No 1 (2019)
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On the 85th Anniversary of Academician V.N. Antsiferov
8-13 688
Abstract
The paper discusses the further development of some ideas of V.N. Antsiferov and the scholar school created by him in obtaining structural powder materials and products. The prospects for obtaining concentration-inhomogeneous steels and trip-steels are noted. The great potential lies in the control of the thickness and volume of the zone of deformation martensitic transformation occurring during fracture. It is advisable to continue the preparation of fullerene- and nitrogen-containing powder compositions and to study the structural heredity of powder steels. The possibility of the synthesis of fullerene-containing phases during the liquidphase sintering of the iron–cast iron and iron–graphite compositions and their subsequent redistribution in the bulk of the material during dynamic hot pressing is worth noticing. Producing nitrogen-containing steels by mechanical activation of powders followed by sintering in dissociated ammonia is advisable to use for obtaining not only wear-and corrosion-resistant materials, but also heat-resistant ones. The studies on the decomposition of supercooled austenite in powder steels of various doping systems with different technological backgroung (sintered, hot-deformed, infiltrated, etc.) are promising. The potential for development is the research of hot-deformed concentration-inhomogeneous materials, obtained, in particular, on the basis of powders of the Distaloy type. The techniques developed by the Antsiferov’s school are significant. The most important one is the method for determining the concentration variation coefficient, as well as a magnetometric complex and a mathematical model, which makes it possible to predict the decomposition of supercooled austenite. Antsiferov’s works can be used for obtaining lean powder steels with the lower bainite structure, which provides the optimal combination of strength and toughness.
Production Processes and Properties of Powders
14-21 1029
Abstract
The object of the study was alloy powders KhN60М (EP367; 06Kh15N60М1). An overview of methods for manufacturing products from heat-resistant alloy KhN60M with an analysis of their advantages and disadvantages is given. It is shown that in comparison with injection molding and hot pressing of powders from high-alloyed special steels and alloys, additive technologies allow to obtain products of complex shape with a high level of physical and mechanical properties and material utilization. The low casting properties of the alloy under study cause the research of the atomization to meet the requirements for size, shape, morphology and fluidity of powders for additive technologies. The goal of the work was to study the effect of argon pressure during gas atomization on the physical, chemical, technological properties of powders for laser surfacing, obtained from alloy KhN60М. The technology of gas spraying of liquid melt with argon on a VIGA 2B laboratory atomizer at a temperature of 1560 °C and varying the pressure of the spraying gas in the range of 22–25 mbar was used for the manufacture of metal powder KhN60М. To select the atomization parameters, the melt viscosity values were calculated using the finite element method and its temperature dependence was constructed. The calculations were made with the ProCAST computer modeling system for casting processes. The shape and size of particles, the grain size composition were investigated using laser sedimentation, electron and optical microscopy. Quantitative metallography data were processed using the VideoTest 4 software. Fluidity of powders was measured. It was found that with increasing pressure of the spraying gas, the proportion of spherical particles increased and the fluidity of the powders improved; Feret diameter, average particle size, and d50 values did not change significantly. An experimental dependence of the increase in the yield of the powder of the target fraction (40–80 μm) with a decrease in the volume of the spray gas supply was obtained. An inversely proportional dependence of the fraction of spherical particles on the fraction of the desired cut was established. The results of the study make it possible to predict the values of the output parameters of powders during the atomization of steel KhN60M. Characteristics of powders of the –80+40 μm fraction with a shape factor of 0.99 and a yield point of 14–15 g/s make it possible to use them for the manufacture of products using additive technologies.
Self-Propagating High-Temperature Synthesis (SHS)
T. L. Talako,
A. I. Letsko,
Yu. A. Reutsionak,
A. P. Abramchuk,
S. A. Oglezneva,
M. N. Kachenyuk,
A. A. Smetkin
22-29 819
Abstract
The dependence of the phase composition and parameters of the fine structure of titanium carbosilicide in powders obtained by the self-propagating high-temperature synthesis on the concentration of aluminum in the 5Ti/2SiC/1C reaction mixture was investigated. The aluminum concentration was varied in the range of 0.1–0.4 mole fraction while maintaining the total carbon content. It has been established that aluminum additives not only affect the yield of titanium carbosilicide, but also contribute to the predominant formation of Ti5Si3 instead of TiSi2 in synthesis products, which is identified in non-aluminum powders. The introduction of a small amount of aluminum (0.1 mole fraction) leads to the formation of a solid solution of Ti3Si1–xAlxC2 and reduces the content of impurity phases in SHS powders by 6 %. With a higher aluminum content in the reaction mixture, the concentration of carbosilicide in SHS powders decreases, and that of binary compounds (TiC, Ti5Si3, TiAl) increases accordingly. Within the concentration range of 0.1–0.25 mole fraction, no noticeable effect was observed from the introduction of aluminum on the crystal lattice parameters of titanium carbosilicide in SHS powders. A significant increase in the parameters a and c of Ti3Si1–xAlxC2 (from a = 3.067 Å, c = 17.67 Å to a = 3.07 Å, c = 17.73 Å) while maintaining the ratio with с/a within known values (с/a = 5.78) is observed only when the aluminum concentration is 0.4 mole fraction. The crystallite size of titanium carbosilicide depends primarily on the burning parameters. At the same time, the deformation of the Ti3Si1–xAlxC2 crystal lattice in SHS powders monotonically grows with increasing aluminum content in the reaction mixture in the investigated concentration range.
