微波熔盐辅助硼热/碳热还原法制备ZrB2-SiC复合粉
Synthesis of ZrB2-SiC Composite Powder by Microwave and Molten-Salt Co-assisted Boro/Carbothermal Reduction Method
摘 要
以ZrO2、SiO2、B4C及活性炭为反应物，以NaCl/KCl为熔盐，采用微波熔盐辅助硼热/碳热还原法制备ZrB2-SiC复合粉，研究了反应温度、反应时间、B4C及熔盐介质用量等对产物物相组成和显微结构的影响。结果表明：随着反应温度的升高，反应时间的延长，B4C和熔盐用量的增加，ZrB2和SiC的合成反应进行得越充分，产物中ZrB2的衍射峰越强；在反应温度为1 200℃，反应时间为20 min，熔盐与反应物质量比为2：1，B4C与ZrO2物质的量的比为0.8的条件下，可以制备得到纯相ZrB2-SiC复合粉，其平均粒径约为38 μm，其中ZrB2为一维棒状结构，直径约为1.35 μm，平均长径比大于10。
微波加热
熔盐
硼热/碳热还原法
ZrB2-SiC composite powder
microwave heating
molten-salt
boro/carbothermal reduction method
Abstract
ZrB2-SiC composite powder was prepared by microwave and molten-salt co-assisted boro/carbothermal reduction method with ZrO2, SiO2, B4C and activated carbon as reactants, and with NaCl and KCl as molten-salt. The effects of reaction temperature, reaction time, B4C and molten-salt content on the phase composition and microstructure of the product were investigated. The results show that with the increase of reaction temperature, reaction time, B4C content and molten-salt content, the synthetic reaction of ZrB2 and SiC occurred more completely, and the diffraction peaks of ZrB2 in the product were getting stronger. When the reaction temperature was 1 200℃, reaction time was 20 min, salt to reactant mass ratio was 2:1 and the molar ratio of B4C to ZrO2 was 0.8, the pure-phased ZrB2-SiC composite powder with average grain size of 38 μm was obtained, where ZrB2 had a one-dimensional rod-like structure with a diameter of about 1.35 μm and an average length to diameter ratio over 10.
中图分类号 TQ174.4 DOI 10.11973/jxgccl201804007
所属栏目 新材料 新工艺
基金项目 国家自然科学基金面上项目（51672194）；湖北省教育厅高等学校优秀中青年科技创新团队计划项目（T201602）；湖北省自然科学基金创新群体项目（2017CFA004）
收稿日期 2017/8/3
修改稿日期 2018/3/12
网络出版日期
作者单位点击查看
备注曾渊(1994-),男,湖北麻城人,硕士研究生
引用该论文: ZENG Yuan,LIANG Feng,LIU Jianghao,TAN Cao,HAN Lei,ZHANG Haijun. Synthesis of ZrB2-SiC Composite Powder by Microwave and Molten-Salt Co-assisted Boro/Carbothermal Reduction Method[J]. Materials for mechancial engineering, 2018, 42(4): 31～34
曾渊,梁峰,刘江昊,谭操,韩磊,张海军. 微波熔盐辅助硼热/碳热还原法制备ZrB2-SiC复合粉[J]. 机械工程材料, 2018, 42(4): 31～34
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参考文献
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【2】FAHRENHOLTZ W G, HILMAS G E, TALMY I G, et al. Refractory diborides of zirconium and hafnium[J]. Journal of the American Ceramic Society, 2007, 90(5):1347-1364.
【3】PENG F, SPEYER R F. Oxidation resistance of fully dense ZrB2 with SiC, TaB2, and TaSi2 additives[J]. Journal of the American Ceramic Society, 2008, 91(5):1489-1494.
【4】MALLIK M, KAILATH A J, RAY K K, et al. Electrical and thermophysical properties of ZrB2 and HfB2 based composites[J]. Journal of the European Ceramic Society, 2012, 32(10):2545-2555.
【5】方舟, 王皓, 傅正义. Zr-B2O3-Mg体系自蔓延高温合成ZrB2陶瓷粉末[J]. 硅酸盐学报, 2004, 32(6):755-758.
【6】CAO Y, ZHANG H, LI F, et al. Preparation and characterization of ultrafine ZrB2-SiC composite powders by a combined sol-gel and microwave boro/carbothermal reduction method[J]. Ceramics International, 2015, 41(6):7823-7829.
【7】GUO W M,ZHANG G J. Reaction processes and characterization of ZrB2 powder prepared by boro/carbothermal reduction of ZrO2 in vacuum[J]. Journal of the American Ceramic Society, 2009, 92(1):264-267.
【8】JUNG E Y, KIM J H, JUNG S H, et al. Synthesis of ZrB2 powders by carbothermal and borothermal reduction[J]. Journal of Alloys and Compounds, 2012, 538:164-168.
【9】SHUGART K, LIU S, CRAVEN F, et al. Determination of retained B2O3 content in ZrB2-30 vol% SiC oxide scales[J]. Journal of the American Ceramic Society,2015,98(1):287-295.
【10】ZHANG S, KHANGKHAMANO M, ZHANG H, et al. Novel synthesis of ZrB2 powder via molten-salt-mediated magnesiothermic reduction[J]. Journal of the American Ceramic Society, 2014, 97(6):1686-1688.
【11】JALALY M, BAFGHI M S, TAMIZIFAR M, et al. Mechanosynthesis of nanocrystalline ZrB2-based powders by mechanically induced self-sustaining reaction method[J]. Advances in Applied Ceramics, 2013, 112(7):383-388.
【12】GUO W M, YANG Z G, ZHANG G J. Effect of carbon impurities on hot-pressed ZrB2-SiC ceramics[J]. Journal of the American Ceramic Society, 2011, 94(10):3241-3244.
【13】LIU J, HUANG Z, HUO C, et al. Low-temperature rapid synthesis of rod-like ZrB2 powders by molten-salt and microwave co-assisted carbothermal reduction[J]. Journal of the American Ceramic Society, 2016, 99(9):2895-2898.
【14】GUO W M, ZHANG G J. New borothermal reduction route to synthesize submicrometric ZrB2 powders with low oxygen content[J]. Journal of the American Ceramic Society, 2011, 94(11):3702-3705.
【15】ZHOU Y, MENG Q, YOU D, et al. Selective removal of aberrant extender units by a type Ⅱ thioesterase for efficient FR-008/candicidin biosynthesis in streptomyces sp. strain FR-008[J]. Applied & Environmental Microbiology, 2008, 74(23):7235-7242.
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