sensors based on SnO2 pay the dominant role beside sensors based on sintered ceramic materials. The role of thin-layered technologies has been noticeably growing. Slow abandonment of thick-layered sensors is related to worse utility properties, compared to thin-layered sensors. The data available in the relevant literature show that high thickness of a gas-sensitive material is connected with big grain, which leads to reduction of the resistance of such material, but also to reduction of the active surface, i.e. of the sensitivity. Thick-layered sensors are also characterised by lower selectivity. In case of thin-layered sensors, surface conductivity - highly dependant on their gas environment - has a considerable share in the electric conductivity. In such sensors, the sensitivity and detection threshold are improved and the response time is reduced. Tin dioxide SnO2 is a material that is most often used in thinlayered[...]
 
Microstructure of Al-Cu thin film deposited by MOCVD
 
Bartosz Sarapata  Anna Zielińska-Lipiec  Constantin Vahlas  
The Al-Cu system is interesting not only because the alloys from this system are widely used in electronics. The copper rich part of the phase diagram contains phases which can be used to create CMAs (Complex Metallic Alloys). CMA is a class of the multinary alloys in which different phases are formed with crystal structures based on giant unit cells, containing hundreds, up to more than thousands atoms per cell. In these giant unit cells, atoms are arranged in the clusters which create huge complexity materials. Copper is a stabilizing agent for quasicrytalline ternary phases based on aluminum, where third element is a transition metal. The &#950;-Al3Cu4 phase is isomorphic to the &#981;-Al10Cu10Fe phase, which is known as a quasicrytaline phase. The &#947;-Al4Cu9 phase belongs to the family of the CMAs, however represents one of the simplest structures and contains &#8220;only" 52 atoms in unit cell [1, 2]. The complexity of the CMAs, offers unique combination of properties such as electrical and thermal resistance, enhanced optical properties with high temperature stability etc. The CMAs are found to exhibit excellent surface properties with respect to wetting, oxidation, corrosion and friction [3÷7]. Due to this fact it was interesting to investigate a possibility of creating the Al-Cu thin films by the means of Metal-Organic Chemical Vapor Deposition (MOCVD) from the Cu-rich part of the Al-Cu phase diagram. The work program involved processing of single Cu and Al coatings, followed by coatings from binary Al-Cu system, preferably the CMA Al43Cu57 phase. Here we present the results of the binary Al-Cu coatings deposition. The MOCVD is a method which allows to deposit metallic thin films at temperatures lower than classical CVD process. It uses metal-organic compounds as precursors for the elements such as Al [...]
 
Microstructure of Cu-Ag-P alloy layers plasma sprayed on AgSnO2 composite material
 
ADRIANA WRONA  MARCIN LIS  MIECZYSŁAW WOCH  MAŁGORZATA KAMIŃSKA  
Plasma spraying is a method currently widely used mainly in the aircraft, automotive, armaments industry for spreading metallic and ceramic layers on construction components working in the extreme mechanical and thermal conditions. During the plasma spraying the material in a form of powder or wire melted in plasma arc falls on the sprayed surface in a form of melted particles [1, 2]. Very high temperature of plasma stream, at the level of several thousand Celsius degrees, and the possibility to control power of the plasma torch in a wide range bring possibility for spraying virtually every kind of material, provided that it will not undergo process of evaporation or decomposition. Most often the technique is used to produce coatings of high-melting metals, oxide materials, nitrides, carbides and cermets. The basic advantage of sprayed coatings is their high resistance to abrasion, corrosion, thermal shocks and high-temperature creep resistance. The additional benefit is high rapidity and repeatability of the process as well as possibility to join materials of different melting points and high coherence of the binding layer-basic material. Current intensity and plasma arc voltage are the basic energy parameters of the spraying process, reflected by power of the plasma torch as well as by the type of plasma forming gazes and intensity of their flow which influence, among others, arc temperature. The properties of the layers produced in the process are also influenced by such geometric parameters as the distance between plasma torch nozzle and surface. When spraying with powder material also powder shape and morphology becomes important. Spherical powders are considered optimal for that application, as they have lower porosity, higher density and better flow rate than the powders of more developed surface (rough). In the study the plasma spraying technique was used for spreading a layer of a binder of Cu-Ag-P type on a composite [...]
 
Microstructure of the complex metallic β-Al3Mg2 phase
 
ANNA ZIELIŃSKA-LIPIE C  BEATA DUBIEL  ALEKS ANDRA CZYRSK A-FILEMONOWICZ  
Aluminium and magnesium are fairly simple metals with close packed lattices: Mg is hcp, whereas Al is fcc. The phase diagram of Al-Mg system contains intermetallic compounds. The mixture of Al/Mg ratio 3:2 atoms yields an extremely complex crystal structure. The &#946;-Al3Mg2, called also Samson phase (Fd-3mS: ICSD 57964, cF 1168), has cubic lattice with a = 28.242 &#197; and a unit cell containing 1168 atoms [1]. It is decorated by a number of large clusters of atoms, with near icosahedral atoms symmetry, leaving few atoms in between to fill-in space [2]. The Samson phase has hardness about 350 HV, Young&#8217;s modulus 68 GPa and low density 2.3 g/cm3. This phase is very brittle at room temperature (fracture toughness K1c is below 0.5 MPa&#8901;m1/2). Under compressive stress and temperatures higher than 250°C, &#946;-phase become plastic [3]. Comparison with Al shows the best compromise between strength and plastic deformation - strength 3 times higher than pure Al and plastic strain of about 40%. It means that application fields for this phase are in aeronautic and automotive industry. Different stability range of the &#946;-Al3Mg2 in Al-Mg phase diagram is proposed in literature [4, 5]. According to the phase diagram published by Murray [4], the &#946;-phase has a congruent point at 451°C and 38.5% Mg. The stability range of this phase extends from 38.5 up to 40.3% Mg in room temperature. On the Al-rich side, &#946;-Al3Mg2 coexists with the &#945;-phase (which is a solid solution of Mg in Al). On the Mg-rich side, the &#946;-phase coexists with &#947;-Al12Mg17 and with R-phase that forms below 350°C by [...]
 
Microstructure of the surface layer of a Ti6Al4V alloy and X5CrNi18-10 steel after laser treatment
 
Magdalena Rozmus -Górnikowska  Jan Kusiński  Marek Blicharski  Roman Major  
One of the relatively new method of mechanical surface treatments is Laser Shock Processing (LSP), which introduce strain hardening and compressive residual stresses into the treated surface layer. LSP uses laser pulses with pulse duration within the nanosecond range to modify the surface layers by means of high pressure [1, 2]. Laser parameters for LSP require power density &#8805;0.1 GW/cm2 and laser pulse duration &#8804;10-6 s. During the process, the laser beam is directed onto the surface of the material. The area to be treated is usually covered with two types of coatings: an absorbing coating, opaque to the laser beam, for example black paint, placed directly on the surface of the investigated material, and over this a transparent to the laser beam coating for example water [3, 4]. Figure 1 shows the scheme of the Laser Shock Processing. When the laser beam with sufficient intensity is directed onto the surface, it passes through the transparent layer and is absorbed by the black coating. The absorbing coating is vaporized and the vapor rapidly achieves very high temperatures at which electrons are ionized and a plasma plume is formed. The rapidly expanding plasma is confined on the surface of the metal by the layer of water, creating high pressures. This pressure propagating into the treated material as a shock wave, can induce microstructural changes and cause high increase of dislocation density and produce a high residual surface compressive stresses [5, 6]. The aim of this work was to investigate the effect of Laser Shock Processing on the microstructure and roughness of the surface layer of the Ti6Al4V titanium alloy and X5CrNi18-10 austenitic stainless steel. MATERIALS AND E[...]
 
Modelling of structure changes in continuous deformation conditions using cellular automata
 
Dariusz Kuc  JERZY GAWĄD  
Over last decade several successful applications of the cellular automata (CA) in simulation of DRX can be found in the literature, e.g. [1, 2]. The CA method leverages computational simplicity with reasonable ability to provide quantitative results. The paper is focused on application of multi-scale 2D CAFE method in hot forming. CAFE approach consists of the cellular automata model of microstructure development and the thermal-mechanical finite element (FE) code. Dynamic recrystallization phenomenon is taken into account in the 2D CA model which takes advantage of explicit representation of microstructure, including individual grains and grain boundaries. The pseudo-hexagonal neighbourhood is used as a context for state transition rule as described in [1]. Flow stress is the main material parameter in mechanical part of the FE and is calculated on the basis of the average dislocation density obtained from the CA model. Some previously published results that were achieved using this approach appear very encouraging [3, 4]. In the present study, austenitic X3CrNi18-9 steel was investigated. This specific material was selected to avoid phase transformation in the lower range of temperatures. The samples were subjected to the axisymmetrical hot compression test. Flow stress is the main material parameter in mechanical part of the FE and is calculated on the basis of average dislocation density obtained from the CA model. The results attained from the CAFE model were validated with the experimental data. CELLULAR AUTOMATA MODEL In general, any Cellular Automaton is described by a quadruplet: <L, S, F, N>, where L is the lattice (spatial ordering) of the cells, S is the state of the cell, F is the state transition rule governing evolution of the state in consecutive time steps and N is a definition of the neighbourhood describing the range of the local interactions between the cells. In the current work the CA are used for modeli[...]
 
Modelling the effect of SiC mass fraction on crystallization of magnesium metal matrix composite; AZ91/SiC
 
Janusz Lelito  Paweł Żak  Józef Suchy  Witold Krajewski  Halina Krawiec  lind say gree r  pete r schumache r  amir shirzadi  kath arina habe r  paweł darłak  
Grain size is one of the most important parameter which determined mechanical properties. Knowing element properties the proper application regions for it can be chosen to achieve best mechanical properties and performance. Nowadays simulation software can be use to predict the element microstructure. Those programs base on micro-macro model of crystallization. The model consists of partial differential equations (PDEs) that described the nucleation rate, diffusion in the casting, casting cooling speed and every single grain growth rate. Often it is hard to find the theoretical value of the parameters that appear in those PDEs. It is possible to find them from experiment. The experimental data that after applying statistical methods let us find approximated values of the so-called &#8220;fitting parameters" in the mentioned models [1÷4]. AZ91 alloy analyzed in this study is hypereutectic alloy. The magnesium primary &#945;-Mg phase is dendritic. During crystallisation there appears eutectic reaction. In this study influence of eutectic is omitted because magnesium primary phase has most significant influence on mechanical properties of the casting. Experimental procedure Composite casting The AZ91 alloy was selected as the matrix for the composites. The chemical composition is shown in Table 1. The reinforcement particles are silicon carbide with an average diameter of 45 &#956;m. Composite specimen with 0, 1, 2, 3 and 4 wt. % of SiC particles were prepared using a liquid mixing and casting process. Processing of the magnesium composites consisted of mixing pre-heated SiC particles to 450°C with liquid magnesium melt stirring and mould casting. About 1.4 kg of composite melts was prepared in an electric resistance furnace using a steel crucible under a SF6/CO2 gas atmosphere. The molten AZ91 alloy was held at 700°C for 1 h. After putting SiC particles composite was stirred for 2 min, and then cast at 700°C into mould to produ[...]
 
Modelling the effect of SiC particle size on crystallization of magnesium metal matrix composite; AZ91/SiC
 
PAWEŁ Żak  Janusz LELITO  JÓZEF S. SUC HY  Witold Krajew ski  HAl ina Krawiec  Katharina Haberl  Peter Shumacher  Lindsay Greer  Amir Shirzadi  BEATA GRACZ  
Grain size is one of the most important structural characteristic that determining mechanical properties. Knowing element properties, the proper application regions for it can be chosen to achieve best mechanical properties and performance. Nowadays simulation software can be use to predict the element microstructure. Those programs base on micro-macro model of crystallization. The model consists of partial differential equations (PDEs) that describe the nucleation rate, diffusion in the casting, casting cooling speed and every single grain growth rate. Often it is hard to find the theoretical value of the parameters that appear in those PDEs. It is possible to find them from experiment. The experimental data after applying statistical methods let us find approximated values of the so-called &#8220;fitting parameters" in the mentioned models [1÷4]. AZ91 alloy analyzed in this study is hypereutectic alloy. The magnesium primary &#945;-Mg phase is dendritic. During crystallisation there appears eutectic reaction. In this study influence of eutectic is omitted because magnesium primary phase microstructure has most significant influence on mechanical properties of the casting. Model description In the mathematical model it is assumed that heat transfer is governed by Fourier-Kirchhoff (FK) equation: &#8706; &#8706;T = - + c q p cp div gradT &#964; &#961; &#961; 1 ( &#955; ) , (1) where: T, K - is temperature, &#964;, s - time; cp, J&#183;kg-1&#183;K-1 - specific heat, &#961;, kg&#183;m-3 - density, &#955;, W&#183;m-1&#183;K-1 - thermal conductivity, q = L(dfs/d&#964;), W&#183;kg-1 - heat of crystallization. During simulation the temperature change speed is calculated. Its value consists of two parts: one, that depends on the temperature gradient and second that is phase change effect. In this article there is an assumption that simulation runs in one element of the melt. With this assumption the gradient depend part of FK can [...]
 
Multilayer wear resistant hard coating of high temperature working tool steel obtained by vacuum-plasma DUPLEX technology
 
Witold Precht  Piotr Małek  
The advance surface engineering, especially surface chemical and structure modification, resulting in modern vacuum-plasma technology of hard and superhard, mulitcomponent, multilayer, gradient and nanocomposite coatings for tribological application. In this work DUPLEX technology, as one of many possible surface engineering methods for increasing life time of machine parts and coating tools, was used, also the influence of ion nitriding before coating on the tribological properties of the coating was investigated. In the literature we can found not enough bright investigation results, connected with influence of technological parameters, architecture and chemical composition on the tribological properties of coated tools especially for high pressure aluminium alloys casting form (Fig. 1). AIM Of THE WORK The purpose of this work was to investigate the influence of ion nitriding process before hard coating of high temperature working steel of the type X37CrMoV5-1 on they structure and tribological properties, for possibility to apply our technology also for high pressure aluminium alloys casting form or other forming tools. EXPERIMENTAL PROCEDURE The substrate specimens of high temperature working steel of the type X37CrMoV5-1 (dim 40×4 cm) after chemical and ion cleaning were coated by ARC PVD method in two different attachement in KUT and VTD Drezden (Fig. 2a÷c), using parameters showed in Table 1. For investigation of structure morphology, roughness, layer thickness, microhardness, friction and wear coefficients and adhesion following instruments were applied: -- for roughness [...]
 
