Abstract：Abstract: Using zirconium n-propoxide (C12H28O4ZR) as the zirconium source, boric acid (H3BO3) as the boron source, sorbitol (C6H14O6) as the carbon source, and acetic acid (C2H4O2) as the solvent, high-purity and ultrafine particlesof Zirconium boride (ZrB2) powder were prepared by the sol-gel cooperative carbothermic reduction method. The effects of carbon content and boron content on the phase and morphology of the product were studied respectively. The zirconium boride powder was characterized and analyzed by X-ray diffractometer, Raman spectrometer, scanning electron microscope, transmission electron microscope and its own X-ray energy spectrometer. The results shown that when the molar ratio of boron to zirconium in the initial raw materials is 3 and the molar ratio of carbon to zirconium is 11, the ZrB2 powder with the best comprehensive properties such as morphology and particle size can be obtained. The zirconium boride particles are spherical or quasi-spherical, with clear particle boundaries, good dispersion, and a particle size distribution between 300 and 500 nm..
[1]杨路平, 周长灵, 王艳艳, 姜凯, 刘福田.超高温材料的研究进展[J].佛山陶瓷, 2017, 27(10):1-7[2]Zhang X.Hu P,Du S.,Han J.,Meng S.. Research progress on ultra-high temperature ceramic composites[J].Chinese Science Bulletin, 2015, 60(3):257-266[3]Levine S.R.,Opila EJ.,Halbig M.C.,Kiser J.D.,Singh M.,Salem J.A.. Evaluation of ultra-high temperature ceramics foraeropropulsion use[J].Journal of the European Ceramic Society, 2002, 22(14-15):2757-2767[4]杨磊, 孙静, 桂涛, 刘宇阳, 白雪, 王星明.添加剂对碳热还原反应制备粒径及形貌的影响[J].稀有金属, 2017, 41(12):1352-1358[5]Reich S.Suhr H,Hankó K.,Szepes L.. Deposition of thin films of Zirconium and Hafnium Boride by plasma enhanced chemical vapor deposition[J].Advanced Materials, 1992, 4(10):650-653[6]张云, 李锐星, 姜沿杉, 赵斌, 李军平, 冯志海.湿化学法合成纳米粉末[J].无机化学学报, 2011, 27(09):1788-1792[7]朱时珍, 车晓盼, 徐强, 刘玲.溶胶-凝胶前驱体裂解法合成超细粉英文[J].稀有金属材料与工程, 2010, 39(S2):18-21[8]张云, 王杰.溶胶-凝胶及碳热还原法制备六角形貌的粉末[J].稀有金属, 2020, 44(04):433-439[9]Guo S.Q.. Densification of ZrB2-based composites and their mechanical and physical properties: A review[J].Journal of the European Ceramic Society, 2009, 29(6):995-1011[10]Cao Y.N.,Du S,Wang J.K.,Zhang H.,Li F.L.,Lu L.L.,et al. Preparation of zirconium diboride ultrafine hollow spheres by a combined sol–gel and borocarbothermal reduction technique[J].Journal of Sol-Gel Science and Technology, 2014, 72(1):130-136[11]Venugopal S.Boakye EE.,Paul A.,Keller K.,Mogilevsky P.,Vaidhyanathan B.,et al. Sol-Gel Synthesis and Formation Mechanism of Ultrahigh Temperature Ceramic: HfB2[J].Journal of the American Ceramic Society, 2014, 97(1):92-99[12]王东伟, 战东平, 屈乐欣, 周永欣, 姜周华, 张慧书.烧结温度对 钢力学性能的影响研究[J].金属功能材料, 2020, 27(03):11-17[13]Hu C.Zou J,Huang Q.,Zhang G.,Guo S.,Sakka,Y.,et al. Synthesis of Plate-Like ZrB2 Grains[J].Journal of the American Ceramic Society, 2012, 95(1):85-88[14]Ma L.Yu J,Guo X.,Zhang Y.,Feng Y.,Zong H.,et al. Effects of HBO2 on phase and morphology of ZrB2 powders synthesized by carbothermal reduction[J].Ceramics International, 2017, 43(15):12975-12978[15]Li R.Zhang Y,Lou H.,Li J.,Feng Z.. Synthesis of ZrB2 nanoparticles by sol-gel method[J].Journal of Sol-Gel Science and Technology, 2011, 58(2):580-585[16]Zhao Y.Li JP.,Wang T.Y.,Li R.X.,Feng Z.H.,Cai H.N.. Synthesis of ZrB2 Nanoparticles by Using Xylitol[J].Journal of Inorganic Materials, 2016, 31(6):597-602[17]Yin T.Jiang B,Su Z.,Huang Q.. Effects of mannitol on the synthesis of ultra-fine ZrB2 powders[J].Journal of Sol-Gel Science and Technology, 2017, 85(1):41-47[18]王恩元, 谢建林, 李学钊.碳热还原法合成粉体及其游离碳的去除[J].耐火材料, 2015, 49(06):435-437[19]Guo W.M.,Zhang GJ.,Silvestroni L.. 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[20]刘海, 杨静, 唐明国, 潘小强, 庾正伟, 张雨.碳热还原法制备高纯粉体[J].金属热处理, 2019, 44(02):7-11[21]Guo W.M.,Zhang GJ.. Reaction Processes and Characterization of ZrB2 Powder Prepared by BoroCarbothermal Reduction of ZrO2 in Vacuum[J].Journal of the American Ceramic Society, 2009, 92(1):264-267[22]Khanra A.K.,Pathak LC.,Godkhindi M.M.. Carbothermal synthesis of zirconium diboride (ZrB2) whiskers[J].Advances in Applied Ceramics, 2013, 106(3):155-160[23]Miao Y.Wang X,Firbas P.,Wang K.,Yang Z.,Liang B.,et al. Ultra-fine zirconium diboride powders prepared by a combined sol–gel and spark plasma sintering technique[J].Journal of Sol-Gel Science and Technology, 2015, 77(3):636-641[24]Watts J.Hilmas G,Fahrenholtz W.G.,Brown D.,Clausen B.. Stress measurements in ZrB2–SiC composites using Raman spectroscopy and neutron diffraction[J].Journal of the European Ceramic Society, 2010, 30(11):2165-2171[25]康峰, 纪维强, 刘维国, 孔立军, 温建明.硅锰合金生产利润空间最大化途径探寻[J].金属功能材料, 2021, 28(02):87-94
2022, Vol. 29 