A. N. Astapov,
Yu. S. Pogozhev,
M. V. Lemescheva,
S. I. Rupasov,
V. I. Vershinnikov,
I. P. Lifanov,
L. N. Rabinskiy
30-41 944
Abstract
The work aims to obtain composite powder ceramics based on ZrB2–ZrSi2–MoSi2 by the self-propagating high-temperature synthesis (SHS) according to the scheme of magnesium thermal reduction from oxide raw materials, as well as its subsequent consolidation by hot pressing (HP). The combustion of the reaction mixtures is characterized by rather high adiabatic temperatures in the range of 2060 to 2120 K and burning rates in the range of 8,3 to 9,4 g/s. The yield of the end product with magnesiothermal reduction is 34–38 %. The resulting powder contains 13–47 % ZrB2, 21–70 % ZrSi2, 2–32 % ZrSi, and 10–18 % MoSi2 depending on the composition of the initial reaction mixture. It is characterized by high structural homogeneity and consists of composite particles of polyhedral shape with an average about 8 microns in size. The structure of ceramics consolidated by the HP method from SHS powder is homogeneous and includes ZrB2 needle grains distributed in a ZrSi2 matrix, MoSi2 inclusions of various morphology and ZrSiO4 silicate, distributed along the grain boundaries of ZrSi2. The samples obtained by HP are characterized by a high degree of homogeneity of the chemical composition and a residual porosity of 2,5–7,4 %.
Refractory, Ceramic, and Composite Materials
42-51 950
Abstract
Using chemical co-precipitation from inorganic precursors, powders based on ZrO2–7wt.%Y2O3 were obtained. Oxides of rareearth elements (REE) – La, Nd, Pr – were introduced into them in concentrated form from 5 to 15 wt.%. Using differential thermal analysis, it was found that an increase in the proportion of concentrate leads to a shift of the temperature maxima of thermal effects to high temperatures from 450 to 505 °C. The influence of the annealing temperature in the range of 600–1200 °C on the phase transformations of the synthesized powders of the ZrO2–7%Y2O3–REE system was studied through Raman spectroscopy. The results showed that their phase composition consists of tetragonal zirconium dioxide ZrO2 regardless of the concentrate content. The effect of sintering temperature on compaction of synthesized powders, phase composition and microstructure of ceramics was examined. It was found that ceramics with 10 % REE concentrate has the highest compaction speed during sintering, and an increase in the concentrate content to 15 % leads to inhibition of compaction during sintering. Ceramics with 15 % REE had the highest open porosity at all sintering temperatures. It was noted that for samples with 10 and 15 % REE concentrate, with increasing sintering temperature, a decrease in the intensity of the Raman spectra peaks and their broadening is observed. It is associated with the formation of a different type of tetragonal modification. The results of atomic force microscopy showed that after sintering at a temperature of 1350 °C in the structure of ceramics containing 15 % REE concentrate, in contrast to other compositions, a new phase with a faceting and a layered structure was detected.
