Abstract—
We examine general aspects of the formation of Ti3SiC2–TiB2–SiC ceramic composites during vacuum carbosilicothermic reduction of titanium oxide mineral raw materials (leucoxene concentrate from the Yaregskoe occurrence) in the presence of B4C as a boron-containing additive, with SiC as a reducing agent. The effect of starting-mixture composition on the phase composition of the reduction product and the formation of minor phases is analyzed. We demonstrate that, with increasing B4C concentration in the starting mixture, the fraction of the forming TiB2 rises systematically, reaching 48 vol %.
Similar content being viewed by others
REFERENCES
Barsoum, M.W., MAX Phases: Properties of Machinable Carbides and Nitrides, Weinheim: Wiley–VCH, 2013.https://doi.org/10.1002/9783527654581
Sun, Z.M., Progress in research and development on MAX phases: a family of layered ternary compounds, Int. Mater. Rev., 2011, vol. 56, no. 3, pp. 143–166.https://doi.org/10.1179/1743280410Y.0000000001
Barsoum, M.W. and Radovic, M., Elastic and mechanical properties of the MAX phases, Annu. Rev. Mater. Res., 2011, vol. 41, pp. 195–227.https://doi.org/10.1146/annurev-matsci-062910-100448
Barsoum, M.W. and Radovic, M., MAX phases: bridging the gap between metals and ceramics, Am. Ceram. Soc. Bull., 2013, vol. 92, no. 3, pp. 20–27.
Yang, S., Sun, Z.M., Hashimoto, H., and Abe, T., Ti3SiC2 powder synthesis from Ti/Si/TiC powder mixtures, J. Alloys Compd., 2003, vol. 358, nos. 1–2, pp. 168–172.https://doi.org/10.1016/S0925-8388(03)00039-2
Kero, I., Tegman, R., and Antti, M.-L., Phase reactions associated with the formation of Ti3SiC2 from TiC/Si powders, Ceram. Int., 2011, vol. 37, pp. 2615–2619.https://doi.org/10.1016/j.ceramint.2011.04.132
Li, H., Chen, D., Zhou, J., Zhao, J.H., and He, L.H., Synthesis of Ti3SiC2 by pressureless sintering of the elemental powders in vacuum, Mater. Lett., 2004, vol. 58, no. 11, pp. 1741–1744.https://doi.org/10.1016/j.matlet.2003.10.057
Istomin, P.V., Nadutkin, A.V., Ryabkov, Yu.I., and Goldin, B.A., Preparation of Ti3SiC2, Inorg. Mater., 2006, vol. 42, no. 3, pp. 250–255.https://doi.org/10.1134/S0020168506030071
Hwang, S.S., Lee, S.C., Han, J.H., Lee, D., and Park, S.-W., Machinability of Ti3SiC2 with layered structure synthesized by hot pressing mixture of TiCx and Si powder, J. Eur. Ceram. Soc., 2012, vol. 32, pp. 3493–3500.https://doi.org/10.1016/j.jeurceramsoc.2012.04.021
Wang, J., Li, A.-J., Wang, S.-M., and Zeng, H.-X., Dependence of the microstructure and properties of TiC/Ti3SiC2 composites on extra C addition, Ceram. Int., 2012, vol. 38, pp. 5967–5971.https://doi.org/10.1016/j.ceramint.2012.04.049
Gao, N.F., Li, J.T., Zhang, D., and Miyamoto, Y., Rapid synthesis of dense Ti3SiC2 by spark plasma sintering, J. Eur. Ceram. Soc., 2002, vol. 22, pp. 2365–2370.https://doi.org/10.1016/S0955-2219(02)00021-3
Zhang, J., Wu, T., Wang, L., Jiang, W., and Chen, L., Microstructure and properties of Ti3SiC2/SiC nanocomposites fabricated by spark plasma sintering, Compos. Sci. Technol., 2008, vol. 68, pp. 499–505.https://doi.org/10.1016/j.compscitech.2007.06.006
