Pub Date : 2022-12-10DOI: 10.17073/1997-308x-2022-4-34-57
A. Amosov, Y. Titova, G. S. Belova, D. Maidan, A. F. Minekhanova
The application of the process of self-propagating high-temperature synthesis (SHS) to prepare highly dispersed powder nitride-carbide compositions from the most common refractory nitride (Si3N4, AlN, TiN) and carbide (SiC) compounds with a particle size of less than 1 μm is considered. The advantages of composite ceramics over single-phase ceramic materials and such trends of its development as the transition to nanostructured ceramics and the application of in situ processes of direct chemical synthesis of nanoparticles of components in the composite body are described. The attractiveness of the SHS process as one of the promising in situ processes characterized by simplicity and cost-effectiveness, the possibility of obtaining highly dispersed ceramic powders by burning mixtures of inexpensive reagents is shown. Considerable attention is paid to the consideration of the results of the application of azide SHS, based on the use of sodium azide and gasified halide salts as part of mixtures of initial powders of nitrided and carbidized elements during their combustion in nitrogen gas. The review of publications devoted to the application of SHS to obtain highly dispersed composite powders Si3N4–SiC, AlN–SiC and TiN–SiC, promising for use in sintering of the corresponding composite ceramic materials of submicron and nano-sized structure with improved properties, lower brittleness, good machinability, lower sintering temperatures compared with single-phase ceramic materials made of nitrides or carbides as well as for other applications, is presented. The results of the application of azide SHS are presented in detail both in the form of the results of thermodynamic calculations and the results of experimental research of combustion parameters, combustion product structure and composition. The advantages and disadvantages of using the combustion process for the synthesis of nitride compositions with silicon carbide, the causes of the disadvantages and the directions of further research to eliminate them are discussed.
{"title":"SHS of highly dispersed powder compositions of nitrides with silicon carbide Review","authors":"A. Amosov, Y. Titova, G. S. Belova, D. Maidan, A. F. Minekhanova","doi":"10.17073/1997-308x-2022-4-34-57","DOIUrl":"https://doi.org/10.17073/1997-308x-2022-4-34-57","url":null,"abstract":"The application of the process of self-propagating high-temperature synthesis (SHS) to prepare highly dispersed powder nitride-carbide compositions from the most common refractory nitride (Si3N4, AlN, TiN) and carbide (SiC) compounds with a particle size of less than 1 μm is considered. The advantages of composite ceramics over single-phase ceramic materials and such trends of its development as the transition to nanostructured ceramics and the application of in situ processes of direct chemical synthesis of nanoparticles of components in the composite body are described. The attractiveness of the SHS process as one of the promising in situ processes characterized by simplicity and cost-effectiveness, the possibility of obtaining highly dispersed ceramic powders by burning mixtures of inexpensive reagents is shown. Considerable attention is paid to the consideration of the results of the application of azide SHS, based on the use of sodium azide and gasified halide salts as part of mixtures of initial powders of nitrided and carbidized elements during their combustion in nitrogen gas. The review of publications devoted to the application of SHS to obtain highly dispersed composite powders Si3N4–SiC, AlN–SiC and TiN–SiC, promising for use in sintering of the corresponding composite ceramic materials of submicron and nano-sized structure with improved properties, lower brittleness, good machinability, lower sintering temperatures compared with single-phase ceramic materials made of nitrides or carbides as well as for other applications, is presented. The results of the application of azide SHS are presented in detail both in the form of the results of thermodynamic calculations and the results of experimental research of combustion parameters, combustion product structure and composition. The advantages and disadvantages of using the combustion process for the synthesis of nitride compositions with silicon carbide, the causes of the disadvantages and the directions of further research to eliminate them are discussed.","PeriodicalId":14693,"journal":{"name":"Izvestiya vuzov. Poroshkovaya metallurgiya i funktsional’nye pokrytiya","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90041783","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-12-10DOI: 10.17073/1997-308x-2022-4-84-92
A. O. Kayasova, E. Levashov
Using the SLM method in a nitrogen blanket with heating to a temperature of 200 °C, samples were obtained at a position of 0° against the build plate. The effect of the hot isostatic pressing (HIP) and heat treatment (HT: hardening + aging) on the structure and mechanical properties of maraging steel CL50 WS was studied (the Russian analogue is ChS4 grade). To analyze the effect of post-processing on the strength characteristics (σb, σ0,2, δ, ψ), tensile tests were conducted. Their results indicated high values of strength and ductility. It has been established that as a result of HT in the steel structure, in addition to α-Fe, γ-Fe, dispersed precipitates of the NiTi3 strengthening phase are formed, the identification of which was carried out by high-resolution transmission electron microscopy. Through the NiTi3 intermetallic phase, the steel has acquired increased tensile strength and yield strength required for the production of critical components and parts for highly loaded turbomachine disks. The change in the porosity of the samples before and after the HIP was analyzed. The microstructure of the samples and the changes that occur under the influence of various post-processing options are studied. The fine-grained homogeneous structure obtained by combining the SLM, HIP and HT provided optimal strength and ductility. Analysis of fractures after mechanical testing showed that the samples after postprocessing are destroyed according to the viscous-pitting mechanism with the formation of a neck.
