The Preparation,Stability of Zirconium Sol and Characteristics of ZrO2 Powder
摘 要
以氧氯化锆为前驱体,采用溶胶-凝胶法快速制备锆溶胶,凝胶后经煅烧制得氧化锆粉体,分析了锆溶胶的制备、稳定和氧化锆粉体的特性.结果表明:随着H2O2与ZrOCl2·8H2O摩尔数的比值m的增大,锆溶胶形成所需的pH值也逐渐增大;m为4~6,且pH值为3~4.5时,所得的溶胶最稳定;随m值的增大,凝胶干燥后氧化锆粉体粒径减小,分布变窄;m为4时,氧化锆粉体的平均粒径为21.4 μm.粉体在450 ℃热处理时有四方相ZrO2析出,随着温度升高,四方相ZrO2结晶趋于完整,并开始析出少量单斜相;900 ℃时亚稳态四方相大部分转化成单斜相;1 020 ℃时转变完成,此时得到粉体粒径在100 nm左右.
Abstract
The zirconium sol was rapidly prepared by sol-gel method with zirconium oxychloride as precursor reagent.The dried gel was calcined to ZrO2 powder.The preparation and stability of zirconium sol and characteristics of ZrO2 powder were analyzed.The pH value for formation of zirconium sol increased with the mole ratio (m) of H2O2 and ZrOCl2·8H2O,and the zirconium sol was stable at m=4-6 and pH=3-4.5.The particle size of dried gel powder decreased and particle-size distribution became narrow with the increase of m,and the mean particle size of dried powder was 21.4 μm at m=4.The crystal phase of ZrO2 powder after calcined at 450 ℃ was tetragonal,transformed into monoclinic after calcined at 900 ℃ and became complete monoclinic after calcined at 1 020 ℃ with a average particle size of 100 nm.
中图分类号 TB321
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收稿日期 2005/6/30
修改稿日期 2005/9/5
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备注宋芳芳(1983-),女,河南洛阳人,硕士研究生.
引用该论文: SONG Fang-fang,GUO Xing-zhong,CHENG Ben-jun,YANG Hui. The Preparation,Stability of Zirconium Sol and Characteristics of ZrO2 Powder[J]. Materials for mechancial engineering, 2006, 30(7): 72~74
宋芳芳,郭兴忠,程本军,杨辉. 锆溶胶的制备、稳定及氧化锆粉体的特性[J]. 机械工程材料, 2006, 30(7): 72~74
被引情况:
【1】邹阳,顾华志,黄奥,张美杰,吉超, "Zr(OH)4添加量对Al2O3-MgO浇注料基质显微结构和阻力系数的影响",机械工程材料 39, 77-80(2015)
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【8】Stefanic G,Popvic S,Music S.Influence of pH on the hydrothermal crystallization kinetics and crystal structure of ZrO2[J].Thermochemica Acta,1997,303:31-39.
【9】Moon Y T,Kim D K,Kin C H.Preparation of monodiesperse ZrO2 by the microwave heating of zirconyl chloride solution[J].J Am Cera Soc,1995,78(4):103-106.
【10】周勋海,顾华志,汪厚植,等.氧氯化锆前驱体制备氧化锆的机理探讨[J].无机盐工业,2004,36(3):14-16.
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