溶胶凝胶、碳热/硼热还原法制备ZrB_(2)-SiC-LaB_(6)超细复相粉体  

Preparation of ZrB_(2)-SiC-LaB_(6) ultrafine multiphase powders by sol-gel and carbothermal/borothermal reduction

作　　者：周哲 夏大旺 李智 廖桓毅 金鑫 ZHOU Zhe;XIA Dawang;LI Zhi;LIAO Huanyi;JIN Xin(School of Materials Science and Engineering,Changsha University of Science and Technology,Changsha 410114,China;School of Materials Science and Engineering,Xiangtan University,Xiangtan 411105,China)

机构地区：[1]长沙理工大学材料科学与工程学院,长沙410114 [2]湘潭大学材料科学与工程学院,湘潭411105

出　　处：《粉末冶金材料科学与工程》2023年第3期223-232,共10页Materials Science and Engineering of Powder Metallurgy

基　　金：湖南省教育厅自然科学研究项目(21B0352)。

摘　　要：以氧氯化锆(ZrOCl_(2)·8H_(2)O)、硼酸(H_(3)BO_(3))、水合氯化镧(LaCl_(3)·7H_(2)O)、正规酸乙酯(TESO)和葡萄糖(C_(6)H_(12)O_(6))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ZrB_(2)-SiC-LaB_(6)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ZrB_(2)-SiC-LaB_(6)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1500℃保温2 h,可合成高纯ZrB_(2)-SiC-LaB_(6)超细复相粉体。颗粒平均粒径为300 nm,其中ZrB_(2)相为六方晶系,SiC相和LaB_(6)相为立方晶系,三元微晶平均尺寸为33.2 nm。ZrB_(2)-SiC-LaB_(6) ultrafine multiphase powders were prepared by the way of sol-gel method and carbothermal/borothermal reduction process,using zirconium oxychloride(ZrOCl_(2)·8H_(2)O),boric acid(H_(3)BO_(3)),hydrated lanthanum chloride(LaCl_(3)·7H_(2)O),ethyl orthoate(TESO),and glucose(C_(6)H_(12)O_(6))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,ZrB_(2)-SiC-LaB_(6) superfine multiphase powders can be synthesized by holding at 1500℃for 2 h under argon atmosphere.The average particle size of multiphase powder is 300 nm,in which ZrB_(2) phase is hexagonal crystal system,SiC and LaB_(6) phase are cubic system,and the average size of ternary crystallite is 33.2 nm.

关 键 词：ZrB_(2)-SiC-LaB_(6) 溶胶凝胶 碳热/硼热还原 超细复相粉体 超高温陶瓷 

分 类 号：U465.3[一般工业技术—材料科学与工程]