{"title":"Features of the impact of hot isostatic pressing and heat treatment on the structure and properties of maraging steel obtained by selective laser melting method","authors":"A. O. Kayasova, E. Levashov","doi":"10.17073/1997-308x-2022-4-84-92","DOIUrl":"https://doi.org/10.17073/1997-308x-2022-4-84-92","url":null,"abstract":"Using the SLM method in a nitrogen blanket with heating to a temperature of 200 °C, samples were obtained at a position of 0° against the build plate. The effect of the hot isostatic pressing (HIP) and heat treatment (HT: hardening + aging) on the structure and mechanical properties of maraging steel CL50 WS was studied (the Russian analogue is ChS4 grade). To analyze the effect of post-processing on the strength characteristics (σb, σ0,2, δ, ψ), tensile tests were conducted. Their results indicated high values of strength and ductility. It has been established that as a result of HT in the steel structure, in addition to α-Fe, γ-Fe, dispersed precipitates of the NiTi3 strengthening phase are formed, the identification of which was carried out by high-resolution transmission electron microscopy. Through the NiTi3 intermetallic phase, the steel has acquired increased tensile strength and yield strength required for the production of critical components and parts for highly loaded turbomachine disks. The change in the porosity of the samples before and after the HIP was analyzed. The microstructure of the samples and the changes that occur under the influence of various post-processing options are studied. The fine-grained homogeneous structure obtained by combining the SLM, HIP and HT provided optimal strength and ductility. Analysis of fractures after mechanical testing showed that the samples after postprocessing are destroyed according to the viscous-pitting mechanism with the formation of a neck.","PeriodicalId":14693,"journal":{"name":"Izvestiya vuzov. Poroshkovaya metallurgiya i funktsional’nye pokrytiya","volume":"89 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87471886","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-12-10DOI: 10.17073/1997-308x-2022-4-67-83
P. Sharin, A. V. Sivtseva, V. Popov
In this work, using the methods of X-ray phase analysis, transmission electron microscopy, X-ray photoelectron spectroscopy and Raman spectroscopy, the features of the impact of annealing in air within the temperature range of t = 200÷÷550 °C on the morphology, elemental and phase composition, chemical state and structure of primary particles of nanopowders obtained by grinding natural diamond and the method of detonation synthesis are studied. It is shown that heat treatment in air at given values of temperature and heating time does not affect the elemental composition and atomic structure of primary particles of nanopowders obtained both by the methods of detonation synthesis (DND) and natural diamond grinding (PND). Using XPS, Raman spectroscopy, and transmission electron microscopy, it has been found that annealing in air within the temperature range of 400–550 °C results in the effective removal of amorphous and graphite-like carbon atoms in the sp2- and sp3-states from diamond nanopowders by oxidation with atmospheric oxygen. In the original DND nanopowder, containing about 33.2 % of non-diamond carbon atoms of the total number of carbon atoms, after annealing for 5 h at a temperature of 550 °C, the relative number of nondiamond carbon atoms in the sp2-state decreased to ~21.4 %. In this case, the increase in the relative number of carbon atoms in the sp3-state (in the lattice of the diamond core) and in the composition of oxygen-containing functional groups ranged from ~39.8 % to ~46.5 % and from ~27 % to ~32.1 %, respectively. In the PND nanopowder, which prior to annealing contains about 10.6 % of non-diamond carbon atoms in the sp2-state of the total number of carbon atoms, after annealing under the same conditions as the DND nanopowder, their relative number decreased to 7.1 %. The relative number of carbon atoms in the sp3-state increased from 72.9 % to 82.1 %, and the proportion of carbon atoms in the composition of oxygen-containing functional groups also slightly increased from 10.2 % to 10.8 %. It is demonstrated that the annealing of PND and DND nanopowders in air leads to a change in their color, they become lighter as a result of oxidation of non-diamond carbon by atmospheric oxygen. The maximum effect is observed at a temperature of 550 °C and an annealing time of 5 h. In this case, the weight loss of PND and DND nanopowders after annealing was 5.37 % and 21.09 %, respectively. The significant weight loss of DND nanopowder compared to PND is primarily caused by the high content of non-diamond carbon in the initial state and the high surface energy of primary particles due to their small size.
