Low-temperature Rapid Synthesis of Ultrafine Hafnium Carbide Ceramic Powders

Abstract

Nano hafnium carbide (HfC) powders were synthesized by sol-gel combining high-temperature rapid heat treatment process using citric acid and hafnium tetrachloride as the raw materials. The effects of ball milling treatment on the phase and morphology of pyrolysis products (HfO₂-C) and final HfC product were investigated and the influences of heat treatment temperature and holding time on the structure and properties of the synthesized hafnium carbide powders were also studied. The experimental results showed that the HfO₂-C powders with good uniformity and small particle size were prepared by controlling the milling time. Pure HfC powders with an average particle size of 500 nm were obtained at 1 700 °C with a holding time of 3 min, and the oxygen content was about 0.69wt%, lower than that of the hafnium carbide powders prepared by SPS (0.97%).

Keywords

hafnium carbides / sol-gel / ball milling / high temperature heat treatment

References

[1] Wang YB, Su XJ, Hou GL, et al. Synthesis and Characterrization of Hafnium Carbide using the Method of Liquid Precursor Conversion[J]. Rare Met. Mater. Eng., 2008, 37(4): 729-732.

[2] Zhang SH, Cheng XH, Liu FT. Elastic and Thermodynamic Properties of Hafnium Carbide[J]. Journal of HeBei Normal University. Nat. Sci. Ed., 2013, 37(1): 41-45.

[3] Opeka M, Talmy IG, Wuchina EJ, et al. Mechanical, Thermal and Oxidation Properties of Refractory Hafnium and Zirconium[J]. J. Europ. Ceram. Soc., 1999, 19: 2405-2414.

[4] Wuchina EJ, Opeka M, Causey S, et al. Arc-jet Testing on HfB2 and HfC-based Ultra-high Temperature Ceramic Materials[J]. J. Mater. Sci., 2004, 39: 5939-5949.

[5] Sacks M W C Y Z, et al. Carbothermal Reduction Synthesis of Nanocrystalline Zirconium Carbide and Hafnium Carbide Powders using Solution-derived Precursors[J]. J. Mater. Sci., 2004, 39: 6057-6066.

[6] Shimada S, Nakajima K, Inagaki M. Oxidation of Single Crystals of Hafnium Carbide in a Temperature Range of 600–900 ?[J]. J. Am. Ceram. Soc., 1997, 80: 1749-1756.

[7] Bergeron CB, Benson RC, Jette AN, et al. Oxidation of Hafnium Carbide in the Temperature Range 1400–2060 ?[J]. J. Am. Ceram. Soc., 1993, 76: 1040-1046.

[8] Yang Y, Liu L, Wei L, et al. In situ Fabrication of HfC-decorated Carbon Nanotube Yarns and Their Field-emission Properties[J]. Carbon., 2010, 48: 531-537.

[9] Yao MQ, Wei YH, Hu LQ, et al. Fabrication of Nanometer Powders by the Sol-Gel Method[J]. Rare Met. Mater. Eng., 2002, 31(5): 325-329.

[10] Song JF. Progress in Research on Sol-Gel Technology[J]. Inorg. Chem. Ind., 2005, 37(11): 14-17.

[11] Wang YH, Zhuang ZQ. Research and Application of Sol-Gel Technique[J]. Ceram. Res. Vocat. Edu., 2003, 1(1): 46-47.

[12] Branko M, Biljana B, Dusan B, et al. Synthesis and Characterization of Hafnium Carbide Fine Powders[J]. Ceram. Int., 2013, 39(1): 719-723.

[13] Munir ZA, Quach DV, Ohyanagi M. Electric Field and Current Effects on Sintering[J]. Sint. Eng. Mater., 2011, 35(94): 137-158.

[14] Xie J, Fu Z, Wang Y, et al. Synthesis of Nanosized Zirconium Carbide Powders by a Combinational Method of Sol–gel and Pulse Current Heating[J]. J. Eur. Ceram. Soc., 2014, 34(1): 13.e1-13.e7.

[15] Lun F, Lee SH, Wang H, et al. Synthesis and Densification of Nano-crystalline Hafnium Carbide Powder[J]. J. Eur. Ceram. Soc., 2015, 35(15): 4073-4081.

[16] Jia Quanli. A Method of Low Temperature Synthesis of Hafnium Caebide Ceramic Powder by Molten Salt Assited Magnesiothermic Reduction[P]. China: 201610114044.6, 2016. 07. 20

[17] Lu D, Wang W, Wang H, et al. Synthesis of Ultra-fine Hafnium Carbide Powders Combining the Methods of Liquid Precursor Conversion and Plasma Activated Sintering[J]. Ceram. Int., 2016, 42(7): 8108-8114.