Nanocrystallization of NiNb(ZrTi)Al metallic glasses
 
Tomasz Czeppe  
Bulk metallic glasses (BMG) are new class of engineering oriented materials [1]. Different compositions of Ni based Nb containing amorphous alloys like: NiNbTi, NiNbZr, NiNbTiZr, NiNbZrTiAl, NiNbTiZrCoCu, NiZrNbHfAl, NiZrTaNb, reveals high glass forming ability (GFA), high fracture strength and good corrosion resistance [2÷7]. Due to the small difference between heat of mixing of Nb and Zr and Ti, Ni based Nb containing glassy alloys may reveal good ductility [6]. A very uncommon, composition dependent property is high thermal stability of the amorphous phase in alloys containing Hf and Ta or Al [7, 8]. In the following paper the melt spun ribbons of composition Ni58Nbx(ZrTi)1-xAly, (x = 5, 10, 20, 25 at. %, y = 3, 7 at. %), were investigated. The alloys were studied from the point of view of the microstructure, crystallization mechanism, phase composition after crystallization and crystallization kinetics during continuous heating. The most often applied are methods of the determination of the kinetics parameters basing on the assumption of the constant transformation rate at the peak temperature in the DSC experiments, when at least three different heating rates must be used. These methods base on the Kissinger [9] and Ozawa [10] equations and let to determine activation energy of crystallization. Last time however also the Matusita [11, 12] method, basing on the transformation rate for one heating rate is quite often presented in papers. The method was originally invented and verified for the oxide glasses, while the crystallization process is much slower than in the case of metallic glasses. The method lets to verify if the activation energy is constant during the transformation as well as determine m parameter connected to the crystals growth dimensions. In the following paper the Matusita method was applied to determine the activation energy in case of the lower crystallization rate observed in amorphous alloys containin[...]
 
Nanomaterials: friends or foes?
 
Małgorzata Lewandowska  Agata Roguska  
Nanomaterials are usually defined as engineered materials which are built of structural elements (grains, layers, fibres, particles) with a size less than 100 nm in at least one dimension. Such a definition is relatively broad and include large-scale bulk materials with the structure controlled at nanoscale (nano-policrystalline materials, nanocomposites containing nanoparticles attached, incorporated or fixed into the matrix) as well as free nanoparticles (including nanowires, nanotubes, nanodots). In the most general and widely recognised classification, nanomaterials can be divided into the 1-D (nanotubes, nanowires, nanofibres), 2-D (nanolayers) and 3-D (bulk materials and nanopowders). It should be noted that in the scientific literature, different terms are used to indicate small-scale structured materials, including nanomaterials, nanostructured materials, nanoparticles, nanosized particles, engineered nanostructured materials etc. Nanomaterials have attracted significant scientific attention and have underwent considerable technological progress. The huge interest in nanomaterials has been motivated by the exceptional properties currently possessed and the perceived potential properties and performance of products produced from such materials. The market for nano-based products is increasing rapidly. Nanomaterials are already being used in sporting goods, tires, stain-resistant clothing, sunscreens, cosmetics, and electronics and will also be utilized increasingly in medicine for diagnosis, imaging and drug delivery. The list of their potential applications is growing rapidly and one should expect that the same applies to the population exposed to interactions with nanomaterials. However, it should be noted that although research and development programmes on nanomaterials have been carried out in a number of institutions worldwide, their focus was mainly on technology, assessment of the properties and potential applic[...]
 
New energy efficient magnesium technology for strip production and its potential
 
KAWALLA RUDOLF  ULLMANN MADLEN  Oswal d Matthias  VOGT HANS -PETER  
Magnesium thin sheets have been manufactured in a complex process from slabs produced by continuous casting by well-known companies like Elektron in Bitterfeld, Dow and Alcoa since the 20th century. This conventional method is still being used by firms like Salzgitter Magnesiumtechnologie and M&B MAG Toronto. The technology of twin roll casting, which was developed at the beginning of the 21st century, reduces the production costs by a substantial amount and is gaining importance worldwide. Numerous research teams in Australia, China, Germany, Japan and in Turkey are dealing with it. Major advantages are the use of cheaper input materials, not having to use continuously cast input material, that no heating is needed during rolling afterwards and that less rolling passes are needed to reach the final dimensions of the sheets. Another characteristic is the fast solidification (10 times faster than in the continuous casting of slabs). This leads to a finer-grained microstructure and the reduction of cavities, pores, segregations and brittle precipitations which give better formability and a better quality of the final product. In Figure 1 the conventional method of production of magnesium thin sheet and twin roll casting are compared schematically. The conventional method which is represented herein is a highly productive, extensive production installation with continuous casting, disconnected roughing and finishing line, decoiler equipment and a coil box. The reduction of process steps which the new technology of producing strips with dimensions closer to the final product with twin roll casting creates is, as mentioned above, mainly caused by not having to use the costly roughing process including mechanical treatment of slabs. Table 1 gives an overview of the producing and production similar twin roll casting plants for the manufacturing of magnesium thin sheet. Small laboratory installations are not being accounted for. All[...]
 
New tool materials based on Ni alloys strengthened by intermetallic compounds
 
PIOTR BAŁA  
Tool steels containing from 0.30% to 0.60% C, up to 5% Cr and Mo, W and V are universally applied as tool materials for operations in high temperature. Tools made of these steels obtain functional qualities by means of heat improvement, it is by combining quenching procedures with medium or high tempering. Tempering of tool steels is usually done in the temperature range: 550÷620°C. Strengthening is achieved by precipitating alloy carbides of MC and M2C (V, Mo and W) type [1÷4]. Several tools have to operate at temperatures above 600°C, sometimes even at 1000°C, at which quenched and tempered steels soften and the lifespan of tools rapidly decreases. The chemical composition of tool steels was, for many years, modified to improve their hot-working properties. The combined alloys Cr-Ni-Co-Fe with additions of W, Mo, Nb, in which a significant part of iron was substituted by Co were developed [5]. A group of alloys based on the Co matrix (Stellite) of good tribological properties intended for cutting tools was obtained. Those alloys can be divided into certain main groups: Co-Cr-W-C and Co-Cr- W/W-Ni/Fe-C with modifications Si + B [6, 7]. Unfortunately, the maximum temperature range in which those alloys can operate is only 600÷750°C. A development of high temperature creep-resisting nickel-base alloys was mainly the modification of 80% Ni and 20% Cr alloy known for its good creepresistance. On account of ineffectiveness of strengthening by carbides in high temperatures a hardening of Ni-base alloys was obtained by intermetallic compound Ni3(Ti, Al) marked as &#947;´ [8, 9]. Several alloys were developed based on the concept of Ni matrix strengthened by the &#947;´ phase, among others alloys of an increased carbon content and a complex chemical composition [10÷12]. There are alloys of Ni matrix - intended for tools operating at temperatures above 600°C - containing from 0.10% to 0.25% C, from 8 to 25% Cr, up to 25% Co, up to 4[...]
 
Nickel aluminate spinel (NiAl2O4) in Al2O3-Ni composites
 
Katarzyna Konopka  
Ceramic materials are toughened by incorporating particles of a ductile metal [1, 2]. Toughness of such composites is due mainly to plastic deformation of the metal particles (the bridging effect) and the deflection of cracks by these particles [1]. Which of these effects predominates depends on the bonds between the metal particles and the ceramic matrix. If the ductile particles are weakly bonded with the ceramic matrix, the crack will propagate along the interface, whereas when this bond is strong, plastic deformation of the metal particles predominates [3]. Among metals Ni is chosen as particles incorporated to the ceramic matrix for its high melting point. During sintering in an oxygen environment (high partial pressure p(O2)), Ni can react with Al and oxygen from the Al2O3 ceramic or from the gaseous phase and forms the NiAl2O4 spinel phase according to the reaction [3]: Ni + Al2O3 + 1/2O2 = NiAl2O4 (1) The stability of the spinel phase depends on the oxygen partial pressure in the protective atmosphere, and on the sintering temperature [3, 4]. When the oxygen partial pressure is low, the NiAl2O4 will eventually reduce to nickel, alumina and oxygen after its formation [4]. The formation of the spinel can be avoided by conducting the sintering process in argon, CO or H2 [3]. The more complicated is the process of phases formation in composites when first the Ni particles are oxidized during the process of forming or sintering. After the oxidation of Ni the spinel can also be formed as a reaction [5]: Al2O3 + NiO = NiAl2O4 (2) In the solid-state formation of the spinel the so-called Wagner mechanism is operated [6]. According to this mechanism Ni2+ ions diffuse through the spinel layer from NiO/NiAl2O4 interphase to the NiAl2O4/Al2O3 boundary. This reaction leads to formation of one equivalent of NiAl2O4 on the NiO side of the interface and three equivalents of spinel on t[...]
 
Numerical simulation of microstructure and internal stresses of the modified bone cement
 
JERZY NOWACKI  ADAM SAJEK  
Hip joint belongs to the most exploited carrying joints in the human motor organ [1]. Static and fatigue strengths affect the size of transferred stresses and overload capacity whereas the surface condition and its physical and chemical features determine the nature and the strength of joint at the border of bone-implant phases [2, 3]. Even though implantology gives possibilities of replacing damaged anatomical structures, it restores the lost functions only for a certain period of time. A reason of that is a wear and tear of artificial joints, which leads with time to a repeated failure of function [4÷7]. The bone cements are modified with many agents that improve their operational properties, with a modifying agent participating in polymerization reaction or being inactive. Addition of reactive modifying agents, apart from affecting strength properties, can also decrease the intensity of heat released during mixture hardening through extension of the reaction time or reduction of the amount of toxic MMA monomer being liberated into human organism after cement hardening [8, 9]. Gentamicin containing cements used so far show that within a certain time interval a drug is released from them into environment. Some authors are of the opinion that gentamicin release takes place by the diffusion of compounds through polymer matrix or capillary through the empty spaces inside it [10]. Nevertheless, a considerable part of scientists examining the phenomenon of drug release from bone cements think that it strongly depends on surface roughness [11÷13]. Until now, the phenomenon of gentamicin release has been closely examined. When comparing popular cements containing gentamicin used at present, one may conclude that release rate depends for the most part on such parameters as cement surface smoothness, porosity and wettability. These cements can be also modified with substances improving drug release rate [14]. Results of the abovementio[...]
 
Optimization of Fe and Al elemental powders sintering parameters by DTA analysis
 
Stanisław Jóźwiak  Krzysztof Karczewski  Zbigniew Bojar  
Sintered iron aluminides are very promising novel structural materials mainly because of their attractive physical and mechanical properties, but also because of the low price of raw materials used for their manufacture [1]. Powder metallurgy (PM) eliminates many of the limitations during the fabrication process [2]. For example, PM enables forming of products with complex shape, choosing almost arbitrary chemical compositions, deals with problem of grain overgrowth, gives better chemical and structure homogeneity as well it is an energy-saving process [3÷5]. However, in case of the Fe-Al phases, the use of this method is limited by the necessity of controlling of the SHS (self-propagating high-temperature synthesis) reaction [3]. SHS occurring during sintering of Fe and Al elemental powders mixture is very rapid and strongly exothermic, which unfortunately may cause unwanted porosity of the sinters [6]. Our previous studies [7÷10] show the great complexity of phenomena taking place during presintering process of Fe and Al powders. These effects correlated with diffusion and phase transformations were also studied by other researchers [1, 3, 4]. It was concluded that the mechanism of exothermic phase transformations is strongly correlated with many factors, such as chemical composition of the sample, elemental powder particles size, atmosphere, and the heating rate. It is important that only the formation of the exothermic Fe2Al5 phase was reported prior to the formation of finally-wanted FeAl phase [1]. Our last investigations show however that not only Fe2Al5 but also other high aluminum phases - FeAl3 and FeAl2 could be found in the samples structure sintered at temperature lower than the SHS reaction temperature. In order to limit unfavorable influence of the SHS on sinter structure, the optimization of the powders particles size, the compact pressure and the heating rate was done in this work. EXPERIMENTAL Investigation[...]
 
Optimization of galvanic bath and operating parameters for amorphous Ni-W electrodeposition
 
PAULINA INDYKA  EWA BELTOWSKA-LEHMAN  AGNIESZKA BIGOS  Leszek Tarkowski  Marcin Kot  JERZY MORGIEL  
Functional coatings obtained by electrodeposition are widely applied commercially to provide enhanced surface performance for engineering applications [1]. In recent years much effort has been put into searching for alternatives to electroplated hard chromium, the properties of which are often used as a standard for other functional coatings [2]. Usually, high hardness, wear and corrosion resistance are the critical properties. Despite the excellent properties of the hard chromium coatings, used in automotive and aviation industries, they should be eliminated from the manufacturing process (according to the EU directives), due to high toxicity and carcinogenity of hexavalent chromium. Up to now, only electroless hard Ni and Ni-P coatings have found use in selected applications [3]. Electrodeposited Ni-based alloys containing refractory metal (molybdenum or tungsten) could be an important alternative to hard chromium. Ni-W alloys are known for their excellent mechanical and tribological characteristics, but they are very difficult to obtain by conventional metallothermic methods, due to the large differences in melting points (Ni - 1455°C, W - 3410°C) as well as limited mutual solubility of both metals [4]. Hence, electrochemical deposition can be proposed as an alternative technique. Electrodeposition, as a cheap, low temperature and simple method, is a superior technique for manufacture of Ni-W coatings. However, compact and well adherent to the substrate Ni-W coatings are still electrodeposited with technical difficulties. Although tungsten cannot be separately electrodeposited from aqueous electrolytes, it can be easy co-deposited with iron-group metals such as nickel to form an alloy [5]. However, the presence of appropriate complexing agents is necessary. This phenomena is classified by Brenner as induced co-deposition [6]. Among many galvanic baths proposed for the Ni-W alloys electroplating (such as sulfamate, pyrophos[...]
 