{"title":"Air-thermal oxidation of diamond nanopowders obtained by the methods of mechanical grinding and detonation synthesis","authors":"P. Sharin, A. V. Sivtseva, V. Popov","doi":"10.17073/1997-308x-2022-4-67-83","DOIUrl":"https://doi.org/10.17073/1997-308x-2022-4-67-83","url":null,"abstract":"In this work, using the methods of X-ray phase analysis, transmission electron microscopy, X-ray photoelectron spectroscopy and Raman spectroscopy, the features of the impact of annealing in air within the temperature range of t = 200÷÷550 °C on the morphology, elemental and phase composition, chemical state and structure of primary particles of nanopowders obtained by grinding natural diamond and the method of detonation synthesis are studied. It is shown that heat treatment in air at given values of temperature and heating time does not affect the elemental composition and atomic structure of primary particles of nanopowders obtained both by the methods of detonation synthesis (DND) and natural diamond grinding (PND). Using XPS, Raman spectroscopy, and transmission electron microscopy, it has been found that annealing in air within the temperature range of 400–550 °C results in the effective removal of amorphous and graphite-like carbon atoms in the sp2- and sp3-states from diamond nanopowders by oxidation with atmospheric oxygen. In the original DND nanopowder, containing about 33.2 % of non-diamond carbon atoms of the total number of carbon atoms, after annealing for 5 h at a temperature of 550 °C, the relative number of nondiamond carbon atoms in the sp2-state decreased to ~21.4 %. In this case, the increase in the relative number of carbon atoms in the sp3-state (in the lattice of the diamond core) and in the composition of oxygen-containing functional groups ranged from ~39.8 % to ~46.5 % and from ~27 % to ~32.1 %, respectively. In the PND nanopowder, which prior to annealing contains about 10.6 % of non-diamond carbon atoms in the sp2-state of the total number of carbon atoms, after annealing under the same conditions as the DND nanopowder, their relative number decreased to 7.1 %. The relative number of carbon atoms in the sp3-state increased from 72.9 % to 82.1 %, and the proportion of carbon atoms in the composition of oxygen-containing functional groups also slightly increased from 10.2 % to 10.8 %. It is demonstrated that the annealing of PND and DND nanopowders in air leads to a change in their color, they become lighter as a result of oxidation of non-diamond carbon by atmospheric oxygen. The maximum effect is observed at a temperature of 550 °C and an annealing time of 5 h. In this case, the weight loss of PND and DND nanopowders after annealing was 5.37 % and 21.09 %, respectively. The significant weight loss of DND nanopowder compared to PND is primarily caused by the high content of non-diamond carbon in the initial state and the high surface energy of primary particles due to their small size.","PeriodicalId":14693,"journal":{"name":"Izvestiya vuzov. Poroshkovaya metallurgiya i funktsional’nye pokrytiya","volume":"34 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78760582","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-12-10DOI: 10.17073/1997-308x-2022-4-58-66
N. A. Kochetov, I. Kovalev
Combustion of powders of transition metals of titanium PTS (average particle size 57 μm), zirconium PCRK-1 (12 μm), tantalum Ta PM-3 (8 μm), hafnium GFM-1 (4 μm), niobium NBP-1a (21 μm) with carbon black grade P-803 dispersion 1–2 μm was studied. The combustion process of the compressed samples (mass 2.5–6.9 g, height 1.2–1.7 cm, relative density 0.55–0.61) was performed in an inert argon medium at a pressure of 760 mmHg in the constant pressure chamber. Combinations were studied, Me1 + Me2 + Me3 + Me4 + 4C, Me1 + Me2 + Me3 + Me4 + Me5 + 5C. XRD patterns of the mixtures were recorded on a DRON-3М diffractometer (CuKα-radiation). Combustion product sections were studied using a LEO 1450 VP scanning electron microscope (Carl Zeiss, Germany). The fractional composition and particle size distribution of the mixture were determined according to standard procedure using a Microsizer-201C laser particle size analyzer. Combustion velocity, elongation of samples, phase composition of products were determined. The maximum combustion temperature of the mixture (Ti + Hf + Zr + Nb + Ta) + 5C was measured experimentally for the first time. The morphology and microstructure of the reaction products were also observed. Combustion products of mixtures (Ti + Zr + Nb + Ta) + 4C and (Ti + Zr + Nb + Hf) + 4C contain high entropy carbides, which are solid solutions with the same structural type B1 (space group Fm-3m) and having different cell parameters. Product samples of mixtures (Ti + Zr ++ Hf + Ta) + 4C and (Ti + Hf + Zr + Nb + Ta) + 5C contain high entropy and medium entropy carbides, also representing solid solutions with the same structural type B1 (space group Fm-3m). The results of this work can be used in the production of high-entropy and medium-entropy multicomponent carbides.