52-60 78403
Abstract
Diffusion and homogenization in powder systems of varying degrees of dispersion «iron (5 μm) – nickel (5 μm or 50 nm)» during sintering (900 and 1000 °C), as well as spark plasma sintering using the Matano-Boltzmann method were studied. In these systems, the calculated diffusion coefficients in pairs of micron powders, sintered without application of pressure (900 °C, 6 h) and the spark plasma method (900 °C, 5 min), were equal to 7·10–10 cm2/s. It is shown that in diffusion pairs based on microdispersed iron powder, the use of nanodispersed nickel powder instead of microdispersed one contributes to an increase in the diffusion coefficient at a temperature of 900 °C by a factor of 2. The constants in the sintering kinetics equation of V.A. Ivensen are calculated for iron–nickel powder systems. Through them the factors activating the sintering of these systems were established. The dependences of the structure-phase composition and physicomechanical properties of carbides of the Fe (base) system — 14 wt.% Ni – 8 wt.% TiC system on the sintering temperature in the interval t = 900÷1200 °C, dispersion and homogeneity of the structure were determined. The dependences of grain size, porosity, hardness, microhardness, toughness, bending strength on sintering temperature are shown. The established dependences of the tribotechnical properties on the degree of homogeneity of the solid solution and the volume of the phase transformation of the metastable austenite to deformation martensite during friction on the abrasive were similar for carbide steels and diamond tools based on carbide steels. The optimal values of the coefficient of variation of nickel concentration in austenite in carbidostils of the same chemical composition, but different dispersion, providing the maximum amount of austenite decomposition and high values of the diamond tool grinding coefficient were 5 in both systems, but the sintering parameters differed. It is shown that the physicomechanical properties of the studied systems depend on the porosity and dispersion of the structure, and the tribotechnical properties are subjected to the homogeneity of the structure of the steel.
61-71 1231
Abstract
In the study of nanoceramics, it is necessary to constantly keep in mind the closest interrelation of the production method with its structure and properties. Nanoceramic materials are used in various technical fields as structural and functional materials. It is also widely used in medicine. Nanoceramics is harmless, stable and has a great affinity with living organisms. ZrO2-based nanoceramics have a lower elastic modulus than other oxide materials. The specificity of its application lies in high resistance to rupture and thermal shock, in chemical stability at high temperatures. However, it is necessary to solve the problem of increasing the fracture toughness of ZrO2-based ceramic materials. The complex doping of ZrO2 with yttrium and cerium oxides and the use of an Al2O3 additive increase the fracture toughness and decrease the negative effect of materials in a biological environment. In this paper, the main physicochemical properties of ceramic powders and materials of the ZrO2–2Y2O3–4CeO2 – Al2O3 system, synthesized by chemical deposition of inorganic precursors using the sol-gel technology, are considered on the basis of scientific data and experimental studies. The doping of pure zirconium oxide with stabilizing oxides Y2O3, CeO2, and thermal hardening of Al2O3 ensures that the tetragonal structure is maintained at room temperature, which makes it possible to slow down and control the crack resistance of the material under load. The effects of sintering temperature and aluminum oxide content on the microstructure and grain size, as well as the physicomechanical properties of the resulting ceramic material of ZrO2–2Y2O3–4CeO2+1 wt.% Al2O3 and ZrO2–2Y2O3–4CeO2+3 wt.% Al2O3 were studied.
Nanostructured Materials and Functional Coatings
72-81 779
Abstract
Surface preparation is a prerequisite for ensuring the required properties of a diamond film obtained by gas-phase deposition. The paper considers the effect of temperature and concentration of the etchant CuSO4 on the structural and phase composition of the surface of hard-alloy materials. The structural and phase composition of a continuous polycrystalline diamond film at its growth stages was also studied. Adhesion of the obtained diamond films to the surface of carbide materials was qualitatively determined. It has been established that surface treatment of a hard alloy in a CuSO4 solution at a temperature t = 23 °C leads to unequal removal of the cobalt bond with chipping of WC grains and the formation of a porous structure in the surface layer of the WC–6%Co alloy. The treatment with an etchant CuSO4 at t = –2 °С ensures uniform etching of the Co-bond along the WC grain boundaries and the formation of a chemically uniform surface. The orientational growth and adhesion of the diamond film depend on the elemental composition of the surface of the WC–Co alloy after treatment with a CuSO4 solution. If the treatment was carried out at a tsolution = 23 °C, then during the synthesis of the diamond film, the removal of copper from the defective surface layer of WC is difficult. This provides the multidirectional growth of diamond crystals in the film in two directions: <111> and <110>, which causes critical biaxial compressive stresses (2,5 GPa) and leads to low adhesion of the film to the surface of the hard alloy. If the treatment was carried out at tsolution = –2 °C, then the orientational growth of diamond crystals in the film occurs in one preferential crystallographic direction <111>. It reduces the biaxial compressive stresses (1,7 GPa) and increases the adhesive adhesion of the film to the surface of the hard alloy . The structure defect, calculated from the ratio of the lines of integrated intensities I1333 / I1580 using the Raman spectroscopy, decreases with concentration growth for negative temperatures and increases for positive ones of CuSO4 solution during surface preparation.