Oxidation and creep behaviour of the CVD aluminized Rene 77 nickel-based superalloy
 
WALDE MARZIAJA  Marek PORĘBA  JAN SIENIAWSKI  
Turbine blades are heavy loaded elements of the aircraft gas turbines. They are subjected to extremely high mechanical and thermal loads in the chemically aggressive environment. The most important criteria for selection of the blades material are high tensile strength at elevated temperature both for static and dynamic loads, high fatigue and creep strength along with good resistance to high temperature corrosion [1, 2]. Required high temperature oxidation resistance of the modern gas turbine elements can be obtained by application of protective coatings. The most effective and widely used are diffusion coatings containing aluminium: Al-Si, Al-Cr, Al-Pt, Pt&#8209;AlCr and others [3÷6]. Widely accepted techniques of obtaining coatings based on intermetallic phases of the Ni-Al system are pack cementation and out of pack methods. Although they fulfil technological requirements for manufacturing of aircraft engines elements, they present threat to environment because of emission of gaseous chlorides during the process [4]. Aluminizing by chemical vapour deposition method, in which reactive atmosphere is generated in external reactor and supplied in the form of aluminium halides into the main reactor, was introduced successfully to produce heat-resisting diffusion layers of the analogous chemical and phase composition like in traditional methods [4, 7]. This method allows to avoid contact between substrate material and powder mixture and provides more precise control of process parameters. The highest chemical cleanness of the coating obtained by low-activity CVD process additionally increases their oxidation resistance [8, 9]. CVD method allows to form the coating both on the external surface of the turbine blade and simultaneously on the internal surface of the cooling channels having small cross-section. Additionally it enables control of the cooling rate of substrate from process temperature. It facilitates complex heat trea[...]
 
Platelets activation and adhesion on TiN+Ti2N+αTi(N) layer produced in plasma space on Ti6Al4V alloy
 
MAŁGORZTA GONSIOR  ROMAN KUSTOSZ  TOMASZ BOROWSKI  MACIEJ OSSOWSKI  MAREK SANAK  BOGUMIŁ JAKIEŁŁA  TADEUSZ WIERZCHOŃ  
The original extracorporeal pulsatile heart support device, called POLVAD, has been developed in Poland. It was used in over 200 patients with the longest duration of 1 year. The innovative tilting disc valve for this device is developing. The valve consists of original valve ring, free of pivot element crossing the blood stream (Fig. 1). The valve ring is made of titanium alloy Ti6Al4V type. Titanium and its&#8217; alloys demonstrate numbers of beneficial properties in medical applications. They are a subject to study metallosis, they demonstrate very good biotolerance to tissue habitat, high resistance to corrosion, and thermodynamical stability in physiological conditions. The thromobogenicity is one among t he problems, regarding titanium and its&#8217; alloys applications as the biomaterials. For that reasons appropriate surface modifying layers of titanium are developed - to improve material properties for blood contact. Nowadays, surface engineering techniques are used as base point for creation a proper chemical composition, structure and physicochemical status of biomaterial surfaces - to obtain its required biological properties and functions. The surface modifications of titanium and its&#8217; alloys influence surface layer structure and morphology, adhesion and inside layer residual stress. They influence a total implant stability in live organism habitat as well as improve biocompatibility. The microstructure, roughness and thrombogenicity of diffusive titanium nitride layers on titanium Ti6A14Al alloy are examined in the work - together with thrombogenicity testing, performing as the material induced platelets activation and its adhesion to the biomaterial surface. MATERIAL AND METHODS The titanium nitride layers were formed at the Surface Engineering Department of Warsaw University of Technology. Three diffusive layers: TiN+Ti2N+&#945;Ti(N), TiO2+Ti2N+&#945;Ti(N), and Ti(OCN[...]
 
Porous Fe-Al intermetallics fabricated by SHS reaction in volume control environmental reactor
 
KRZYSZT OF KARCZEWSKI  STA NIS ŁAW JÓŹWIAK  MICHA Ł CHOJNACKI  ZBIGNIEW BOJAR  
Recently, there has been a considerable increase in interest for porous materials due to their unique properties such as high energy absorbing capacity, reduced thermal conductivity, enhanced acoustic damping ability and so forth. Currently, a great deal of attention is focused on metallic foams. However, if metals could be substituted by ceramics, intermetallics or their composites, such foam materials could be used for applications in extremely severe environments, such as in thermal barrier coatings at high-temperatures and filter materials in severe corrosive environments [1, 2]. Among intermetallics, FeAl have been well studied as structural materials in the past decades [3÷6]. Due to their sound physical and mechanical properties, FeAl were expected to replace traditionally materials in many engineering applications. In addition, FeAl intermetallic compounds have a relatively low density and low cost. Nevertheless, the brittle fracture and low ductility of FeAl at ambient temperatures limit their cold working. The powder metallurgy processing technique may overcome this problem. The technology based on powder metallurgy eliminates a number of limitations in the manufacturing process, allowing for complicated shapes of the semi-finished or finished products. Furthermore, the technology enables a wide selection of various compositions, eliminates a problem of the grain coarsening, inhomogeneity of chemical composition and structure and, finally, assures easier control of the process of shaping the structure of material, as well as reduces the use of raw elements [4, 5]. In t[...]
 
Powder production method for thermal spraying of wear-resistant and low-friction coatings
 
Piotr Kula  Robert Pietrasik  Łukasz Kaczmarek  Adam Krasiński  Konrad Dybowski  
The universal drive towards developing pro-innovative ecological technologies has contributed significantly to the development of recycling technologies and remanufacturing of worn-out machine components. The application of these technologies can substantially lower the production costs of new spare parts that would possess similar or even better operational properties; the latter is the case where refurbishing is combined with modern surface treatment technologies [1, 2]. Some components are refurbished using Multiplex technologies that combine reconstruction of the geometry of the components with improvement in their operational properties through thermal and chemical treatment. They are particularly useful for, e.g. low- -friction gradient layers [3÷6]. An optimum, energy-saving and universal solution for this technology would be to combine surface reconstruction with simultaneous addition of low-friction coatings resistant to wear. This would be feasible through the possibility of thermal spraying [7] using specially prepared powders that would have such properties as high hardness, durability and a low friction coefficient. These could include coatings based on, for example, thermochemically hardened powders conta[...]
 
Producing and properties of the polylactide-alumina nanocomposite fibres
 
PATRYCJA CZARNEC KA  TOMASZ CIAC H  ANTONI KUNICKI  ANDRZE J OLSZYNA  MONIKA GOŁASZEWSKA  AGNIESZ KA JASTRZĘBSKA  
Electro-spinning is a very promising and very interesting process of fibre production. This technique allows us to produce fibres of a diameter ranging from few na nometers to 1 mm [1÷5]. Experiments have showed that almost every polymer can be made into fibres by electro-spinning. Electro-spun fibre can be applied in an aerosol filtration but it can also be used as a drug carrier or bandage. First publications about electro-spinning for fibre production were published by Petrianov [6]. Other current applications include medical applications of electro-spun fibres as wound dressings. A portable device for fibres electro-spinning can be applied directly on the wound and produce a permeable wound dressing, applicable especially in the case of vast burns [7]. Electro-spun fibres, even if they are very fine, can be easily collected, if compared to other methods. The method for electro-spinning fibres collection is showed in Figure 1. Polylactide (PLA) is polyester produced in the lactide ring-opening polymerization process. Polylactide is the most important plastic material that can be derived from renewable resources. It also has an omnipresent status in the biomedical field, because of ability to decompose over a period of time [8]. In case of materials that can be decomposed in human organism, it is crucial to use filler, which will serve as a scaffold for human tissue after polylactide decomposition. Among all inert inorganic fill[...]
 
Properties of high alloyed CrMnNi steels with strain induced α′ martensite formation
 
Andreas Jahn  Alexander Kovalev  Steffen Wolf  Andreas WeiSS  Lutz Krüger  Piotr R. Scheller  
It is well known that austenitic chromium-nickel or chromium-manganese- nickel steels with low stacking fault energy show a stress and strain induced formation of martensite during mechanical loading. The transformation induced plasticity (TRIP) effect occurs in metastable austenitic or austenitic-martensitic steels for wrought and also cast alloys [1]. The strain induced formation of martensite is controlled as well by its chemical composition as by stresses [2], which are higher than the yield stress of the initial microstructure. They activate shear processes accompanied by deformations. For each type of strain induced martensite formation a triggering stress exists which is controlled by the temperature and the chemical composition of the steel. This can be obtained from suitable experiments [3÷5]. Generally three mechanisms of the martensite formation, the &#947;&#8594;&#949;, &#949;&#8594;&#945;&#8242; and &#947;&#8594;&#945;&#8242; transformation, are discussed in Cr-Ni steels. During the &#947;&#8594;&#949; transformation the &#949; phase is observed as thin straight lines in the microstructure of the austenite [6]. The &#947;&#8594;&#949; and &#949;&#8594;&#945;&#8242; transformation can proceed simultaneously. The result is the &#947;&#8594;&#949;&#8594;&#945;&#8242; sequence [3÷4]. During this process the &#949; martensite is an instable intermediate phase and usually cannot be detected. In Cr-Mn-Ni steels the &#949; martensite is an intensively discussed subject. It is open either the &#949; martensite is a unique phase or a pseudo-phase caused by the concentration of stacking faults in the direction of load. The reasons for these plastic deformations are the commonly observed phenomena as shearing strain, twinning and different slip processes in the initial phase. Thus, some of these mechanisms are linked to special movements of dislocations. The strain induced formation of martensite generates the TRIP effect. It is [...]
 
Quantitative evaluation of γʹ phase in CMSX-4 superalloy
 
AGNIESZKA SZCZOTOK  TOMASZ RZYCHOŃ  JAN CWAJNA  
The microstructure of nickel-base superalloys determines their mechanical behaviour. The strength of Ni-base superalloys is dependent on such factors as volume fraction, size, coarsening rate, and composition of &#947;&#697; phase precipitates [1]. The content and size of &#947;&#697; phase precipitates embedded in a cubic face-centred &#947; matrix can be adjusted by the alloy design and heat treatments. The composition of the ordered &#947;&#697; precipitates does differ, i.e. Ni3(Al, Ti, ...), and depends on the alloy composition and processing [2]. The characterization of &#947;&#697; phase precipitates in different nickelbased superalloys has been the subject of extensive research work. Volume fraction of the &#947;&#697; phase in Ni-base superalloys is a significant element influencing on working out the superalloys chemical compositions [3]. MATERIAL The measurements of &#947;&#697; phase precipitations were carried out on a monocrystalline cylindrical bar of 8 mm diameter made of CMSX-4 nickel-base superalloy [4]. The bar was cast in Laboratory of Material Research for Aircraft Industry in Rzeszów. The material was investigated in the as-cast condition. IMAGE ACQUISITION AND ANALYSIS OF &#947;&#697; PHASE PRECIPITATES The bar intended for investigations was cut perpendicularly to the main axis. The procedure of metallographic specimen preparation was described in details in Table 1. Quantitative metallography of CMSX-4 requires the revealing of &#947;&#697; precipitates by means of an appropriate etching conditions selection as well as use of appropriate image acquisition in order to observe the &#947;&#697; precipitates and register the images of the superalloy microstructure with them. In the previous work two etching methods of the &#947;&#697; phase precipitates were described [5]. For a quantitative evaluation of the precipitates etchant caused their etching and leaving the &#947; matrix is better, so in the ca[...]
 
Real kinetics of Fe-Al type intermetallic phases sintering analysis based on extended JMA model
 
MICHAŁ CHOJNACKI  STANISŁAW JÓŹWIAK  KRZYSZTOF KARCZEWSKI  ZBIGNIEW BOJAR  
Production of certain advanced ceramics, composites, and intermetallic compounds in most cases is connected with complex and high energy consumption techniques. Increasing tendency to limit costs of fabrication requires development of efficient and energy-saving technologies. In case of Fe-Al intermetallic materials fabrication Powder Metallurgy (PM) methods associated by Self-propagating High-temperature Synthesis (SHS) become more popular [1]. Nevertheless, SHS assisted sintering is connected with high intensity, high synthesis temperature and limited possibilities of reaction control which lead to high porosity of sinters [2]. Such issues require deep study of intermetallic phases nucleation and transformation mechanisms during SHS reaction. Kinetic parameter of those transformations, for example the Avrami exponent n, could be calculated from DSC experiments according to the JMA model adapted to non-isothermal conditions [3÷12]. Unfortunately the JMA equation which allows to determine nucleation and growth mechanism on the basis of Avrami exponent n value has some limitations [13]. In theory Avrami plot should be a straight line of which slope is the Avrami exponent n. The experimentally observed kinetics show some deviations from this theory. They are connected with continuously changing reaction conditions forcing to calculate the slope of straight linear fragment of such plot in range from about 25 to about 75% of degree of phase transformation &#945;. Thereby calculated value of n is affected by some error and does not give any insight in phase formation mechanism at the beginning and the final stage of the process. Some authors suggest that in order to eliminate this inaccuracy the local Avrami exponent should be calculated [14]. The aim of this study was to compute the local Avrami exponent n(T) from slope of lines parallel to tangent to Avrami plot lines in following points from entire range of particular phase form[...]
 
Research on the texture of Cu/Ni multilayers with a diversified period thickness
 
Barbara Kucharska  Edyta Kulej  Małgorzata Witkowska  Zygmunt Nitkiewicz  
The modification of materials surface, including the production of surface layers and coatings, constitutes now one of the key problems of materials engineering. Particularly interesting is the production of coatings in a multilayer system, whereby materials of unique properties resulting from the diversified composition of components (such as metals, semiconductors, and their combinations) can be obtained [1]. From the point of view of magnetic properties, multilayers in ferromagnetic/diamagnetic material systems are being intensively investigated, owing to the gigantic magnetoresistance (GMR) phenomenon that has been discovered in them by a team of scientists under the guidance of Alberta Fert and Peter Grünberg. A thin-layered Cu/Ni structure is a classical example of a multilayer of such properties, which could be applied in construction of hard discs [2÷7]. The identical crystallographic structure, fcc, and the very small misfit (2.5%) of the copper and nickel lattices cause Cu/Ni multilayers to exhibit good mutual adhesion and to be easily made by various techniques, including PVD [8, 9]. Depending on their production technique and thickness, multilayers can exhibit a different degree of texturing. A heavy texturing of sublayers causes an increase in the roughness of interfacial surfaces, which adversely affects the quality of the multilayers, e.g. impairs their magnetic properties [10, 11]. For the examination of the structure and quality of coatings, the X-ray diffraction technique is commonly used [12÷14]. Material and methodology The material used for tests were Cu/Ni multilayers produced on a monocrystalline Si(100) silicon substrate by the magnetron sputtering method. The multilayers were diversified in terms of Ni sublayer thickness (1, 3 and 6 nm), while maintaining a fixed Cu sublayer thickness of 2 nm. Each multilayer was built of 100 periods, each of a thickness[...]
 