{"title":"Features of SHS of multicomponent carbides","authors":"N. A. Kochetov, I. Kovalev","doi":"10.17073/1997-308x-2022-4-58-66","DOIUrl":"https://doi.org/10.17073/1997-308x-2022-4-58-66","url":null,"abstract":"Combustion of powders of transition metals of titanium PTS (average particle size 57 μm), zirconium PCRK-1 (12 μm), tantalum Ta PM-3 (8 μm), hafnium GFM-1 (4 μm), niobium NBP-1a (21 μm) with carbon black grade P-803 dispersion 1–2 μm was studied. The combustion process of the compressed samples (mass 2.5–6.9 g, height 1.2–1.7 cm, relative density 0.55–0.61) was performed in an inert argon medium at a pressure of 760 mmHg in the constant pressure chamber. Combinations were studied, Me1 + Me2 + Me3 + Me4 + 4C, Me1 + Me2 + Me3 + Me4 + Me5 + 5C. XRD patterns of the mixtures were recorded on a DRON-3М diffractometer (CuKα-radiation). Combustion product sections were studied using a LEO 1450 VP scanning electron microscope (Carl Zeiss, Germany). The fractional composition and particle size distribution of the mixture were determined according to standard procedure using a Microsizer-201C laser particle size analyzer. Combustion velocity, elongation of samples, phase composition of products were determined. The maximum combustion temperature of the mixture (Ti + Hf + Zr + Nb + Ta) + 5C was measured experimentally for the first time. The morphology and microstructure of the reaction products were also observed. Combustion products of mixtures (Ti + Zr + Nb + Ta) + 4C and (Ti + Zr + Nb + Hf) + 4C contain high entropy carbides, which are solid solutions with the same structural type B1 (space group Fm-3m) and having different cell parameters. Product samples of mixtures (Ti + Zr ++ Hf + Ta) + 4C and (Ti + Hf + Zr + Nb + Ta) + 5C contain high entropy and medium entropy carbides, also representing solid solutions with the same structural type B1 (space group Fm-3m). The results of this work can be used in the production of high-entropy and medium-entropy multicomponent carbides.","PeriodicalId":14693,"journal":{"name":"Izvestiya vuzov. Poroshkovaya metallurgiya i funktsional’nye pokrytiya","volume":"10 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89552353","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-12-08DOI: 10.17073/1997-308x-2022-4-14
V. Lebedev, V. Polyakov
The paper is devoted to a detailed study of cathodic processes, their influence on the anode process, and electrolysis performance. The polarization of a steel cathode in a CaCl2–BaCl2–NaCl melt at t = 610 °C was measured. The polarization curve clearly shows the potentials and current densities of the formation of a saturated sodium solution in the electrolyte (Esat = –2.97 V, ic = 0.04 A/cm2, lgic = –1,4), and the occurrence of sodium metal on the cathode (ENa = –3.22 V, iNa = 0.12 A/cm2, lgiNa = –0.92).The value of Esat was used to calculate the concentration of sodium in the electrolyte at t = 610 °С (1.3·10–4 mol. fr.). The values of Esat, ENa, and their difference (E = 0,25 В) were confirmed by long-term electrolysis. These fundamental characteristics are the basis for process control and management. During long-ter 3 regions close to rectilinear ones were revealed: the discharge of sodium ions from supersaturated solutions at E more negative than Esat (from ENa to Esat), from mixtures of supersaturated and saturated solutions (at a constant E equal to Esat), from diluted solutions (with E more positive than Esat). The activity coefficients of sodium in supersaturated solutions are close to 1, which ensures their increased reducing ability. Maximum degrees of supersaturation (>100) are created at formation and decomposition on the cathode of metallic sodium nuclei, which are sufficient to intensify and prolong electrolysis, to lower the lower temperature limit of its realization from 600 to 350 °С. The formation of metallic titanium in the near-anode layer is explained by the disproportionation of Ti2+ ions entering the near-anode electrolyte from the anode surface and from the near-cathode melt.
