Skip to main content
SpringerLink
Log in

Preparation of CaB6 powder via calciothermic reduction of boron carbide

  • Published:
International Journal of Minerals, Metallurgy and Materials Aims and scope Submit manuscript

Abstract

The method of calciothermic reduction of B4C was proposed for preparing CaB6. The phase transition and morphology evolution during the reaction were investigated in detail. The experimental results reveal that Ca first reacts with B4C to generate CaB2C2 and CaB6 at a low temperature and that the CaB2C2 subsequently reacts with Ca to produce CaB6 and CaC2 at a high temperature. After the products were leached to remove the byproduct CaC2, pure CaB6 was obtained. The grain size of the prepared CaB6 was 2–3 μm, whereas its particle size was 4–13 μm; it inherited the particle size of B4C. The residual C content of the product was decreased to 1.03wt% after the first reaction at 1173 K for 4 h and the second reaction at 1623 K for 4 h.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Similar content being viewed by others

References

  1. Nisso Tsushinsha, ed, Handbook on High-melting-point Composites, Nisso Tsushinsha, Ehime, 1977.

    Google Scholar 

  2. R.A. Cutler, Engineered Materials Handbook, Vol. 4, S.J. Schneider Jr. ed., ASM International, The Materials Information Society, Metals Park, Ohio, 1991, p. 787.

    Google Scholar 

  3. P.A. Dearnley and T. Bell, Engineering the surface with boron based materials, Surf. Eng, 1(1985), No. 3, p. 203.

    Article  CAS  Google Scholar 

  4. H.J. Tromp, P. Van Gelderen, P.J. Kelly, G. Brocks, and P.A. Bobbert, CaB6: a new semiconducting material for spin electronics, Phys. Rev. Lett., 87(2001), art. No. 016401.

  5. D.P. Young, D. Hall, M.E. Torelli, Z. Fisk, J.L. Sarrao, J.D. Thompson, H.R. Ott, S.B. Oseroff, R.G. Goodrich, and R. Zysler, High-temperature weak ferromagnetism in a low-density free-electron gas, Nature, 397(1999), p. 412.

    Article  CAS  Google Scholar 

  6. L.H. Bao, X.P. Qi, L.M. Chao, and O. Tegus, Synthesis, and magnetic and optical properties of nanocrystalline alkaline-earth hexaborides, CrystEngComm, 18(2016), p. 1223.

    Article  CAS  Google Scholar 

  7. H. Razavi-Zadeh and S. Mirdamadi.T, Deoxidizing copper with CaB6, JOM, 39(1987), No. 2, p. 42.

    Article  CAS  Google Scholar 

  8. K.G. Schmitt-Thomas, A. Lipp, and K. Schwetz, Process for the Production of Oxygen-Free Copper Casting and Moldings, United States Patent, Appl. 738819, 1976.

    Google Scholar 

  9. T. Rymon-Lipinski, B. Schmelzer, and S. Ulitzka, Tests on the oxidation-inhibiting effect of CaB6 in refractory MgO-C materials, Steel Res., 65(1994), No. 6, p. 234.

    Article  CAS  Google Scholar 

  10. J.W. Butler, Neutron-absorbing bricks made from CaB6, Nucl. Instrum. Methods, 7(1960), No. 2, p. 201.

    Article  CAS  Google Scholar 

  11. M.T. Zheng, H.W. Dong, Y. Xiao, S.T. Liu, H. Hu, Y.R. Liang, L.Y. Sun, and Y.L. Liu, Facile one-step and high-yield synthesis of few-layered and hierarchically porous boron nitride nanosheets, RSC Adv., 6(2016), No. 51, p. 45402.

    Article  CAS  Google Scholar 

  12. B.A. Galanov, V.V. Kartuzov, O.N. Grigoriev, L.M. Melakh, S.M. Ivanov, E.V. Kartuzov, and P. Swoboda, Penetration resistance of B4C-CaB6 based light-weight armor materials, Procedia Eng., 58(2013), p. 328.

    Article  CAS  Google Scholar 

  13. P. Seenuvasaperumal, A. Elayaperumal, and R. Jayavel, Influence of calcium hexaboride reinforced magnesium composite for the mechanical and tribological behviour, Tribol. Int., 111(2017), p. 18.

    Article  CAS  Google Scholar 

  14. Y. Gao, Z.D. Liu, Q. Wang, and Y.T. Wang, Mcrostructure and mechanical properties of Nb-Mo-ZrB2 composites prepared by hot-pressing sintering, Int. J. Miner. Metall. Mater, 25(2018), No. 7, p. 824.

    Article  CAS  Google Scholar 

  15. Y.R. Zhang, Q. Cai, Y.C. Liu, Z.Q. Ma, C. Li, and H.J. Li, Evaluation of precipitation hardening in TiC-reinforced Ti2AlNb-based alloys, Int. J. Miner. Metall. Mater, 25 (2018), No. 4, p. 453.

    Article  CAS  Google Scholar 

  16. L. Zhang, G.H. Mn, and H.S. Yu, Reaction mechanism and size control of CaB6 micron powder synthesized by the boroncarbide method, Ceram. Int., 35(2009), No. 8, p. 3533.

    Article  CAS  Google Scholar 

  17. M. Kakiage, S. Shiomi, I. Yanase, and H. Kobayashi, Low-temperature synthesis of calcium hexaboride powder via transient boron carbide formation, J. Am. Ceram. Soc, 98 (2015), No. 9, p. 2724.