Resistance to isothermal oxidation of austenitic cast steel with Ti addition
 
MAŁGORZATA GARBIAK  RENATA CHYLIŃSKA  BOGDAN PIEKARSKI  
Highly alloyed nickel-chromium cast steels form a group of structural materials that ensure durability of components at elevated and high temperatures in a corrosive environment. The durability of these alloys is owed to their good mechanical properties and excellent chemical stability [1]. Most of the working environments that these alloys are subjected to contain oxygen, carbon dioxide and water vapours. The good corrosion resistance of these alloys is attributed to the ability to form continuous, dense layer of oxides on the surface of the material, which consists mainly of Cr2O3 [2, 3]. Such layers act also as protective coatings in carburising atmospheres [4]. Apart from required level of chromium the protective effectiveness of such oxide layers is strongly influenced by addition of other alloying elements such as Si, elements of the group III and IV of the periodic table (e.g. Nb, Ti, Zr) or rare earth elements (Ce, Nd, Pr). These may be introduced to the alloy individually or as a mixture adding up from tenth parts to several percents [1÷3, 5]. The aim of this work is to describe the influence of Ti additions in 30Ni-18Cr alloys on resistance to isothermic oxidation in air at 900°C temperature. Titanium belongs to the group of elements with high affinity to oxygen. The oxides of titanium are stable in a wide range of temperatures. Although the role of titanium on oxidation resistance improvement of austenitic alloys is not established in undeniable manner [6] it is nonetheless recommended for alloys working in oxidising atmospheres. However, due to difficulties with introduction of Ti to these alloys in the melting process and related castability deterioration in practice addition of niobium is preferred [1, 7, 8]. EXPERIMENTAL Two sets of specimens from 30Ni-18Cr creep resistant cast steel were prepared with two levels of Ti (Tab. 1) using sand gravity casting. The materials preparation, melting and casting process w[...]
 
Rheological behavior of nanosized silica suspensions
 
Tomasz Żmigrodzki  Anna Danelska  Łukasz Wierzbicki  Marcin Leonowicz  Mikołaj Szafra n  
Most materials behave in such a way that they have a combination of viscous and elastic response under stress or deformation. Materials behave in linear manner, as described by Hooke or Newton, on in a small scale. Among real liquids the Newtonian and non-Newtonian fluids can be distinguished. Viscosity is one of the rheological parameters which can characterize the liquids. By measurements of the viscosity versus share rate one can classify the liquid into a particular group. If the viscosity is decreasing vs. shear rate the liquid has shear thinning properties, when the viscosity is rapidly increasing the shear thickening effect or dilatancy is observed. The rheological classification of liquids is presented in Figure 1 [1]. Shear thickening effect appears in suspensions having various concentration and morphology of solid phase. The shear thickening of fluids can be explained by a few theories. The most popular is the clustering theory. According to its main assumption the particles, at low shear rates, are prevented from aggregation by steric repulsive and Brownian forces. Under increasing shear rate the hydrodynamic forces also increase and the particles form chains, blocking the flow of the fluid. The next potential explanation of the dilatancy phenomenon, is Order-Disorder Transition (ODT) theory, which claims that t[...]
 
Selection of heat treatment and aluminizing sequence for Rene 77 superalloy
 
MAREK PORĘBA  JAN SIENIAWSKI  
One of the key issues of modern aerospace industry is protection of the hot part of the aircraft engine against oxidation and corrosive atmosphere. Development of the engines is related not only to growing efficiency but also to operational reliability of the components critical for flight safety. Nickel-base alloys have been used for blades in gas turbines since early 50s of XX century [1, 2]. Extension of the service life of turbine blades and their reliability is possible through increase of heat and creep resistance of the material. Creep resistance can be controlled by proper heat treatment whereas heat resistance can be raised by protective coatings application. One of the possible solutions is deposition of diffusion coating based on nickel aluminides in the process of aluminizing [3, 4]. Advantageous properties of aluminium result from its high affinity to oxygen. Production of aluminides coatings containing intermetallic phases of the Ni-Al system is most often realized by pack cementation and chemical vapour deposition (CVD). Among the various phases of the Ni-Al system like &#947;&#697;-Ni3Al, &#946;-NiAl, &#948;-Ni2Al3 and &#949;-NiAl3, the primary phase of the coatings obtained in the aluminizing process of nickel-base superalloys is &#946;-NiAl. Specific physicochemical properties of that phase are high heat resistance, heat conductivity and density which is smaller comparing to the nickel-base alloys [4÷6]. Aluminizing by CVD method enables simultaneous forming of the coating both on the external surface of the turbine blade and on the internal surface of the cooling channels, allows to control the cooling rate of substrate and to combine it with heat treatment of the cast nickel-base superalloys [7÷9]. The aim of the study was to determine the effect of the parameters of thermochemical treatment of Rene 77 superalloy (precipitation hardening and aluminizing) on its oxidation resistance and creep properties. ma[...]
 
Self-lubricanting cold forging tools
 
Hanna Wiśniewska-Weinert  Jacek Borowski  Mikhail Ignatev  BOHUMIL Jedovnicky  Tomasz RY BAK  Volf Leshchynsky  
In recent years, larger, more complex parts have been successfully cold forged due to improvements in forming equipment, die and workpiece materials, die coatings, and process design. In addition to the savings in energy costs, modern cold forging enables parts to be produced to near net shape [1]. Working conditions of forging tools have become severer with the years and it has been required for forging tools used to this end to increase the hardness, wear resistance and heat resistance. A typical shape of the tools exhibits an assembling in which a Cemented Carbides (CC) or High Speed Steel Insert (HSS) mounted into the casing. In these CC and HSS tools, the surface of the insert is ordinarily coated by CVD/PVD methods [2]. Many factors influence component accuracy in the form of systematic and random dimensional errors in the cold forming processes. There are four important factors that affect the component systematic errors, i.e.: imperfection of the material plastic flow, elastic deformation of the press system, elastic&#8211;plastic deformation and thermal behaviour of the tools and component [3]. The later two factors are most important and relevant to process and tool design of formed components. These effects become evident during different stages in the cold forming process, typically including forming, unloading, ejection and cooling. The repetitive production cycles in the industrial practice will bring further issues of dimensional changes due to tool wear and temperature increase developed over time. Thus, the tool wear resistance is one of the most important requirements.[...]
 
Shape recovery characteristic of ferrous shape memory alloy by prestrain of biaxial stress
 
Hisashi NAOI  TAKAMASA GAMOU  TAIKI KAWAGUchI  MANABU WADA  TADAKATSU MAruyama  
As for the ferrous shape memory alloy, the application to the connection components including the tube fittings [1] and the large- -scale structural material with the functionality is expected. In order to apply this alloy to the connecting materials, it is necessary to estimate the amount of deformation and the connecting strength after prestrain is supplied and shape recovery heat-treatment is performed. Because the forming method of the prestrain is often given not only uniaxially but also multiaxially, the investigation of the shape recovery characteristic to the multiaxial forming is important for wide practical use of the alloy. Authors investigated [4, 8, 9] the shape recovery characteristic concerning the prestrain formed during the uniaxial stretching of tensile test and the biaxial stretching of the hydraulic pressure bulge forming. In addition, the consideration based on the mechanism of the stress-induced martensitic transformation that rules the shape recovery behavior has been studied. However, a wide-ranging investigation has been requested as for the data of the shape recovery strain of the transitional region from the uniaxial stretching to the biaxial stress condition because the shape recovery data are not sufficient. Figure 1 shows the schematic of stress-strain and temperature-strain curve in the shape recovery process. The strain worked by plastic deformation to the specimen in this report is defined as &#949;p of prestrain, and the strain measured by the displacement of the gauge length from before to after the heat treatment is defined as &#949;r of shape recovery strain. When the alloy is applied to a fixed amount of deformation and is heated at a fixed temperature repeatedly, larger shape recovery strain will be developed. This phenomenon is called training effect. It is reported [4] that the shape recovery strains of Fe-28%Mn- 6%Si-5%Cr alloy are measured in the case of without training and with trai[...]
 
Structural and mechanical properties of Al-0.25Zr alloy obtained on the way of RS ribbons consolidation
 
Tomasz Tokarski  
During the last decade, an extensive research programmes on development of new materials that are capable to meet a constantly rising industry demands were run. Nanotechnology and grain size refinement techniques generated new possibilities in the fields of materials construction. Those novel procedures can be applied to design new products that could meet contradictory requirements, for example material for energy transmission lines. Such materials should be characterized by as high as possible electrical conductivity and specific strength, stable at elevated temperatures [1]. There is always a contradiction between the two, since usually an improvement of one parameter results in decrease of the other. First generation power lines were constructed from aluminum cables reinforced with steel strands. Aluminum has lower electrical conductivity than copper but it is more than compensated by lower density and cost. A direction of further development was to increase the ampacity (current carrying capability). Second generation, self supporting cables, was devoid of steel core. The required strength in order to be able to self support was obtained by addition of alloying elements to aluminum. Mechanical properties were effectively enhanced by solid solution strengthening or precipitation strengthening. Usage of these conventional strengthening mechanisms results in degradation of electrical conductivity as a consequence of the presence of alloying elements in the solute form in the matrix. Total ampacity change is positive due to elimination of steel core and increase of crosssection utilization for carrying the current. Investigations are carried out in order to enhance conductivity while keeping mechanical properties at the highest possible level. In order to meet these requirements, usage of a completely different strengthening mechanism is proposed. It is well known that materials strength increase can be obtained by refinement[...]
 
Structural and physical properties of chromium layers obtained by pulse plating techniques
 
Naroa Imaz  EVA GARCÍA-LECINA  José Antonio Díez  Miren OSTRA  MarIa SARRET  
Chromium plating has successfully been used since 1925, representing one of the most important processes in the galvanic industry due to its unique combination of wear, hardness and corrosion properties at low cost. Chromium electrodeposition is widely used in automotive, aerospace, industrial and general engineering applications for both decorative and functional coatings [1, 2]. Two types of chromium coatings can be classified according to their thickness: decorative chromium (0.80 &#956;m) and functional or hard chromium (20÷500 &#956;m). The most common hard chromium electrolyte is constituted by chromium oxide solutions containing a low concentration of one or more catalysts, usually sulphate. The current efficiency of chromium electrodeposition is low, using only 10÷15% of the applied current: the majority of the electric charge is consumed by the hydrogen evolution reaction (80÷90%) and 5% of the current is used in the reduction of hexavalent chromium to trivalent chromium species. However, and in spite of its low current efficiency and the carcinogenity and toxicity of hexavalent chromium, this process is not currently replaceable due to the excellent properties of the coatings obtained [3]. A key factor to modify the properties of a coating is to focus on its microstructure. Thus, it is well known that there is a relationship between the processing parameters and the microstructure, morphology and properties of the coatings. Different approaches can be undertaken to modify the microstructure of a coating. In this sense, pulse plating techniques are widely used in the electrodeposition of metals and alloys due to their reported influence into metallic distribution, efficiency, microstructure, morphology and coating properties [4÷6]. In pulse plating the current is interrupted or alternated on a short time scale during the metal electrodeposition, offering a higher number of variables comparing to direct current proces[...]
 
Structure and properties of Al-Cu-Fe thin films deposited by PLD technique
 
SŁAWOMIR KĄC  MAŁGORZATA KĄC  
Recent progress in the development of quasicrystals (QCs) as low- -friction, hard materials, makes these alloys ideal candidates for protective coatings. However one disadvantage of quasicrystals is that they are quite brittle. To overcome this problem, we are taking advantage of nonstructural materials and produce coatings, which consist of a nanograin quasicrystals and metal. Quasicrystals are alloys, which have long-range rotational symmetry, but lack translational periodicity in three dimensions. In spite of the lack of translational periodicity, these materials show sharp diffraction patterns with symmetries, which are forbidden for ordinary crystals (five-fold or ten-fold axes, for instance) [1]. Analysis of bibliography [2÷4] shows that quasicrystals exhibit intriguing surface properties in air. First of all, they have low coefficient of friction, low propensity to wetting by polar liquids, excellent oxidation resistance and high hardness. However, given that they are brittle materials they are usually employed as film coatings. Up to now, quasicrystalline phases have been observed in over 100 different metal alloy systems. One of the systems creating of quasicrystal phases are Al-Cu-Fe alloys. Their friction properties and hardness makes them an interesting material for wear-resistant coatings. Their low thermal conductivity and their improved ductility above 750°C make them suitable for thermal barrier coatings [2, 5, 7]. The production of good quality quasicrystalline Al-Cu-Fe alloys on an industrial scale is still difficult. Literature study shows, that is possible to form Al-Cu-Fe quasicrystals using different methods, like melting and solidification, melt spinning, gas atomization, mechanical alloying [2], and by PLD technique [4, 6, 8]. Literature study [9, 10] indicates that PLD technique which allows to transform stoichiometrically material from the target to film seems to be an ideal method for preparation of[...]
 