Abderrazak, H., Turki, F., Schoenstein, F., Abdellaoui, M., and Jouini, N., Effect of the mechanical alloying on the Ti3SiC2 formation by spark plasma sintering from Ti/Si/C powders, Int. J. Refract. Met. Hard Mater., 2012, vol. 35, pp. 163–169.https://doi.org/10.1016/j.ijrmhm.2012.05.011
El Saeed, M.A., Deorsola, F.A., and Rashad, R.M., Optimization of the Ti3SiC2 MAX phase synthesis, Int. J. Refract. Met. Hard Mater., 2012, vol. 35, pp. 127–131.https://doi.org/10.1016/j.ijrmhm.2012.05.001
Istomin, P., Nadutkin, A., and Grass, V., Fabrication of Ti3SiC2-based ceramic matrix composites by a powder-free SHS technique, Ceram. Int., 2013, vol. 39, pp. 3663–3667.https://doi.org/10.1016/j.ceramint.2012.10.196
Bazhin, P.M., Stel’makh, L.S., and Stolin, A.M., Effect of strain on the formation of a MAX phase in Ti–Al–C materials during self-propagating high temperature synthesis and extrusion, Inorg. Mater., 2019, vol. 55, no. 3, pp. 330–335.https://doi.org/10.1134/S0020168519030051
Wang, Q., Hu, C., Huang, Q., Cai, S., Sakka, Y., and Grasso, S., Synthesis of high-purity Ti3SiC2 by microwave sintering, Int. J. Appl. Ceram. Technol., 2014, vol. 11, pp. 911–918.https://doi.org/10.1111/ijac.12065
Foratirad, H., Baharvandi, H., and Maraghe, M.G., Effect of excess silicon content on the formation of nano-layered Ti3SiC2 ceramic via infiltration of TiC preforms, J. Eur. Ceram. Soc., 2017, vol. 37, no. 2, pp. 451–457.https://doi.org/10.1016/j.jeurceramsoc.2016.09.004
Li, S.B., Zhai, H.-X., Zhou, Y., and Zhang, Z.L., Synthesis of Ti3SiC2 powders by mechanically activated sintering of elemental powders of Ti, Si and C, Mater. Sci. Eng., A, 2005, vol. 407, pp. 315–321.https://doi.org/10.1016/j.msea.2005.07.043
Liang, B.Y., Wang, M.Z., Sun, J.F., Li, X.P., Zhao, Y.C., and Han, X., Synthesis of Ti3SiC2 in air using mechanically activated 3Ti/Si/2C powder, J. Alloys Compd., 2009, vol. 474, pp. 18–21.https://doi.org/10.1016/j.jallcom.2008.06.147
Fakih, H., Jacques, S., Berthet, M.-P., Bosselet, F., Dezellus, O., and Viala, J.-C., The growth of Ti3SiC2 coatings onto SiC by reactive chemical vapor deposition using H2 and TiCl4, Surf. Coat. Technol., 2006, vol. 201, no. 6, pp. 3748–3755.https://doi.org/10.1016/j.surfcoat.2006.09.040
Furgeaud, C., Brenet, F., and Nicolai, J., Multi-scale study of Ti3SiC2 thin film growth mechanisms obtained by magnetron sputtering, Materialia, 2019, vol. 7, paper 100369.https://doi.org/10.1016/j.mtla.2019.100369
Hendaoui, A., Vrel, D., Amara, A., Benaldjia, A., and Langlois, P., Ti–Al–C MAX phases by aluminothermic reduction process, Int. J. Self-Propag. High-Temp Synth., 2008, vol. 17, no. 2, pp. 125–128.https://doi.org/10.3103/S1061386208020076
Cetinkaya, S. and Eroglu, S., Synthesis and reaction mechanism of Ti3SiC2 ternary compound by carbothermal reduction of TiO2 and SiO2 powder mixtures, Ceram. Int., 2012, vol. 38, pp. 6445–6453.https://doi.org/10.1016/j.ceramint.2012.05.020
Istomin, P., Nadutkin, A., and Grass, V., Fabrication of Ti3SiC2-based composites from titania–silica raw material, Mater. Chem. Phys., 2015, vol. 162, pp. 216–221.https://doi.org/10.1016/j.matchemphys.2015.05.060
Goldin, B.A., Istomin, P.V., and Ryabkov, Yu.I., Reduction solid-state synthesis of titanium silicide carbide, Ti3SiC2, Inorg. Mater., 1997, vol. 33, no. 6, pp. 577–579.
