溶胶凝胶、碳热/硼热还原法制备ZrB<sub>2</sub>-SiC-LaB<sub>6</sub>超细复相粉体

doi:10.19976/j.cnki.43-1448/TF.2023005

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摘要以氧氯化锆(ZrOCl₂∙8H₂O)、硼酸(H₃BO₃)、水合氯化镧(LaCl₃∙7H₂O)、正规酸乙酯(TESO)和葡萄糖(C₆H₁₂O₆)为主要原料,以聚乙二醇(PEG)为分散剂,采用溶胶凝胶法和碳热/硼热还原工艺制备ZrB₂-SiC-LaB₆超细复相粉体。利用X射线衍射、扫描电镜、红外光谱和差示扫描量热分析等对ZrB₂-SiC-LaB₆粉体进行表征,研究烧结温度、原料配比对复相粉体合成过程的影响。结果表明,当原料中n(Zr)∶n(B)∶n(Si)∶ n(La)∶n(C)=1∶3∶0.7∶0.16∶8时,在氩气气氛中1 500 ℃保温2 h,可合成高纯ZrB₂-SiC-LaB₆超细复相粉体。颗粒平均粒径为300 nm,其中ZrB₂相为六方晶系,SiC相和LaB₆相为立方晶系,三元微晶平均尺寸为33.2 nm。

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	周哲
	夏大旺
	李智
	廖桓毅
	金鑫

关键词 ： ZrB₂-SiC-LaB₆, 溶胶凝胶, 碳热/硼热还原, 超细复相粉体, 超高温陶瓷

Abstract：ZrB₂-SiC-LaB₆ ultrafine multiphase powders were prepared by the way of sol-gel method and carbothermal/borothermal reduction process, using zirconium oxychloride (ZrOCl₂·8H₂O), boric acid (H₃BO₃), hydrated lanthanum chloride (LaCl₃·7H₂O), ethyl orthoate (TESO), and glucose (C₆H₁₂O₆) as the main raw materials, polyethylene glycol (PEG) as the dispersant. The effects of different temperatures and raw material ratios on the synthesis process of composite powders were studied and characterized by X-ray diffraction, SEM, infrared spectroscopy, and differential thermal scanning. The results show that when n(Zr)∶n(B)∶n(Si)∶n(La)∶n(C) =1∶3∶0.7∶0.16∶8 in the raw material, ZrB₂-SiC-LaB₆ superfine multiphase powders can be synthesized by holding at 1 500 ℃ for 2 h under argon atmosphere. The average particle size of multiphase powder is 300 nm, in which ZrB₂ phase is hexagonal crystal system, SiC and LaB₆ phase are cubic system, and the average size of ternary crystallite is 33.2 nm.

Key words： ZrB₂-SiC-LaB₆ sol-gel carbothermal/borothermal reduction ultrafine multiphase powders ultra-high temperature ceramics

收稿日期: 2023-01-19 出版日期: 2023-07-06

ZTFLH:

U465.3

基金资助:湖南省教育厅自然科学研究项目(21B0352)

通讯作者: 周哲,博士,讲师。电话：13627422416;E-mail: zhozuhe0810@csust.edu.cn

引用本文:

周哲, 夏大旺, 李智, 廖桓毅, 金鑫. 溶胶凝胶、碳热/硼热还原法制备ZrB₂-SiC-LaB₆超细复相粉体[J]. 粉末冶金材料科学与工程, 2023, 28(3): 223-232.
ZHOU Zhe, XIA Dawang, LI Zhi, LIAO Huanyi, JIN Xin. Preparation of ZrB₂-SiC-LaB₆ ultrafine multiphase powders by sol-gel and carbothermal/borothermal reduction. Materials Science and Engineering of Powder Metallurgy, 2023, 28(3): 223-232.

链接本文:

http://pmbjb.csu.edu.cn/CN/10.19976/j.cnki.43-1448/TF.2023005 或 http://pmbjb.csu.edu.cn/CN/Y2023/V28/I3/223

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