Structure and properties of low temperature nitrided/oxidized NiTi alloy
 
Józef Lelątko  Tomasz Goryczka  Tadeusz Wierzchoń  Maciej Ossowski  Bożena Łosiewicz  
NiTi alloys have been widely used in biomedical field due to their shape memory effect, superelasticity and good biocompatibility [1]. They are excellent biomaterials for orthopaedics, dental applications, vascular and organ surgeries. However, these applications, especially as a long term implants, require special attention with respect to nickel ion release into the patient&#8217;s metabolism system and the surrounding tissue. The nickel can cause allergies if persons are highly sensitive and has a toxic effect on the cell when its concentration exceeds a certain level [2]. In order to improve the corrosion resistance of the NiTi alloy and suppress the release of nickel ions, many surface modification techniques have been used. Titanium oxide and nitride has been found a good candidate for layers, which sufficiently protect human body [3, 4]. Additionally, combination of a layer sequence, forming the titanium oxide and titanium nitride layers, increases corrosion resistance and biocompatibility [5]. The titanium oxide, especially TiO2 [6], increases the stability of the surface, creates the physical and chemical barrier against oxygen migration to the top and limits the way of the nickel oxidation [7]. Low chemical reactivity, high hardness as well as wear and corrosion resistance are characteristic properties of the titanium nitride and titanium oxide layers. Reported results show that layers were thick. Moreover, between the layer and the NiTi matrix a sublayer of intermetallic phases such as Ni3Ti or Ti2Ni were formed [5, 8]. All phases reveal low plastic properties, which limit their practical application in the field of medicine where the shape memory effect or superelasticity is required. Therefore, the formation of very thin surface layers of TiN, TiO2 or TiN+TiO2 with suitable nanostructure is the way to improve the biocompatibility of NiTi alloy with shape memory effect. In the present work the thin nitride-oxide lay[...]
 
Structure of sintered Ni-Ti-Fe shape memory alloys
 
Tomasz Goryczka  Barbara Szaraniec  Józe Flelątko  
Properties of NiTi shape memory alloy (SMA) are sensitive to any modification that can change the atom environment. It is due to the occurrence of the reversible thermoelastic martensitic transformation. This transformation is so called &#8220;civil" transition and proceeds by a correlated atom shuffle. Among the known modifications of NiTi properties there are changes in the chemical composition [1], thermomechanical treatment [2] and/or manufacturing technique [3]. First of all, the NiTi alloys are sensitive to changes in chemical composition. The raise of titanium contents of 0.1 at. % increases the transformation temperatures of 10 degrees. Moreover, substitution of either nickel or titanium by third alloying element strongly influences thermal behavior. The third element can be use for controlling transformation temperatures, thermal hysteresis width, change of the transformation course and sequences as well as for increase the stability of the transformation temperatures [4]. For example addition of zirconium or hafnium increases transformation temperatures [5], whereas cobalt, iron or aluminum decreases of their values [6]. Copper reduces [7] while hafnium [5] broadens thermal hysteresis of the martensitic transformation. In comparison to a binary NiTi alloy, addition of iron or cobalt causes change in the course of the martensitic transformation. In the NiTi alloy the B2 parent phase transforms directly to the B19´ monoclinic martensite. In ternary NiTiFe or NiTiCo alloy this transformation is preceded by additional phase transition - the R-phase transformation [8]. It is worth to note that the B2-R-B19´ transformation sequence can occur without any special thermal or thermo- -mechanical treatment. In order to directly influence the martensitic transformation the nonconventional production techniques such as powder metallurgy (PM) [9], melt-spinning (MS) [9] or twin roll casting (TRC) [10] for manufacturing the NiTi-ba[...]
 
Structure, thermal and magnetic properties of ferromagnetic Co-Ni-Al alloys
 
Wojciech Maziarz  Jan dutkiewicz  Aleksandra kolano-burian  Ritta szymczak  
Ferromagnetic shape memory alloys (FSMAs) are being intensively studied because of their potential applications as smart materials. Martensitic transformations and lattice reorientation processes in FSMAs can be triggered not only by changes in temperature and stress, as in conventional SMAs, but also by applying an external magnetic field. The martensitic phase transformation of the ferromagnetic Co-Ni-Al alloy systems has been studied in several papers [1÷5]. The Curie and the martensitic transition temperatures of the &#946; phase increase and decrease with increasing the Co content, respectively. The shape memory effect proceeds due to the thermoelastic martensitic transformation from the B2 parent phase into the martensite phase with L10 structure. The unique properties of the Co-Ni-Al alloy system is an improved ductility allowing hot rolling and cold rolling of a presence of &#947; phase with fcc structure. The &#946; single-phase polycrystalline alloys show a poor ductility [2]. It has been reported that the hot fabricability of NiAl-based alloys could be improved by the introduction of &#947; phase [6, 7]. Since the composition range of &#946; phase exhibiting the FSM is located near the &#946; + &#947; two-phase region, the &#946;-based alloys are able to introduce the &#947; phase by suitable choice of composition and heat treatment temperature [1, 2]. Several percent of &#947; phase significantly improves the ductility of the Co-Ni-Al two-phase alloys, which is of great advantage for practical applications [8]. Compounds with a strong coupling between crystallographic structure and magnetism usually exhibit a magnetic field dependence of the structural transitions. A typical example is the Gd5(SixGe1-x)4 alloys (0.24 &#8804; x &#8804; 0.5), where a transformation from the paramagnetic monoclinic phase to the ferromagnetic orthorhombic phase can be induced either by cooling or by the application of a magnetic field [9[...]
 
Study of the properties of Al2O3-Ag nanopowders produced by thermal decomposition-reduction method and colloidal nanosilver impregnation
 
AGNIESZKA JASTRZ ĘBSKA  ANDRZE J OLSZYNA  ANTONI KUNICKI  
There is a great need for antimicrobial materials across many industries and disciplines. That is why silver nanoparticles have been the centre of great interest in recent years. Owing to their small size, silver nanoparticles present good chemical activity, which is size and shape dependent [1]. They also possess good antirheumatic and antiphlogistic properties. As well as silver cations, silver nanoparticles affect wide range Gram-positive, Gram-negative bacteria and fungi [2]. Furthermore, it is unlikely that microorganisms will acquire resistance toward silver nanoparticles, compared to other biocides like antibiotics [3]. As a result, the potential for nanosilver-doped materials is limitless. Silver nanoparticles have been investigated as an addition to various types of matrices, due to their antimicrobial properties. Currently most important applications in the medical field include: wound dressings [4], medical implant coatings [5], ultrafiltration membranes and antifouling materials [6]. Although such &#8220;free" nanoparticles are not suitable in most applications (e.g. wound dressings) because they can be subsequently removed from the material while using it. In case of those materials, it is crucial to incorporate silver nanoparticles permanently. However, this problem can be solved by using a support. Among all inert supports, alumina is the most promising one. For silver nanoparticles incorporation, only alumina porous sinters [7], spheres [8] or needles [4] have been applied. Owing to alumina nanoparticles small size, which is no greater than 100 nm, they present large surface area. They are also characterized as the most inert ceramic for human organism, which have a good biocompatibility [5]. Due to these properties, alumina nanoparticles can be used as a support for silver nanoparticles. OBTAINING ALUMINA -SIL VER NANO PARTICLES For the synthesis of nanosilver particles (20 nm) supported on the alumina nanop[...]
 
Surface modification of titanium subjected to hydrostatic extrusion
 
Krz ysztof Topolski  Halina Garbacz  Wacław Pachla  Krzysztof J. KurzydLowski  
The basic technology for producing large volumes of bulk nanocrystalline metals is based on the Severe Plastic Deformation (SPD) methods, which enable refining the structure from the micrometric to the nanometric level. The microstructural changes are accompanied by a significant improvement of the mechanical strength and hardness [1÷7]. One of the SPD methods is hydrostatic extrusion, employed in the present experiments, which has been proven to efficiently refine the grains in aluminum, copper, nickel and steel [8÷12]. Our earlier studies have shown that hydroextrusion can also be used for producing nanostructured titanium [13÷15] with an equivalent diameter of grains about 60 nm and substantially increased strength and hardness. The chief difficulty in producing nanocrystalline titanium by HE is that the reduction of the rod cross-section must be realized gradually in many passes. Other disadvantageous effects that occur during HE of Ti are: the high extrusion pressure, the recurrent elastic deformation, the stick slip effect (stepwise displacement of the material) and a considerable wear of the die resulting from the tribological conditions. The aim of the study was to reduce or eliminate these adverse effects, and thereby to optimize the hydroextrusion process of titanium. To this end the surface of titanium was subjected to various modifications. The beneficial effect of Ti-Al coatings was shown in our earlier publications [15, 16]. Even though the extrusion pressure was reduced, the Ti-Al layers underwent wear in a short time. In the present study, the Ti billets were covered with Al coatings of various thicknesses. The effect of these coatings on hydroextrusion process, the surface topography of the Ti products and their microstructure after the extrusion were investigated. The maximum strain was also determined that could be applied in a single and two extrusion passes. MATERIALs AND PROCESSING The material examine[...]
 
Synthesis and properties of hot-pressed Ti-Al-C-N materials
 
Leszek Chlubny  Jerzy Lis  Mirosław m. Bućk o  
Among many covalent materials such as carbides or nitrides there is a group of ternary compounds referred in literature as H-phases, Hägg-phases, Novotny-phases or thermodynamically stable nanolaminates. These compounds have a Mn+1AXn stoichiometry, where M is an early transition metal, A is an element of A groups (mostly IIIA or IVA) and X is carbon and/or nitrogen. Heterodesmic structures of these phases are hexagonal, P63/mmc, and specifically layered. They consist of alternate near close-packed layers of M6X octahedrons with strong covalent bonds and layers of A atoms located at the centre of trigonal prisms. The M6X octahedra, similar to those forming respective binary carbides, are connected one to another by shared edges. Variability of chemical composition of the nanolaminates is usually labelled by the symbol describing their stoichiometry, e.g. Ti2AlN represents 211 type phase and Ti3AlC2 - 312 typ. Structurally, differences between the respective phases consist in the number of M layers separating the A layers: in the 211&#8217;s there are two whereas in the 321&#8217;s three M layers [1÷3]. The layered, heterodesmic structure of MAX phases led to an extraordinary set of properties. These materials combine properties of ceramics like high stiffness, moderately low coefficient of thermal expansion and excellent thermal and chemical resistance with low hardness, good compressive strength, high fracture toughness, ductile behavior, good electrical and thermal conductivity characteristic for metals. They can be used to produce ceramic armor based on functionally graded materials (FGM) or as a matrix in ceramic-based composites reinforced by covalent phases [4]. This work was focused on synthesis of three materials in Ti-Al-C-N system, namely Ti3AlC2, Ti2AlN, Ti3Al(C, N)2, by the Self-propagating High-temperature Synthesis (SHS), than obtained powders were hot-pressed and some of their properties were examined. PREPARATI[...]
 
Synthesis and properties of magnetorheological fluids
 
JOANNA KOZŁOWSKA  MARCIN LEONOWICZ  
Magnetorheological fluids (MRFs) belong to a group of smart materials, which have the ability of &#8220;intelligent" response to external stimuli. In the case of MRFs external factor is magnetic field. MRFs contain micrometric size magnetic particles, randomly distributed in non-magnetic liquid, which usually is synthetic or natural oil, water etc. The change of rheological parameters under magnetic field is called magnetorheological effect. MRFs were discovered by Jacob Rainbow in 1948 y. However, more extended interest in MRFs occurred at the end of XX century, when advantages of their potential application were noticed. The considerable interested in MRFs arise from their unique ability of rapid and reversible changes of rheological properties. Applications of MRFs include actuators, shock absorbers, dampers, brakes and clutches [3÷6]. MRFs are composite materials that basically consist of three components: -- filler material - magnetically polarizable particles, which provide the magnetorheological effect, -- carrier fluid, having a function of dispersing medium, -- stabilizer - protecting the particles from agglomeration. Factors that influence properties of MRFs can be classified into two groups: 1. Extrinsic factors: -- strength of magnetic field, -- shear rate, -- temperature. 2. Intrinsic factors: -- type of magnetic particles, their saturation magnetization and coercive force, -- size of magnetic particles and particle size distribution, -- volume (mass) fraction of components, -- carrier liquid type, its viscosity and thermal stability, -- stabilizer type. In order to increase the yield stress capability it is necessary to have a higher percentage of metal powder to support the chain structure in a magnetic field [1]. The saturation magnetization of the particles should be high enough to achieve strong magnetorheological effect. Moreover, low coercivity of the magnetic particles is required to ensure reversi[...]
 
Synthesis of magnetic nanocrystallites in carbon matrix
 
Ewa Szmidt  MARCIN LEONOWICZ  MARTA IZYDORZAK  Elżbieta Jezierska  
Nanoscopic magnetic systems attract substantial scientific attention due to the unusual properties which differ them from their bulk counterparts. In the consequence of reduced dimensions increases overall magnetic anisotropy of the particles, which is accompanied by decrease of the magnetic moment and Curie temperature. Magnetic nanostructures exhibit several new phenomena, which do not occur in bulk magnetics, such as superparamagnetism, magnetic quantum tunneling, giant magnetoresistance, exchange bias, spin torque, spin Hall effect and other. Magnetic nanoparticles can exist as individual nanocrystallites [1] or be dispersed within beads [2÷7]. Their properties depend on the size and nature of magnetic interactions. Single domain particles, below certain critical size, usually 5÷15 nm, may exhibit superparamagnetic properties, in which remanence and coercivity goes to zero and saturation magnetization is the same as in the ferromagnetic ordering. Such nanoparticles do not &#8220;stick" together in the absence of the magnetic field, however, they still agglomerate tending to reduce the surface energy. Thus, synthesis of magnetic nanoparticles within larger beads, where they are separated within a matrix, seems to be a proper solution. The characteristic magnetic properties of nanostructures predispose them for various new applications, mostly in electronics and medicine. Biomedical applications are rapidly growing areas of applications for nanosystems and comprise magnetic resonance imaging [8, 9], hyperthermia [10], targeted drug delivery [11÷15], tagging of biological nanomaterials [16, 17], biological sensors and several other. Wide application of magnetic nanosystems is possible due to the rapid development of fabrication and characterization techniques. Among the former one can mention vapour deposition, solution chemistry, elektrophoretic deposition, arc discharge and other. In this study magnetic nanocrystallites we[...]
 