本文详细研究了阴极过程及其对阳极过程和电解性能的影响。在t = 610℃时，测量了钢阴极在CaCl2-BaCl2-NaCl熔体中的极化。极化曲线清晰地显示了电解质中形成饱和钠溶液的电位和电流密度(Esat = -2.97 V, ic = 0.04 a /cm2, llogic = - 1,4)，以及阴极上金属钠的发生(ENa = -3.22 V, iNa = 0.12 a /cm2, lgiNa = -0.92)。用Esat值计算t = 610°С(1.3·10-4 mol. fr.)时电解质中钠的浓度。Esat、ENa值及其差值(E = 0,25 В)经长期电解确认。这些基本特征是过程控制和管理的基础。在较长的时间内，发现了3个接近直线的区域:在E比Esat更负的过饱和溶液中(从ENa到Esat)，在过饱和溶液和饱和溶液的混合物中(在恒定的E等于Esat时)，在稀释溶液中(E比Esat更正)，钠离子的放电。钠在过饱和溶液中的活度系数接近于1，保证了其还原能力的增强。金属钠核在阴极形成和分解时产生最大过饱和度(>100)，这足以加强和延长电解，使其实现的下限从600°降至350°С。金属钛在近阳极层的形成可以解释为从阳极表面和近阴极熔体进入近阳极电解质的Ti2+离子的歧化。
{"title":"Electrode processes in the production of microdispersed titanium powder by volumetric electrolytic reduction of its ions with sodium dissolved in the BaCl2–CaCl2–NaCl melt in the absence of titanium halides in the initial melt","authors":"V. Lebedev, V. Polyakov","doi":"10.17073/1997-308x-2022-4-14","DOIUrl":"https://doi.org/10.17073/1997-308x-2022-4-14","url":null,"abstract":"The paper is devoted to a detailed study of cathodic processes, their influence on the anode process, and electrolysis performance. The polarization of a steel cathode in a CaCl2–BaCl2–NaCl melt at t = 610 °C was measured. The polarization curve clearly shows the potentials and current densities of the formation of a saturated sodium solution in the electrolyte (Esat = –2.97 V, ic = 0.04 A/cm2, lgic = –1,4), and the occurrence of sodium metal on the cathode (ENa = –3.22 V, iNa = 0.12 A/cm2, lgiNa = –0.92).The value of Esat was used to calculate the concentration of sodium in the electrolyte at t = 610 °С (1.3·10–4 mol. fr.). The values of Esat, ENa, and their difference (E = 0,25 В) were confirmed by long-term electrolysis. These fundamental characteristics are the basis for process control and management. During long-ter 3 regions close to rectilinear ones were revealed: the discharge of sodium ions from supersaturated solutions at E more negative than Esat (from ENa to Esat), from mixtures of supersaturated and saturated solutions (at a constant E equal to Esat), from diluted solutions (with E more positive than Esat). The activity coefficients of sodium in supersaturated solutions are close to 1, which ensures their increased reducing ability. Maximum degrees of supersaturation (>100) are created at formation and decomposition on the cathode of metallic sodium nuclei, which are sufficient to intensify and prolong electrolysis, to lower the lower temperature limit of its realization from 600 to 350 °С. The formation of metallic titanium in the near-anode layer is explained by the disproportionation of Ti2+ ions entering the near-anode electrolyte from the anode surface and from the near-cathode melt.","PeriodicalId":14693,"journal":{"name":"Izvestiya vuzov. Poroshkovaya metallurgiya i funktsional’nye pokrytiya","volume":"294 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-12-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79549111","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-12-08DOI: 10.17073/1997-308x-2022-4-25-33
A. Linde, A. A. Kondakov, I. A. Studenikin, N. A. Kondakova, V. Grachev
The synthesis of MAX phase Ti2AlN from several mixtures of Ti, Al, TiN, and AlN powders by vacuum sintering of greensamples in the form of dense compacts, bulk powder in silica tubes, and plain layer in a closed rectangular molybdenum boat was studied upon variation in charge composition and sintering temperature Ts. The sintering of 2 : 1 Ti–AlN mixture was carried out at 1100, 1200, 1300, 1400, and 1500 °С with exposure time of 60 min. The largest MAX phase content (94 wt.%) was reached at Ts = 1400 °С. The sintering of 1 : 1 TiAl : TiN composition at the same temperature gave 93 wt.% Ti2AlN. The best result (singlephase Ti2AlN in a 100-% yield) was achieved upon the sintering of 1 : 1 : 1 Ti–Al–TiN composition at Ts = 1400 °С. The scalability of our process was checked by the fabrication of a large (0.5 kg) and uniform cake of single-phase Ti2AlN. In experiments we used green samples with shielded lateral surface (bulk powder in silica tubes, plain layer in a closed molybdenum boat) and without shield (dense compacts). It has been shown that shielding of Ti–Al–TiN samples restricts the escape of Al vapor from a sintered mixture, thus providing more favorable conditions for the synthesis of single-phase Ti2AlN. Our process can be readily recommended for practical implementation.