82-90 807
Abstract
The phase and structural transformations of a powder magnetically hard alloy of the system Fe–30%Cr–27%Co–1%Si–0,07%B with a metastable α1+α2 phase composition, a high content of cobalt, and a high level of magnetic properties were studied. The density and coefficient of variation of the concentration of the main elements of the sintered blanks at the level of deformable analogs are achieved by sintering in the α-phase with contact melting in the presence of a «vanishing» liquid phase formed due to the addition of silicon and boron ferroalloys. A kinetic approach to the development of a competitive hard magnetic alloy with a high proportion of the strongly magnetic phase is proposed. The effect of boron additions on the incubation period of the formation of an undesirable σ-phase and the temperature range of the concentration stratification of the α-solid solution on the strongly magnetic α1-phase and the weakly magnetic α2-phase were established. Optical microscopy, X-ray phase analysis and differential scanning calorimetry were used to determine temperature and time parameters of heat treatment of the alloy, including hardening, thermomagnetic treatment (TMT) and final aging, providing the required combination of Hc and Br by increasing the stability of the metastable α-phase up to 20 minutes in the interval temperatures of spinodal decomposition α → α1 + α2. The greatest increase in magnetic properties after TMT, observed at the 1st and 2nd steps of final aging, is related to the decomposition of the α-solid solution and the formation of subgrain boundaries. Elements of the obtained structure are characterized by submicron and nanometric sizes, which correlate with the research results on deformable alloys based on the Fe – Cr – Co system. The anisotropic α1+α2-structural state achieved by thermomagnetic treatment provided an increase in the magnetic properties of the studied 30H27KSR powder alloy to 30 % and the squareness coefficient of the magnetic hysteresis loop equal to 0,82 .
Materials and coatings fabricated using the additive manufacturing technologies
91-97 1126
Abstract
The objects of study were stainless steel powder 12Kh18N10T of the 20–63 μm fraction and experimental samples obtained on the basis of it by selective laser melting (SLM). The powder was obtained by spraying with argon at a temperature of 1640 °C and a pressure of 27 bar. The particles have the dendritic-cellular structure, with a decrease in their size (<35 μm), the cellular structure prevails, and the dendritic one almost disappears. The distinctive particle size is d50 = 37 μm, d100 = 67 μm. The differential distribution curve is close to the Gaussian form, and asymmetry is associated with satellite and the presence of a small number of particles less than 20 microns in size. The fluidity of the powder was 3,27 g/s, and the bulk density was 4,41 g/cm3. The density of the 12Kh18N10T steel samples grown at the Concept Laser M2 facility with a laser power of 180 W and a speed of 700 mm/s averaged 7,89 g/cm3. Since the density of compact steel is 7,95 g/cm3, the obtained material has enough high density. The microstructure of the 12Kh18N10T sample was described by continuity, the absence of pores and cracks. It was a solid solution of austenite. The average size of coherent scattering regions in the grain volume was 19 nm. The observed arcuate boundaries of parallel semicircular tracks are due to heat removal during crystallization through SLM. The elongated crystallites in the tracks are oriented inward from this boundary. The microhardness of the samples in the transverse plane of the thin section is higher than the microhardness of the planar plane. But the microhardness of the samples obtained from the powder by the SLM is higher than that of the standard compact alloy. Tensile strength and elongation are 651 MPa and 47 %, respectively. The increase in strength is probably due to the grinding of structural parameters in SLM. The fracture surface of the samples is characterized by a pronounced viscous type.
Application of Powder Materials and Functional Coatings
98-106 1280
Abstract
The analysis of trends and prospects for the development of the industry on the materials of European and world congresses of powder metallurgy, publications in leading specialized foreign publications was carried out. The steady growth of the production of powder construction parts for the automotive industry, including using assembly technology during joint sintering, are noted in the developed countries. The production using MIM methods is constantly growing; micro MIM technology has emerged as a separate sub-industry, which allows manufacturing products with a mass of 0,1 g or less. HIP methods found its second wind: with them it became possible to obtain large-sized blanks from corrosion-resistant steels weighing up to 1000 kg, titanium and high-temperature alloys; the post HIPing technology is widely used to improve the quality of products obtained by additive technologies and important castings. With additive technologies, products weighing up to 100 kg are already being manufactured. The authors also formulated their own opinion about the prospects for the development of powder metallurgy in Europe and in the world, determined the development directions of the industry in Belarus and its influence on the development of world powder metallurgy. In particular, new grades of economically alloyed powder steels are developed. They make it possible to reduce the cost of mass structural parts without prejudice to their technical characteristics. For the same purpose, processes combined with hardening of sintering are optimized, and, in contrast to foreign analogues, endogas is used for cooling instead of nitrogen.
ISSN 1997-308X (Print)
ISSN 2412-8767 (Online)
ISSN 2412-8767 (Online)