TEM analysis of creep mechanisms of single-crystalline nickel-base superalloys
 
Beata Dubiel  Aleksandra czyrska-Filemonowicz  
Single crystal (SC) superalloys are especially designed for gas turbine blades in jet aircraft engines and stationary turbines generating electricity. The basis criterion in material selection for gas turbine blades is a high creep strength, because they have to withstand centrifugal forces acting during operation. The main creep mechanisms in polycrystalline superalloys are: -- dislocation creep by combined slip and climb of dislocations, -- diffusion creep by Nabarro-Herring or Coble mechanism [1, 2]. As it was shown for many superalloys [3÷5], in the range of temperature and stresses characteristic for service conditions of turbine blades, grain boundary diffusion by Coble mechanism is the main factor controlling the creep rate. Therefore the elimination of grain boundaries is necessary for improvement of creep resistance of superalloys. It can be achieved by a directional solidification with a grain selector, as was demonstrated first by B. Piearcey from Pratt & Whitney in 1970 [6]. Single crystal superalloys exhibit the highest creep resistance among metallic materials. The development of chemical composition of SC superalloys resulted in elaboration of four generations of these alloys [7, 8] and progress continues already towards the fifths generation [9]. The as-cast single crystal superalloys exhibit a dendritic structure with the eutectic areas between dendrite arms, which can be homogenized by heat treatment. The typical microstructure consists of about 70% of cuboid &#947;&#697; precipitates, about 400 nm in size, separated by &#947; matrix channels about 30 nm wide. Residual eutectic areas contain large irregular &#947;&#697; precipitates. Such two-phase microstructure guarantees the high creep resistance of single-crystalline turbine blades. The &#947;&#697; precipitates are an ordered Ni3Al-base intermetallic phase with the lattice parameter only slightly smaller than the Ni-base &#947; solid solution. This produc[...]
 
Texturization of polycrystalline silicon by metal assisted chemical etching
 
Marek Lipiński  
Cell reflectance is one of the factors influencing the efficiency of silicon solar cells. Therefore, the reduction of optical losses can significantly improve the efficiency of the solar cell. At present, the monocrystalline silicon wafers with (100) crystallographic orientation are textured by an anisotropic alkaline chemical etching. However, this method is not suitable for polycrystalline silicon due to different crystallographic orientations of the crystal grains. On the other hand, an isotropic acidic texturization based on a HF/HNO3 etching solution gives better results for polycrystalline silicon because every grain orientation is etched with the same rate. Unfortunately, isotextured mc-Si solar cells still suffer from high surface reflection. The new method of texturization is based on metal-assisted chemical etching (MAE). It was shown that MAE can produce the black silicon with very low surface reflectivity [1]. It is based on the deposition of metal clusters (Au, Ag, Pt, Pd) as catalyst for chemical etching in a solution containing HF acid and an oxidizing agent [1÷8]. In this work, palladium is deposited as a catalytic metal by immersing silicon wafers in PdCl2 aqueous solution [9÷12]. A metal assisted etching in HF:H2O2:H2O forms a porous Si. The consecutive chemical etching based on HF:HNO3 solution change the porous structure into the textured surface, which is more convenient for solar cells than the porous layer. EXPERIMENT AL AND RESU LTS Palladium clusters deposition The p type polycrystalline silicon wafers with resistivity &#961; of 0.5 to 2 &#[...]
 
The application of artificial neural networks in designing single-segment processes of vacuum carburizing
 
Piot r Kula  Emilia Wołowiec  
Today&#8217;s rapid technical progress of civilization and growing expectations of consumers forces equally fast development in all branches of the mechanical industry. It also concerns thermochemical treatment, in which traditional gas carburization is superseded by a modern technology of vacuum carburization . The reason for such a state of being is the high potential of carburizing atmospheres of vacuum carburization processes, which reduces both the time and costs of treatment of thermally improved machine parts. Nowadays, universal vacuum furnaces constitute basic technological equipment of state-of-the-art hardening plants as well as corporate divisions in charge of thermal treatment in the aviation, automotive, tool making and machine construction industries. However, as opposed to gas carburization, vacuum carburization is a much more complex process, which makes treatment with the use of this method more difficult to control, and hence, enforces more intensified control over the whole technological process. Therefore, in recent years, we have been observing increased demand for computer-aided tools (simulators) used to design and simulate these processes. A precise simulator requires an accurate model of a particular phenomenon simulated, which will be the core of its calculations; however, building such an accurate mathematical model is not always possible or affordable. The application of the artificial intelligence method, in particular artificial neural networks, is one of the ways to simulate the process of carburization without the necessity of creating a mathematical model [1, 11]. The following paragraphs briefly describe the essence and objectives of research on the possibility of applying artificial neural networks in the technology of vacuum carburization, the architecture of a sample neural network that achieves this goal and examples of vacuum carburization processes and single-segment processes meeting [...]
 
The application of grain size evaluation method on non-planar surfaces in the studies of aircraft engine turbine blades
 
STANIS ŁAW ROSKOSZ  
In polycrystalline blades of aircraft engine turbines, the size and shape of the grain constitutes one of the most significant quality control criteria of the casts made. In industrial practice, the macrostructure of the airfoil and the blade lock is evaluated in terms of the presence of equiaxial, columnar and frozen grains. The grain size has a significant influence on the mechanical properties, creep resistance as well as heat-resistance of the blades [1÷5]. It is impossible to directly measure the size of the grain due to the variable curvature of the airfoil surface. This requires measuring the grain size on a non-planar surface of the blade airfoil, on the basis of its perpendicular projection [6]. Research material The research material consisted of three polycrystalline blades produced from MAR M247, IN-100 and IN-713C alloys through investment casting at WSK &#8220;PZL Rzeszów" S.A. The blades differ from one other in their chemical composition, size and variable geometry of the airfoil (Fig. 1). Methodology To detect the presence of primary grains in the investigated superalloys, the airfoil surfaces were etched in a reagent of the following chemical composition: 18 g/l HNO3, 280÷320 g/l HCl, 151÷173 g/l FeCl3 (anhydrous) and 110 ml/l H2O. Before etching, the blade must be degreased; the etching time is 5 seconds (Fig. 1). To obtain an image of the airfoil projection, a stereoscopic microscope, Olympus SZX-9, was used. Images were recorded in polarized light at magnification of 10÷25×. Individual fields of view were recorded by means of a ColorView IIIu digital camera. The individual fields of view recorded[...]
 
The computer aided pressure casting die
 
Jacek Sawicki  Marek Górecki  Zbigniew Gawroński  Łukasz Kaczmarek  
The demand for improvement of the quality of products is characteristic of any purposeful human activity. One of the aspects of product quality is their reliability. At the same time, the prevailing belief is that the greatest possibilities to influence product durability exist at the stage of design. In die casting today, a global market for cooperation supplies has evolved where numerous companies of various sizes and with different technical equipment compete with one another. In order to meet the customers&#8217; requirement in the face of such fierce competition, the manufacturers of die castings must continually improve their products, lower their production costs and respond quickly and flexibly to new orders. A serious problem here concerns the process of quick design and manufacture of die casting dies and ensuring their high durability to achieve price competitiveness of the final product. This is a difficult engineering problem due to the highly individualised nature of the design and production of every die, as it is hard to draw on previous experience. Additionally, any optimization of the construction and technology of dies is complicated due to the complex nature of wear processes including: thermal fatigue, mechanical fatigue, erosion cavitation, dissolution of some components of die material by liquid metal, adhesion of the casting to the die, etc. Die durability largely depends on the correct selection of materials, heat treatment as well as the appropriately formed surface layer preventing the occurrence of macrocracks, and at the same time delaying the occurrence and propagation of thermal cracks for as long as possible. More and more experience drawn from practice proves the usefulness of such surface treatments[...]
 
The corrosion resistance of 7475 aluminium alloy processed by hydrostatic extrusion
 
EWA URA-BINCZYK  ALICJA BALKOWIEC  MAłGORZATA LEWANDOWSKA  KRZYSZTO F JAN KURZYDŁOWSKI  
High strength 7xxx aluminium alloys are commonly used in aircraft structure applications. Conventionally, they are precipitation strengthened which makes them the strongest among aluminium alloys. The grain refinement down to nanometre scale offers an additional possibility to improve their mechanical properties as the yield stress is a linear function of inverse square root of grain size (Hall-Petch relationship). The efficiency of such an approach was already confirmed in a number of studies [1, 2]. The size of grains can be efficiently refined down to nanoscale via a number of processing routes, among others utilizing severe plastic deformation. Such a processing enables micrograined aggregates to be transformed into nanograined via accumulation and rearrangement of defects, primarily dislocations, generated during the deformation. Experimental observations showed, that for such a transformation to take place, a large degree of plastic deformation is required, which usually exceeds the maximum equivalent strain achievable in simple plastic forming methods [3, 4]. As a result, special deformation methods have been developed, e.g. equal channel angular pressing and high pressure torsion. Also, it was recently demonstrated that hydrostatic extrusion (HE) can be used to efficiently refine the grain size in a number of metals and alloys [5, 6]. In comparison to the other SPD methods, HE usually requires a significantly smaller total strain. This is primarily due to the high strain rates, which frequently exceed 102 s-1 and reduce the extrusion time to seconds. As a result, the work associated with plastic deformation is more efficiently transformed into the energy of the accumulated defects. It was already established that nanograin refinement in SPD metals results in a high strength not possible to obtain by other strengthening mechanisms. However, it should be noted that wider industrial applications of these materials are res[...]
 
The degradation of mechanical properties of Al-Si5-Cu2-Mg and Al-Cu4-Ni2-Mg alloys after soaking at high temperature
 
Małgorzata Wierzb ińska  Jan Sieniawski  Grażyna Mrówka-Nowotnik  
The application of aluminium alloys for aircraft industry is determined by their properties - low density and high relative mechanical strength (Rm/&#948;) in particular, good electrical and thermal conduction, and very good technological properties - castability and plastic deformability. The progress of engineering and science in all aspects of world aviation is inseparable connected to production and application of aluminium alloys characterized by lower density and better mechanical properties than other applied alloys. The casting aluminium- -silicon-copper alloys with magnesium addition are widely used in the aeronautical engineering. Silicon and copper (the main alloy additions) improve the technological properties (fluidity and lower solidification shrinkage), reduce the value of thermal linear expansion - important factor for pistons production, improve the wear resistance, tensile and fatigue strength. It is known that the addition of Mg and Cu facilitates the precipitation of fine Mg2Si and Al2Cu phases and therefore improves hardening [1÷12]. A great number of investigations have recently been devoted to the effect of Cu, Ag and Sn addition on mechanical properties of Al alloys. It was found that increasing of Cu contents causes increase in tensile strength and yield stress of alloys with no harmful effect on their plasticity. Due to technological problems occurring during processing (microcraks formation) the Al-Cu alloys are not used as a widely as Al-Si-Cu alloys. Nevertheless they are commonly used as a base material for multicomponents alloys. An example is quarternary Al-Cu-Ni-Mg alloys containing up to 4.5% Cu, 2% Mg and 2% Ni charcterized by very good thermal resistance to high temperatures. This is due to presence of intermetallic phases Al6Cu3Ni and Al2CuMg forming during primary crystallization and hardening process. The [...]
 
The effect of heavy deformation on the structure of Mg-AZ31 alloy at ambientand elevated temperatures
 
JAN BONARSKI  JAN POSPIE CH  
Constructional Mg alloys like AZ31 (96 wt % Mg, 3 wt % Al, 1 wt % Zn) reveal relatively low density (63% of pure Al density) together with good strength properties. However, their plasticity is low as well as deformability at room temperature, documented in the curves of nominal strain in dependence on relative strain shown in Figure 1. Their shape indicates that exceeding the instability point (maximum of the curve equivalent to Rm value) brings about nearly immediate failure of the specimen. It leads to the conclusion, that the ductility - a feature better describing deformability than elongation - is low. The deformability of Mg alloy increases significantly only at elevated temperature. The Mg&#8209;based alloys, like AZ31 or AZ91 alloy is usually hot-deformed with the use of conventional methods like extrusion at least at 300°C [1]. Low ductility of hexagonal metals at low temperatures caused by the deficiency of easy-activated slip systems decreases their chance to use a method of Severe Plastic Deformation (SPD) as a way of grain structure refinement. Since the deformation at high temperatures is accompanied by the recrystallization process (dynamic or static one), the advantageous effects of plastic deformation are removed. That is why, cold pressing through an angular channel using an ECAP (Equal Channel Angular Pressing) method has become recently very promising when stable structure refinement using SPD is to be achieved. The ECAP is a process of intensive plastic deformation, in which the material is extruded with change of deformation path in the angular channel [2], where it is subjected to shear maintaining the dimensions of the cross&#8209;section. The mentioned already change of the deformation path as well as a generated strong hydrostatic component of the strain field, is used in the ECAP process to prevent from formation of cracks in conditions of strong external constraints. The method enables to process r[...]
 
The effect of lattice distortion on the course of the martensitic transformations in NiTi shape memory alloys
 
Danuta Stróż  Dariusz Chrobak  
In the Ni-Ti system it is the B2 intermetalic NiTi phase that undergoes the reversible martensitic transformation to the B19&#8242; monoclinic phase. For an alloy of any composition (provided it ensures the B2 phase presence) cooled down very slowly the transformation occurs always at the same temperature i.e. about 60°C. In the Ni-rich alloys the precipitation process may take place that changes the transformation characteristic temperatures and/or its sequence. There are several variants of this process depending on the ageing temperature [1], these are: &#946;0 &#8594; &#946;1 + Ni4Ti3 &#8594; &#946;2 + Ti2Ni3 &#8594; &#946;3 + TiNi3, Ta < 680 &#177; 10°C &#946;0 &#8594; &#946;&#8242;1 + Ni3Ti2 &#8594; &#946;&#8242;2 + TiNi3, 680 &#177; 10°C < Ta < 750 &#177; 10°C &#946;0 &#8594; &#946;&#8243;1 + Ni3Ti for Ta > 750 &#177; 10°C. However, the most significant influence on the course of the martensitic transformation in the NiTi alloy have the Ni4Ti3 particles. The strain fields around these coherent precipitates as well as the decrease of the Ni concentration in the matrix change the characteristic transformation temperatures and cause occurrence of the R-phase transition preceding the B19&#8242; martensite formation. Similar effects take place in the NiTi equiatomic alloys deformed and then annealed at temperatures below the recrystallisation temperature. In both cases additional effects in form of a multistage transformation were often observed. The first data on the multistage martensitic transformation were given by Todoroki and Tamura [2], Stróż et al. [3] and Zhu et al. [4]. It was found that depending on the applied thermal treatment there exist three or even four more or less overlapping peaks on the DSC cooling curves. The occurrence of the R-phase transition in these alloys is understandable as this transition causes less lattice distortions and thus is favoured when the internal stresses exist in the sample. Howeve[...]
 