{"title":"MAX phase Ti2AlN synthesis by reactive sintering in vacuum","authors":"A. Linde, A. A. Kondakov, I. A. Studenikin, N. A. Kondakova, V. Grachev","doi":"10.17073/1997-308x-2022-4-25-33","DOIUrl":"https://doi.org/10.17073/1997-308x-2022-4-25-33","url":null,"abstract":"The synthesis of MAX phase Ti2AlN from several mixtures of Ti, Al, TiN, and AlN powders by vacuum sintering of greensamples in the form of dense compacts, bulk powder in silica tubes, and plain layer in a closed rectangular molybdenum boat was studied upon variation in charge composition and sintering temperature Ts. The sintering of 2 : 1 Ti–AlN mixture was carried out at 1100, 1200, 1300, 1400, and 1500 °С with exposure time of 60 min. The largest MAX phase content (94 wt.%) was reached at Ts = 1400 °С. The sintering of 1 : 1 TiAl : TiN composition at the same temperature gave 93 wt.% Ti2AlN. The best result (singlephase Ti2AlN in a 100-% yield) was achieved upon the sintering of 1 : 1 : 1 Ti–Al–TiN composition at Ts = 1400 °С. The scalability of our process was checked by the fabrication of a large (0.5 kg) and uniform cake of single-phase Ti2AlN. In experiments we used green samples with shielded lateral surface (bulk powder in silica tubes, plain layer in a closed molybdenum boat) and without shield (dense compacts). It has been shown that shielding of Ti–Al–TiN samples restricts the escape of Al vapor from a sintered mixture, thus providing more favorable conditions for the synthesis of single-phase Ti2AlN. Our process can be readily recommended for practical implementation.","PeriodicalId":14693,"journal":{"name":"Izvestiya vuzov. Poroshkovaya metallurgiya i funktsional’nye pokrytiya","volume":"113 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-12-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80031979","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-12-08DOI: 10.17073/1997-308x-2022-4-15-24
N. P. Cherezov, M. Alymov
The results of the study of the structure and properties of titanium hydride powders obtained from titanium sponge by SHS hydrogenation and mechanical grinding are presented. Hydrogenation was carried out in a reactor at a constant hydrogen pressure of 3 MPa. After passing the combustion wave, the hot titanium sponge was cooled to room temperature in a hydrogenatmosphere. As a result, titanium hydride spongy granules with a hydrogen content of 4.2 wt.% were obtained. Titanium hydride was ground in a ball mill and divided into 4 fractions corresponding to the fractional composition of titanium powder PTK, PTS, PTM and PTOM. Particle size analysis showed that the samples of the PTK and PTOM powders have a narrower particle distribution in comparison with the PTS and PTM ones. Further, obtained powders chemical composition and surface morphology studies were carried out and bulk density, compaction, pycnometric density and specific surface area were determined. According to the chemical analysis results the content of carbon and oxygen impurities decreases during SHS-hydrogenation and the iron content slightly increases during mechanical grinding depending on the grinding time. The study of morphology showed that the hydride titanium particles have an irregular fragmentary shape, such morphology is characteristic of powders obtained by this technology. The surface structure has partially preserved structure of the initial titanium sponge and consists of elongated oriented grains. It is established that with a decrease in the particle size, the bulk density decreases, and the compaction increases. Pycnometric density and specific surface area values are approximately equal for all powder samples.