Istomin, P., Istomina, E., Nadutkin, A., Grass, V., and Presniakov, M., Synthesis of a bulk Ti4SiC3 MAX phase by reduction of TiO2 with SiC, Inorg. Chem., 2016, vol. 55, no. 21, pp. 11050–11056.https://doi.org/10.1021/acs.inorgchem.6b01601
Istomina, E.I., Istomin, P.V., and Nadutkin, A.V., Preparation of Ti3SiC2 through reduction of titanium dioxide with silicon carbide, Inorg. Mater., 2016, vol. 52, no. 2, pp. 134–140.https://doi.org/10.7868/S0002337X16020056
Istomina, E.I., Istomin, P.V., Nadutkin, A.V., Grass, V.E., and Bogdanova, A.S., Optimization of the carbosilicothermic synthesis of the Ti4SiC3 MAX phase, Inorg. Mater., 2018, vol. 54, no. 6, pp. 528–536.https://doi.org/10.1134/S0020168518060055
Istomin, P., Istomina, E., Nadutkin, A., Grass, V., Leonov, A., Kaplan, M., and Presniakov, M., Fabrication of Ti3SiC2 and Ti4SiC3 MAX phase ceramics through reduction of TiO2 with SiC, Ceram. Int., 2017, vol. 43, no. 18, pp. 16128–16135.https://doi.org/10.1016/j.ceramint.2017.08.180
Istomin, P., Istomina, E., Nadutkin, A., Grass, V., and Kaplan, M., Fabrication of Ti3SiC2–Ti4SiC3–SiC ceramic composites through carbosilicothermic reduction of TiO2, Int. J. Appl. Ceram. Technol., 2019, vol. 16, pp. 746–752.https://doi.org/10.1111/ijac.13101
Zou, W., Li, F., Zhang, H., Yang, J., Peng, S., and Qiu, T., Microstructure and mechanical properties of in-situ hot pressed (TiB2 + SiC)/ Ti3SiC2 composites with tunable TiB2 content, Adv. Appl. Ceram., 2016, vol. 115, no. 5, pp. 282–287.https://doi.org/10.1080/17436753.2016.1138580
Song, K., Yang, J., Qiu, T., and Pan, L.M., In situ synthesis of (TiB2 + SiC)/Ti3SiC2 composites by hot pressing, Mater. Lett., 2012, vol. 75, pp. 16–19.https://doi.org/10.1016/j.matlet.2012.01.061
Kraus, W. and Nolze, G., Powder cell – a program for the representation and manipulation of crystal structures and calculation of the X-ray powder patterns, J. Appl. Crystallogr., 1996, vol. 29, pp. 301–303.https://doi.org/10.1107/S0021889895014920
Razavi, M., Rahimipour, M.R., and Kaboli, R., Synthesis of TiC nanocomposite powder from impure TiO2 and carbon black by mechanically activated sintering, J. Alloys Compd., 2008, vol. 460 P, pp. 694–698.https://doi.org/10.1016/j.jallcom.2007.06.080
Hajalilou, A., Hashim, M., Ebrahimi-Kahizsangi, R., Ismail, I., and Sarami, N., Synthesis of titanium carbide and TiC–SiO2 nanocomposite powder using rutile and Si by mechanically activated sintering, Adv. Powder Technol., 2014, vol. 25, pp. 1094–1102.https://doi.org/10.1016/j.apt.2014.02.008
Khalafalla, S.E. and Haas, L.A., Kinetics of carbothermal reduction of quartz under vacuum, J. Am. Ceram. Soc., 1972, vol. 55, no. 8, pp. 414–417.https://doi.org/10.1111/j.1151-2916.1972.tb11324.x
Youm, M.R., Yun, S., Choi, S.C., and Park, S.W., Synthesis of β-SiC powders by the carbothermal reduction of porous SiO2–C hybrid precursors with controlled surface area, Ceram. Int., 2020, vol. 46, pp. 4870–4877.https://doi.org/10.1016/j.ceramint.2019.10.223
ACKNOWLEDGMENTS
In this study, we used equipment at the Khimiya Shared Research Facilities Center, Institute of Chemistry, Komi Scientific Center (Federal Research Center), Ural Branch, Russian Academy of Sciences.
Funding
This work was supported by the Russian Foundation for Basic Research and the Komi Republic Ministry of Education, Science, and Youth Policy (research project no. 20-48-110001).
Author information
Authors and Affiliations
Corresponding author
Additional information
Translated by O. Tsarev
Rights and permissions
About this article
Cite this article
Istomin, P.V., Belyaev, I.M., Istomina, E.I. et al. Carbosilicothermic Synthesis of Ti3SiC2–TiB2–SiC Ceramic Composites from Leucoxene Concentrate. Inorg Mater 57, 308–315 (2021). https://doi.org/10.1134/S0020168521030067
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S0020168521030067