The effect of metallic inter-layers on multilayer ceramic/metal coatings properties
 
Łukasz Major  Marcin Kot  Jürgen Lackner  
Wear resistant coatings are used to protect surface of industrial components working under high and constant wear loads. Within this group the ceramic hard coatings like titanium nitride (TiN) are of special interest in a number of technological fields due to their corrosion resistance and mechanical properties [1, 2]. The wear of hard coatings can change dramatically with adjustment of parameters like load, sliding speed, contact geometry and humidity. Cracks initiation and propagation are often responsible for wear. Nowadays it is a tendency to connect the properties of different type of materials, like for example combination of hard and soft phases in composite like coating or application of multilayer systems where soft (metallic Ti) and hard (ceramic TiN) interlayers are deposited in a sequence way [3÷5]. The Ti layers would allow extensive plastic deformation at crack tip and also, due to a lower elastic modulus compared to TiN, deflect the cracks. Consequently, multilayered Ti/TiN coatings display an improved fracture resistance as compared to homogenous TiN [6]. On one side the presence of plastically deformed metallic layers play an important role in cracks propagation mechanisms. Their presents can stop crack propagation, on the other side the decrease of the amount of this, metallic phase may have an influence on mechanical properties like for example hardness. The current work is focused on how the change of the ratio of ceramic phase to metallic one influence on the microstructure and mechanical properties of coating. Experimental The hybrid PLD (Pulsed Laser Deposition + magnetron sputtering) system equipped with high purity titanium target (99.9 at. % Ti) was used for deposition of Ti/TiN multilayered coatings. The details of deposition process is described in reference [7]. Two types of coatings (with differ[...]
 
The effect of structure on the stability of Al-Si coatings under salt mist conditions
 
Joanna Wróbel  Barbara Kucharska  Zygmunt Nitkiewicz  
The high corrosion resistance of Al alloys, as well as their sufficient heat resistance, have contributed to the use of these alloys for anodic protective coatings being applied on steels intended for, e.g., exhaust system elements. Developing coatings that would meet the ever-increasing operation parameters of cars is the subject of continuous research work. The new customer demands, technological solutions, and increasing car performance parameters are all urging the designers to use increasingly expensive steel grades with bettered mechanical parameters. However, a significant limitation on the wide application of stainless steels is the fact that, in spite of the absence of visible corrosion products, in acidified oxidizing media containing some anions, these steels undergo spontaneous, often localized dissolution. Due to the weight and economy of product, the basic element used for protective coatings in the automotive industry still remains to be aluminium [1÷4]. The problem of properly selected protective coatings is crucial in the manufacture of car exhaust silencers, because the whole exhaust system, in addition to mechanical damage during service, is exposed to aggressive chemical agents that accelerate the steel corrosion processes. At present, steels of a chromium content above 10% with an aluminium-silicon hot-dip coating applied are used for the manufacture of car exhaust systems. Exhaust system elements are formed in a stamping process. The main technological problem during their production from aluminium-coated steel sheet is to maintain the integrity of the coating. This problem has been partially solved by using silicon as an alloying element. However, it has been demonstrated in the author&#8217;s studies, that such coatings often exhibit an uneven arrangement and size of silicon crystals (as a result of the trade-off between the technical capabilities to produce a coating by the hot-dip coating method and th[...]
 
The elevated temperatures influence on the cobalt base cladding layer
 
Hanna Smoleńska  
Many structural components contemporary used in engines, gas turbine or industrial applications like for example: moulds for glass and ceramics, automotive valves, chemical and petrol-chemical valves, lamination cylinders, plastics extrusion screws and dies [1] are subjected thermal, mechanical and chemical loads at the same time. It needs materials which presented a good combination of strength and hardness properties, corrosion and thermal fatigue resistance and excellent fabrication. In modern technology hardfacing by producing surface coating is often used. Such surface coating can protect the parts from wear and, depending on coating material selection, from chemical or high temperature corrosion. Various processes such as spray and fusion, gas tungsten arc welding and submerged arc welding process are used to the clad the wear resistant layer. Among these different deposition techniques, plasma-transferred arc (PTA) is one of the most interesting processes because of its high deposition rate and low heat input and especially for its wide range of material which can be used [2÷8] also the deposits can be obtained with completely automated unmanned machines. During recent decades, the high-temperature oxidation on structural materials, such as Fe-, Co-, and Ni-base alloys, for which high-temperature oxidation resistance is an important parameter, has been investigated intensively. In general, these alloys developed good oxidation resistance by possessing proper amounts of Al, Cr, and Si and are called as alumina, chromia, and silica formers. For chromia formers, maximum protection against oxidation is obtained only if a continuous and coherent Cr2O3 scale layer is formed and maintained. That alloys must have a sufficient chromium content to initially form a chromium oxide and supply of chromium by diffusion within the underlying alloy in order to continuous growth of the protective scale. [9]. In spite of the long history [...]
 
The evolution of the gradient microstructure of the hard magnetic alloy FeCr30Co8 subjected to plastic deformation by tension combined with torsion
 
Anna Korneva  Galija Korznikova  Magdalena Bieda-Niemiec  Aleksandr Korznikov  Marek Faryna  Krzysztof SZTWIERTNI A  
The FeCr30Co8 alloy belongs to the hard magnetic materials of the Fe-Cr-Co system [1]. Due to its good ductility, the excellent magnetic properties and the low cost, it is used to produce permanent magnets of various sizes and shapes, as wires, tubes, bars, and strips [2, 3]. The high coercive state of the Fe-Cr-Co alloys can be obtained in the process of a magnetic treatment and multi-stage tempering, which resulted in a spinodal decomposition of an &#945; solid solution into isomorphous, ordered and coherent phases: magnetic &#945;1 and paramagnetic &#945;2 [4]. The formation of such a structure, where each precipitate of the &#945;1 phase (with sizes of about 50÷100 nm) appears as a single domain, provides high magnetic properties. On the other hand, the microstructure (&#945;1 + &#945;2) causes a reduction of the material&#8217;s plasticity and strength to the level of 200÷400 MPa. This is a serious technological problem, since the commonly used industrial magnets require strength greater than ~900 MPa. The brittleness and the low strength of hard magnetic alloys in a high-coercive (&#945;1 + &#945;2) state limit the possible range of their applications. It is known that the magnetic and mechanical properties are dependent on the microstructure: they are changing significantly with the decreasing of the grain size, to nano- or submicron scale, and with the alteration of the phase morphology or the phase transformation. All these modifications of the microstructure can be achieved by means of an intensive plastic deformation, which is considered as one of the methods improving the material properties [5, 6]. In order to achieve the refinement of microstructure with a gradient character, the FeCr30Co8 alloy was deformed by tension combined with torsion at 700, 750, 800 and 850°C. It is known that the gradient microstructure results in gradual changes of material properties. This can be beneficial in the case of magnets, which[...]
 
The influence of grain size of Ni3Al alloy on cavitation wear of Ni3Al intermetallic after cold rolling and recrystallization during incubation period
 
Dariusz Zasada  Zbign iew Zarański  Robert Jasionowski  
Unbeneficial phenomenon of cavitation is very common and can be observed in many fields of life. In particular, it appears in hydraulic machines and systems, and as well as in automotive and shipbuilding industries. Cavitation wear has been a subject of many publications and scientific works since the end of 19th century. However, recent state of knowledge of this phenomenon is still insufficient. Osborn Reynolds was the first who described this phenomenon in 1894. The meaning of term cavitation was taken from latin word cavitas which means cavern, void. Cavitation was firstly recognized as the reason of screw propellers and turbine rotors destruction at the turn of the 19th century. The first accurate definition of cavitation has been created in 20th century, and then material research as an attempt to full explanation of this effect has been introduced. Cavitation has been also noted in sliding vane-pumps, gear wheels, pipelines and fittings. Cavitational erosion is an effect of mechanical devastation of material, due to implossions of cavitational bubbles in the nearby or directly on material&#8217;s surface, what results in weight loss. Microbubbles serve as a cavitation embryos, which can be periodically recreated, due to release of gases from liquid. The effect of periodically repeated compression and implosion of gas bubbles is accompanied by rapidly changing impulses of pressure with value of even 1 GPa. Especially dangerous conditions can be achieved if microbubbles form cavitational clouds, which can lead to simultaneous implossion of large amount of bubbles and creation of very high pressure impulse. Formation of accumulative beam of liquid which moves with speed of 100 m/s, is also possible in critical conditions [1÷5]. Surface zone strengthening, microcracks, material loss and microstructure changes are appearing in the material as a result of continous impact of pressure pulses [6÷8]. Special attention has been f[...]
 
The investigations of Fe-Al phases formation arround SHS reaction in isothermal conditions
 
EWELINA POCHEĆ  STANISŁAW JÓŹ WIA K  KRZYSZTO F KARCZEWSKI  ZBIGNIEW BOJAR  
The process of Fe-Al phases formation has been the subject of interest for many years and it was described by many scientists. There are a lot of different theories explaining the mechanisms occurring during phases formation. One of the main theory was described by Deevi and Gedevanishvili [1]. They observed, that during the heating of Fe and Al powders mixture two exothermic reactions have occured. At temperature range of 540÷560°C the self-propagating high-temperature synthesis (SHS) [2, 6÷8] occurs and it is responsible for formation of the hard and fragile Fe2Al5 phase. Next reaction, at temperature range of 650÷670°C, leads to nucleation and growth of FeAl secondary solid solution. It is the effect of interaction between remaining iron and Fe2Al5 phase what was confirmed by Gao and coworkers [3]. Wei-Jen and Wang coated mild steel by hot-dipping in a molten aluminum bath and they obtained thin layers of FeAl3 and Fe2Al5 phases [4]. Whole set of phases in the Fe-Al system (FeAl3, FeAl2, Fe2Al5, Fe3Al and FeAl) was observed by other authors after sintering process and SHS reaction [5, 10, 17] The aim of this paper is to explain the phenomena occurs before and during SHS reaction. It is very important to describe phases transformations around SHS reaction, because they can influence the final structure of Fe-Al sinters. The obtained results showed that in sinter structure there are not only Fe2Al5 phase and aluminumlow Fe(Al) solid solution but also high-aluminum FeAl2 and FeAl3 phases, formed prior the SHS reaction. EXPERIMENTAL Elemental powders of 99.8% pure iron with an average particle size of 200 &#956;m and 99.6% pure aluminum with an average particle size of 70 &#956;m were mixed at a steichiometric ratio of 50 at. % Fe-50 at. % Al in a Uniball 5 mill (without milling balls) for 1 h. Than the cylindrical DSC specimens (3 mm in diameter and 20 mg in weight) were cold compacted uniaxially at a pressure of 700 MPa. Ob[...]
 
The microstructure of rapidly quenched Fe-Cu-based alloy with a liquid miscibility gap
 
Tomasz Kozieł  Zb igniew Kędzierski  Anna Zielińska-Lipiec  Jerzy Latuch  
Although superior properties of metallic glasses such as high strength and high elastic limit, its application is very limited due to highly localized shear banding [1, 2] and thus very low ductility. Ductility of metallic glasses could be improved by formation of composite materials consisting of crystalline phases dispersed in the amorphous matrix. Such composites might be produced by in-situ formation of the crystalline phase. In 2004 Kündig et al. [3] for the first time showed two-phase amorphous structure in metallic system. The system he studied included one pair of elements with high positive heat of mixing (La- Zr) while negative heat of mixing of the other elements (Al, Cu, Ni) to both, La and Zr. Positive heat of mixing between two major elements forced liquid phase separation into La-rich and Zr-rich melts during cooling of the homogeneous melt below critical temperature required for decomposition. Negative heat of mixing of the other alloying elements to La and Zr, increased glass forming ability of both separated melts. Rapid cooling enabled formation of two glassy structures, La-rich and Zr-rich, with surface fractal microstructure [3]. This work initiated research of systems based on elements with positive heat of mixing and thus possible formation of two amorphous phases. Several two-phase metallic glasses were reported up to date including Y-Ti-Al-Co [4], Ni-Nb-Y [5], Ag-Cu-Zr [6], Cu-Zr-Al-Y [7] and Nd-Zr-Al-Co [8]. Since two-phase amorphous structure was obtained, one can expect different thermal stability of both glassy phases. Thus formation of amorphous-crystalline composites with nanocrystalline structure is possible by partial devitrification of one of the amorphous phases. This work deals with another system based on two elements, namely Fe and Cu, with positive heat of mixing as high as +13 kJ/mol [9]. Although the Fe-Cu phase diagram does not contain a liquid miscibility gap, Turchanin et al. [10] p[...]
 
The process of glow discharge assisted oxynitriding of titanium alloy in aspect of its application in artificial heart components
 
Tomasz Borowski  Agnieszka Sowińska  Maciej Ossowski  Elżbieta Czarnowska  Tadeusz Wierzchoń  
Medical industry is constantly searching for new biomaterials, that may meet the requirements connected with their application. The best biocompatible metallic materials are titanium and its alloys which besides their good biocompatibility have low density and high mechanical properties [1÷4]. They are widely used for among others osseous implants, osseous fixation elements, pins, plates and screws, elements of dental implants and medical instruments [5]. In order to improve resistance to frictional wear, corrosion resistance and fatigue strength, as well as to eliminate occurrence of metalosis and improve biocompatibility of titanium materials various methods of surface engineering are successfully applied [1, 6÷8]. Application of surface engineering methods to give antithrombogenic properties to titanium alloys used in artificial heart or other components contacting with blood is a new challenge. The latest research shows that titanium oxide is a prospective hemocompatible material. Most of currently conducted research works dealing with hemocompatibility of titanium oxide regards layers made on polyurethane, polyethylene or pyrolytic carbon (LTI-carbon) substrate. Examination of hemocompatibility of oxide layers produced on siliceous substrate with a method of plasma immersion ion implantation and deposition (PIII-D) revealed better biocompatibility of these materials in contact with endothelium cells as well as antiadhesive properties of layers of crystal structures in comparison with layers of amorphous structure [9, 10]. Various methods of oxide layers modification are being searched for. For example doping with lanthanum oxide impurities La2O3 of TiO2 layer made with an application of RF-magnetron sputtering method on silica substrate considerably increases hemocompatibility of produced layers and reduces coagulation of blood platelets [11]. Successful attempts of improving biological properties of pyrolitic low tempera[...]
 