{"title":"Structure and properties of titanium hydride powder obtained from titanium sponge by SHS hydrogenation","authors":"N. P. Cherezov, M. Alymov","doi":"10.17073/1997-308x-2022-4-15-24","DOIUrl":"https://doi.org/10.17073/1997-308x-2022-4-15-24","url":null,"abstract":"The results of the study of the structure and properties of titanium hydride powders obtained from titanium sponge by SHS hydrogenation and mechanical grinding are presented. Hydrogenation was carried out in a reactor at a constant hydrogen pressure of 3 MPa. After passing the combustion wave, the hot titanium sponge was cooled to room temperature in a hydrogenatmosphere. As a result, titanium hydride spongy granules with a hydrogen content of 4.2 wt.% were obtained. Titanium hydride was ground in a ball mill and divided into 4 fractions corresponding to the fractional composition of titanium powder PTK, PTS, PTM and PTOM. Particle size analysis showed that the samples of the PTK and PTOM powders have a narrower particle distribution in comparison with the PTS and PTM ones. Further, obtained powders chemical composition and surface morphology studies were carried out and bulk density, compaction, pycnometric density and specific surface area were determined. According to the chemical analysis results the content of carbon and oxygen impurities decreases during SHS-hydrogenation and the iron content slightly increases during mechanical grinding depending on the grinding time. The study of morphology showed that the hydride titanium particles have an irregular fragmentary shape, such morphology is characteristic of powders obtained by this technology. The surface structure has partially preserved structure of the initial titanium sponge and consists of elongated oriented grains. It is established that with a decrease in the particle size, the bulk density decreases, and the compaction increases. Pycnometric density and specific surface area values are approximately equal for all powder samples.","PeriodicalId":14693,"journal":{"name":"Izvestiya vuzov. Poroshkovaya metallurgiya i funktsional’nye pokrytiya","volume":"161 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-12-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73801031","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-09-06DOI: 10.17073/1997-308x-2022-3-24-36
A. Amosov, E. I. Latukhin, E. Umerov, D. Davydov
The article discusses the features of combining the self-propagating high-temperature synthesis (SHS) of the Ti3AlC2 MAX phase porous skeleton with infiltration by aluminum melt in a spontaneous mode in order to obtain enlarged samples of Ti3AlC2–Al ceramic-metal composite (MAX cermet) in an air atmosphere. A new scheme was developed for obtaining long-length SHS cermet samples from a bulk density charge with spontaneous infiltration by melt in the same direction with the combustion wave movement, which makes it possible to regulate the time gap between the end of the Ti3AlC2 synthesis and the beginning of the spontaneous pore filling with aluminum melt. This technology was used to obtain a Ti3AlC2 SHS skeleton with a total length of 250 mm and a diameter of 22–24 mm where the depth of infiltration with pure aluminum was about 110 mm, and impregnation with the Al–12%Si alloy was 130 mm. The paper provides comparative data on density, microstructure, and phase composition at different areas along the length of MAX cermet samples obtained. It was found that infiltration with pure aluminum destroys the Ti3AlC2 MAX phase to transform it into a mixture of TiC + TiAl3 phases in the SHS cermet, and 12 % Si added to the Al melt promote Ti3AlC2 preservation in the cermet to a some extent. Instead of MAX cermet samples with the target composition of Ti3AlC2–Al and Ti3AlC2–(Al–12%Si), long-length samples of SHS cermets with a different actual phase composition were obtained: TiC–TiAl3–Al and TiC–Ti3AlC2–TiAl3–(Al–12%Si), respectively, where the Ti3AlC2 MAX phase either practically absent or present in small quantities. The average hardness values of TiC–TiAl3–Al and TiC–Ti3AlC2–TiAl3–(Al–12%Si) SHS cermets were HB = 640 and 740 MPa, density ρ = 2.88÷3.16 g/cm3 and 3.03÷3.13 g/cm3, and residual porosity П = 17.0÷24.6 % and 17.6÷20.3 %, respectively.