    Article  CAS  Google Scholar 

  18. D. Yilmaz, U. Savaci, N. Koç, and S. Turanb, Carbothermic reduction synthesis of calcium hexaboride using PVA-calcium hexaborate mixed gels, Ceram. Int., 44(2018), No. 3, p. 2976.

    Article  CAS  Google Scholar 

  19. M. Kakiage, S. Shiomi, T. Ohashi, and H. Kobayashi, Effect of calcium carbonate particle size on formation and morphology of calcium hexaboride powder synthesized from condensed boric acid-poly (vinyl alcohol) product, Adv. Powder Technol, 29(2018), No. 1, p. 36.

    Article  CAS  Google Scholar 

  20. K. Bao, L.X. Lin, H. Chang, and S.W. Zhang, Low-temperature synthesis of calcium hexaboride nanoparticles via magnesiothermic reduction in molten salt, J. Ceram. Soc. Jpn., 125(2017), No. 12, p. 866.

    Article  CAS  Google Scholar 

  21. Ö. Balcı, D. Ağaoğulları, İ. Duman, and M.L. Öveçoğlu, Synthesis of CaB6 powders via mechanochemical reaction of Ca/B2O3 blends, Powder Technol, 225(2012), p. 136.

    Article  Google Scholar 

  22. X. Huang, J.C. Zhong, L.S. Dou, and K. Wang, Combustion synthesis of CaB6 powder from calcium hexaborate and Mg, Int. J. Refract. Met. Hard Mater, 28(2010), No. 2, p. 143.

    Article  CAS  Google Scholar 

  23. X. Wang and Y.C. Zhai, An electrochemical method for the preparation of CaB6 crystal powder, J. Appl. Electrochem., 39(2009), p. 1797.

    Article  CAS  Google Scholar 

  24. W. Weng, M.Y. Wang, X.Z. Gong, Z. Wang, D. Wang, and Z.C. Guo, Electrochemical conversions of soluble borates to CaB6 with superior optical property in NaCl-CaCl2 melt, J. Electrochem. Soc, 165(2018), No. 10, p. E477.

    Article  CAS  Google Scholar 

  25. S. Angappan, M. Helan, A. Visuvasam, L.J. Berchmans, and V. Ananth, Electrolytic preparation of CaB6 by molten salt technique, Ionics, 17(2011), No. 6, p. 527.

    Article  CAS  Google Scholar 

  26. S.Q. Zheng, G.H. Min, Z.D. Zou, H.S. Yu, and J.D. Han, Synthesis of calcium hexaboride powder via the reaction of calcium carbonate with boron carbide and carbon, J. Am. Ceram. Soc, 84(2001), No. 11, p. 2725.

    Article  CAS  Google Scholar 

  27. B. Albert and K. Schmitt, CaB2C2: Reinvestigation of a semiconducting boride carbide with a layered structure and an interesting boron/carbon ordering scheme, Inorg. Chem., 38(1999), No. 26, p. 6159.

    Article  CAS  Google Scholar 

  28. J. Akimitsu, K. Takenawa, K. Suzuki, H. Harima, and Y. Kuramoto, High-temperature ferromagnetism in CaB2C2, Science, 293(2001), No. 5532, p. 1125.

    Article  CAS  Google Scholar 

  29. A.V. Blinder, S.P. Gordienko, É.V. Marek, and V.B. Muratov, Thermodynamic properties of calcium hexaboride, Powder Metall. Met. Ceram., 36(1997), No. 7–8, p. 409.

    Article  CAS  Google Scholar 

  30. W. Ostwald, Über die vermeintliche Isomerie des roten und gelben Quecksilberoxyds und die Oberflächenspannung fester Körper, Z. Phys. Chem., 34(1900), p. 495.

    Google Scholar 

  31. L. Zhang, G.H. Min, H.S. Yu, H.M. Chen, and G. Feng, The size and morphology of fine CaB6 powder synthesized by nanometer CaCO3 as reactant, Key Eng. Mater, 326–328(2006), p. 369.

    Article  Google Scholar 

  32. S.S.N. Murthy, M. Patel, J.J. Reddy, and V.V. Bhanu Prasad, Influence of B4C particle size on the synthesis of ZrB2 by boro/carbothermal reduction method, Trans. Indian Inst. Met, 71(2018), No. 1, p. 57.

    Article  CAS  Google Scholar 

Download references

Acknowledgement

This work was financially supported by the Fundamental Research Funds for the Central Universities of China (No. FRF-GF-17-B41).

Author information

Authors and Affiliations

  1. State Key Laboratory of Advanced Metallurgy, University of Science and Technology Beijing, Beijing, 100083, China

    Yu Wang, Guo-hua Zhang & Yue-dong Wu

  2. Institute for Advanced Materials and Technology, University of Science and Technology Beijing, Beijing, 100083, China

    Xin-bo He

Authors
  1. Yu Wang
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Guo-hua Zhang
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Yue-dong Wu
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Xin-bo He
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Guo-hua Zhang.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Wang, Y., Zhang, Gh., Wu, Yd. et al. Preparation of CaB6 powder via calciothermic reduction of boron carbide. Int J Miner Metall Mater 27, 37–45 (2020). https://doi.org/10.1007/s12613-019-1873-y

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12613-019-1873-y

Keywords

Search

Navigation