The zinc coating solidification on surface silicon steels and DI castings
 
Dariusz Kopyciński  Edward Guzik  aldemar wo łcz yński  
[...]
 
The zinc coating solidification on surface silicon steels and DI castings
 
Dariusz Kopyciński  Edward Guzik  Waldemar Wołczyński  
Hot dip galvanizing of reactive steels with high silicon content is a very interesting problem still lacking a complete and practically acceptable solution, although the currently used practice of steel making forces in a way the use of high silicon levels. An important issue in hot dip galvanizing is the phenomenon of the formation of a thick, brittle and dull-grey coating when the content of silicon (and phosphorus) in steel exceeds the critical but quite commonly used level, expressed by equation (1): (Si + 2.5P)&#183;103 = ESi,P (1) Below this value, the obtained coating is characterized by a correct glossy finish and ,,normal" thickness, while above the critical level of silicon and phosphorus equivalent the coating loses its adhesive force and as such can have poor adhesion, which means that the zinc volume necessary to produce the finally required coating thickness may be too large and therefore too expensive. As follows from the studies described in [1÷4], the chief solution to the problem of a wide range of the silicon and phosphorus equivalent values in steels (so more in cast iron) available at present in the domestic market seems to be a conformity certificate specifying precisely the composition of the steel used for elements which are to be subjected to the galvanizing treatment or proper selection of steel already at the stage of designing or making these elements (as far as it is possible). Procedure of this type should be effectively implemented in the galvanizing plants which use a wide spectrum of different steel grades, while the plants which make on request galvanizing of single elements should try to optimize the composition of the zinc bath they commonly use. Recently, some novel solutions have been offered in the field of hot dip galvanizing. One of them, widely used by industry, is the process of zinc-nickel galvanizing [5÷8]. The process of hot-dip galvanizing in Zn-Ni bath is at present considered to[...]
 
Thermal stability of Ni3Al-based intermetallic alloys structure upon long-lasting annealing
 
Paweł Jóźwik  Wojciech Polkowski  Zbigniew Bojar  
Intermetallic alloys present a group of intensively investigated hightemperature structural materials. A lot of work has been focused on Ni3Al-based alloys. Due to large aluminium content and high degree of structure ordering, these alloys posses some advantages over actually applied nickel-based superalloys [1]: -- much better oxidation and carburization resistance at temperature up to 1100°C, -- good mechanical strength at high temperature (with effect of an anomalous temperature dependence of yield strength), -- excellent wear resistance, also at high temperature, -- relatively low density and costs of raw materials. However, the main drawback in wide commercialization of Ni3Al-based alloys (and other intermetallic-based materials) is their low fracture thouhgness and, related with that, problematic manufacturing and processing of these materials. The problem of Ni3Al-based alloys brittleness has already been prominently reduced by the modification of chemical composition (e.g. by alloying with small amounts of boron and zirconium [2, 3]) and development of effective manufacturing technologies [4], what has resulted in few successful industrial applications of these materials [5]. The current applications of Ni3Al-based casting alloys include, e.g. heat treating trays and fixtures for carburizing and air environments, transfer rolls for austenitizing furnaces, forging dies and special components. Additionally, Ni3Al-based alloys in the form of cold-rolled thin foils (with thickness even below 50 &#956;m) are considered as promising substrate material for applications in microelectromechanical systems (MEMS). Ni3Al thin foils formed in so-called honey-comb structures can also be applied in electrochemical systems such as catalytic production of hydrogen from methanol system [6]. Neverthless, an quantitative description of relationship between structure and properties of Ni3Al-based alloys is rather difficult, due to their h[...]
 
Thermodynamics of Cu-Sn-X (X=Bi, Nb, Sb, Zn) liquid alloys
 
Jolanta Romanowska  
A fundamental goal in materials science is to be able to control the final physical or chemical properties of a material. In order to do that one must understand the relations between raw materials, their chemical composition, processing conditions, microstructure and properties of the final material. During processing, and often in use, most materials undergo reactions and phase transformations. This is particularly obvious in melt processing where materials are completely or partially melted and then solidified. Phase diagrams are the fundamental aid for understanding interrelations between chemical composition, processing conditions and microstructure. Since a phase diagram is a representation of the thermodynamic properties of a system it is possible to calculate it, unless the thermodynamic properties are known. By combining the knowledge on the phase diagram and the thermodynamic properties a model description of the system suitable for phase diagram calculations can be created. Descriptions of low order systems can be combined to make extrapolations to higher order systems. For this purpose the Gibbs energy of each phase is described by a suitable model containing a relatively small number of variable coefficients. The thermodynamic properties of a binary system can be calculated using the Gibbs free energy expression comprising contributions of both elements in each phase existing in the system. Further parameters are introduced to describe the mutual interaction between elements in each phase. Difficulty in extension of the calculated results to higher order systems is much less than in the case of experimental work, since the essence of the calculation does not change so much between a binary system and a higher order one [1]. Sometimes, due to the lack of experimental data for ternary systems, parameters for ternary systems are calculated on the basis of values for binary ones and different simplifications and models[...]
 
Transport properties of nanocrystalline and microcrystalline Gd-doped ceria
 
Guido Baldinozzi  Mickael Dolle  Jan Kusiński  Claude Petot  Georgette Petot-Ervas  
Solid oxide fuel cells (SOFC) are regarded to be amongst the cleanest and most efficient technologies for chemical-to-electrical energy conversion. However, to be economically competitive it is necessary to lower their operation temperature in the range 500÷600°C. This provides several advantages, including lower degradation rate of both components and cell performances and lower fabrication cost through the use of less expensive materials for interconnections, heat exchangers and structural components. To realize the lowering of the operation temperature, there are different options, the use of thin-film electrolytes or new solid electrolytes with high ionic conductivity, for instance, because this component is the main material of SOFC, whose structure and properties affect directly the fuel cell efficiency. Ceria based oxides have been considered as one of the most suitable alternative [1÷3] to yttria stabilized zirconia (YSZ), the solid electrolyte utilized up to the present time in conventional SOFC, operating at around 1000°C. This is due to their higher oxygen-ion conductivity (0.025 &#937;-1cm-1 at 600°C) compared with ZrO2-based materials (<0.005 &#937;-1cm-1). Furthermore, these oxides enhanced electrode reactions due to an electrocatalytic effect via the Ce+3/Ce+4 couple, resulting in a mixed conductivity zone at the electrode level (solid electrolyte/electrode material interface) which leads to a decrease of the electrode resistance. Recently, the use of nanocrystalline polycrystals was considered as a promising approach to improve even more fuel cell performances. Indeed, given the high surface-to-volume ratio of nanoceramics, these materials possess a wide range of original properties [2÷6] due to the high grain boundary density and interfacial surface, such as enhanced mechanical properties and chemical reactivity. To date, the impact of the reduction of grain size from the microcrystalline range into the nanocr[...]
 
Tribological behaviour of Fe-Al intermetallic coatings obtained by HVOF method
 
Cezary Senderowski  Zbigniew Bojar  Bolesław Formanek  Krzysztof Szymański  
One of the current challenges in materials science is to find versatile materials able to withstand a good resistance for different service performance situations. Currently, intermetallic compounds are being investigated as a good compromise for the good mechanical properties, corrosion, oxidation and wear resistance. Much attention has been paid to iron-aluminium (Fe-Al) intermetallic compounds because of their potential applications as either high-temperature bulk materials or coating materials. They show relatively high melting points, high thermal conductivity, relatively low density and low cost as well as excellent anti-oxidation and anticorrosion properties as compared with Fe and Ni-based superalloys [1÷3]. Especially, FeAl intermetallic compounds containing 35÷50 at. % Al possess good resistance to oxidation and sulfidation corrosion, due to formation of protective alumina scale at elevated temperature in aggressive working conditions [3, 4]. Its applications include, among others, molten salt systems for chemical air separation, automotive exhaust systems and coal conversions systems. In a previous study, the oxidation behaviour of HVOF and Dgun sprayed FeAl coatings was already reported [5, 6]. Xiao et al. [3] reported that the sulfidation resistance of HVOF sprayed FeAl coating can be effectively improved by doping with CeO2 at an optimum dosage of 2÷5 wt. %. Iron aluminides have been also proposed lately as promising materials for wear applications. Many researches [7÷11] have focused their attention on the friction behaviour of FeAl coatings, emphasizing the role of the Fe-Al type intermetallic phase as a new matrix to embed ceramic particles and replace the extensively studied WC-Co cermet system for abrasive environments in high temperature. Friction has been the most investigated mechanism and delamination was found to be the predominant cause for volume loss in coatings [7÷9]. The other two wear mechanisms, [...]
 
Ultra-fine grain structure of AA3104 alloy analyzed by TEM and SEM orientation mappings
 
Henryk Paul  Thierry Bau din  Anna Tarasek  
It has been frequently shown that the application of electron backscattered diffraction (EBSD) and high resolution scanning electron microscopy (SEMFEG) to structure and texture analyses of cold deformed and/or lightly annealeded materials gives reasonable results only up to moderate strains (~1.5). In the case of higher deformations, the resolution of SEM/EBSD technique is not always sufficient. The application of systems of local orientation measurements based on transmission electron microscopy (TEM) is one of the ways towards the solution of the problem. Because of the good spatial resolution (which is usually estimated to be below 10 nm [1]) and the accuracy of orientation determination (better than 0.1°) the local orientation measurements in TEM appears to be the suitable method for the investigation of fine grained structures. Recent studies leading to designing a fully automatic TEM system are focused on automatic indexation of transmission Kikuchi bands, e.g. [2÷5]. The application of fully automatic indexing in TEM is more difficult than in the case of SEM mainly due to smaller acquisition angle and higher indices of the diffraction planes as well as because of poorer quality of diffraction patterns. The latter &#8216;parameter&#8217; depends not only on the dislocation density (surface strains) but also specimen thickness. Moreover, according to Schwarzer [2] the accuracy of the system by the use of automatic indexing was proved up to 0.5°, whereas it is only 0.1° by manual indexing. Thus manual indexing is still widely used for accurate determination of crystallographic orientations. They are other problems related to the acquisition time and long range drift. The pattern acquisition is still the main factor determining the time needed for map creation (usually ~25÷30 patterns per minute). Additionally, the intensities in the original patterns significantly decrease with the distance from the center of the image. Th[...]
 
Ultrasonic method applied to defects identification in the forging ingots
 
Józef KOWALSKI  Jolanta DEDA  Anna Maria JANUS  Robert MARTYNO WSKI  Waldemar WOŁCZYŃSKI  
The typical massive forging ingots produced in the steelwork has a mass of about 10÷100 T (Fig. 1). According to the technology of casting a porosity is expected along the ingot axis (Fig. 2). Each forging ingot is subjected to an ultrasonic test at a production line. But the result of this kind of industry test are not evident. In the case of the ingot of the mass about 12 T the acoustic signal indicated porous less than 1 mm longue (reduced distance). However, in the case of the ingot of the mass about 50 T the acoustic signal was completely damped by the grains boundaries so that no results of acoustic measurement were obtained. Therefore, some additional tests have been made by means of the light microscopy (LM) and scanning acoustic microscopy (SAM) for six samples along a given radius of the ingot shown in Figure 1. EXPERIMENTAL The results of the microstructure observation are shown in Fig. 3. A morphology of a one defect can be shown in more details (Fig. 4). The light microscopy is not able to reveal all the details of morphology of some single defects as these shown in Figures 3 and 4. Therefore, an attempt to identify the details of some defects was done by the scanning acoustic microscopy (Fig. 5, 6, 7a). Identification of the defects is performed by the SAM technique through density analysis of the different sample sublayers (Fig. 6). Microscope reveals a defect by comparison of the difference between density of bulk sample and density of a given defect. It is possible because scans can be made at different fixed distances. &#727; Fig. 1. Massive forging ingot produced in the steelwork Rys. 1. Masywny wlewek kuzienny produkcji hu[...]
 
XRD investigations of electrodeposited Ni and Ni/Al2O3 coatings
 
ANNA GÓRAL  EWA BEŁTOWSKA-Lehman  
Recently, metal matrix composite (MMC) coatings containing ceramic particles have been widely investigated due to their enhanced material properties (i.e. higher hardness, wear and corrosion resistance) compared to the pure metal or alloy [1÷4]. The MMC properties depend mainly on the type, structure, shape, size, morphology and content of the inert ceramic particles as well as on their distribution in the metal matrix. Several metals, e.g. nickel, copper, gold, chromium have been mainly used as a metal matrix, whereas metal oxides, carbides, borides and polymers were the co-depositing particles [5]. Electrolytic nickel coatings exhibit specific properties as hardness, durability, good corrosion resistance and catalytic activity in many electrochemical processes [6]. The addition of hard ceramic particles into Ni matrix can improve its hardness and wear resistance. These phenomena are mainly attributed to the hardening of the metal matrix by finely dispersed ceramic particles [7]. Al2O3 particle has many superior properties, such as low price, good chemical stability, high microhardness wear resistance at high temperature [8]. Insoluble particles are suspended in a conventional electrolytic bath and embedded in the growing metal during co-deposition process. The Ni/Al2O3 nanocomposites are one of the most promising materials, that can find wide engineering application as coatings of engine cylinders, high-pressure valves, car accessories, aircraft microelectronics etc. [9÷10]. Functional properties of electrodeposited composites are mainly controlled by their composition and structure. Among others, they depend strongly on their microstructure, residual stresses and due to the anisotropic properties on the distribution of crystallographic orientation. It is widely accepted that the state of residual stress on the coating surface and in the near surface area is one of the most important parameters of surface deposit quality. Mac[...]
 

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