{"title":"Investigation of possibility of fabrication of long-length samples of Ti3AlC2–Al MAX-cermet by the SHS method with spontaneous infiltration by aluminum melt","authors":"A. Amosov, E. I. Latukhin, E. Umerov, D. Davydov","doi":"10.17073/1997-308x-2022-3-24-36","DOIUrl":"https://doi.org/10.17073/1997-308x-2022-3-24-36","url":null,"abstract":"The article discusses the features of combining the self-propagating high-temperature synthesis (SHS) of the Ti3AlC2 MAX phase porous skeleton with infiltration by aluminum melt in a spontaneous mode in order to obtain enlarged samples of Ti3AlC2–Al ceramic-metal composite (MAX cermet) in an air atmosphere. A new scheme was developed for obtaining long-length SHS cermet samples from a bulk density charge with spontaneous infiltration by melt in the same direction with the combustion wave movement, which makes it possible to regulate the time gap between the end of the Ti3AlC2 synthesis and the beginning of the spontaneous pore filling with aluminum melt. This technology was used to obtain a Ti3AlC2 SHS skeleton with a total length of 250 mm and a diameter of 22–24 mm where the depth of infiltration with pure aluminum was about 110 mm, and impregnation with the Al–12%Si alloy was 130 mm. The paper provides comparative data on density, microstructure, and phase composition at different areas along the length of MAX cermet samples obtained. It was found that infiltration with pure aluminum destroys the Ti3AlC2 MAX phase to transform it into a mixture of TiC + TiAl3 phases in the SHS cermet, and 12 % Si added to the Al melt promote Ti3AlC2 preservation in the cermet to a some extent. Instead of MAX cermet samples with the target composition of Ti3AlC2–Al and Ti3AlC2–(Al–12%Si), long-length samples of SHS cermets with a different actual phase composition were obtained: TiC–TiAl3–Al and TiC–Ti3AlC2–TiAl3–(Al–12%Si), respectively, where the Ti3AlC2 MAX phase either practically absent or present in small quantities. The average hardness values of TiC–TiAl3–Al and TiC–Ti3AlC2–TiAl3–(Al–12%Si) SHS cermets were HB = 640 and 740 MPa, density ρ = 2.88÷3.16 g/cm3 and 3.03÷3.13 g/cm3, and residual porosity П = 17.0÷24.6 % and 17.6÷20.3 %, respectively.","PeriodicalId":14693,"journal":{"name":"Izvestiya vuzov. Poroshkovaya metallurgiya i funktsional’nye pokrytiya","volume":"27 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-09-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77508032","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-09-06DOI: 10.17073/1997-308x-2022-3-78-87
A. Zhadyaev, D. Zakharov
Since 2017, Volgaburmash JSC (Samara, Russia) tested purchased 90%WC–10%Co carbide powder mixtures and finished carbide drill bits from various manufacturers. The work was carried out in order to check the possibility of using purchased products as raw materials at the plant to reduce the production cycle for the manufacture of carbide inserts for roller cone bits. This intercommodity substitution (outsourcing) is carried out with the aim of potential cone bit cost reduction and production process acceleration so that the plant can operate in the heavily competitive environment of foreign and domestic markets. The article focuses on the analysis and detailed comparison of the micro- and macrostructure, physical, mechanical, chemical and processing properties of purchased hard-alloy mixtures and sintered inserts of various manufacturers including Volgaburmash JSC. All properties of materials under study were determined in accordance with the VBM JSC company standard STP 582-17. Much attention is paid to comparing crack resistance or Palmqvist fracture toughness values of the alloy and analysis of microstructure images and fracture propagation pattern after using scanning electron microscopy tests. In addition, consideration is given to such important hard alloy properties as hardness and transverse bending strength. Based on the results of the conducted research, conclusions are presented on the expediency of using purchased hard-alloy materials at the Volgaburmash JSC metallurgical shop in comparison with internally manufactured materials.
{"title":"About the experience of using hardmetals in the production of roller cone bits at Volgaburmash JSC","authors":"A. Zhadyaev, D. Zakharov","doi":"10.17073/1997-308x-2022-3-78-87","DOIUrl":"https://doi.org/10.17073/1997-308x-2022-3-78-87","url":null,"abstract":"Since 2017, Volgaburmash JSC (Samara, Russia) tested purchased 90%WC–10%Co carbide powder mixtures and finished carbide drill bits from various manufacturers. The work was carried out in order to check the possibility of using purchased products as raw materials at the plant to reduce the production cycle for the manufacture of carbide inserts for roller cone bits. This intercommodity substitution (outsourcing) is carried out with the aim of potential cone bit cost reduction and production process acceleration so that the plant can operate in the heavily competitive environment of foreign and domestic markets. The article focuses on the analysis and detailed comparison of the micro- and macrostructure, physical, mechanical, chemical and processing properties of purchased hard-alloy mixtures and sintered inserts of various manufacturers including Volgaburmash JSC. All properties of materials under study were determined in accordance with the VBM JSC company standard STP 582-17. Much attention is paid to comparing crack resistance or Palmqvist fracture toughness values of the alloy and analysis of microstructure images and fracture propagation pattern after using scanning electron microscopy tests. In addition, consideration is given to such important hard alloy properties as hardness and transverse bending strength. Based on the results of the conducted research, conclusions are presented on the expediency of using purchased hard-alloy materials at the Volgaburmash JSC metallurgical shop in comparison with internally manufactured materials.","PeriodicalId":14693,"journal":{"name":"Izvestiya vuzov. Poroshkovaya metallurgiya i funktsional’nye pokrytiya","volume":"91 10 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-09-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87731638","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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