溶胶-凝胶法低温合成硅酸锆粉体
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摘要
采用溶胶-凝胶法(sol-gel)合成ZrSiO4粉体,以正硅酸乙酯[Si(OC2H5)4]和氧氯化锆(ZrOCl2·8H2O)为原料,无水乙醇和去离子水为溶剂,氟化钠为矿化剂,并借助XRD、SEM等测试手段分析了合成样品的晶相组成及其微观形貌。结果表明:没有引入矿化剂的样品,合成硅酸锆的初始温度高达1250℃以上,当温度达到1500℃时,硅酸锆的合成率也不是很高;然而,在溶胶中引入矿化剂NaF后,前驱体热处理温度为550℃时,粉体中开始有ZrSiO4的晶相生成,当温度升高至800℃时,硅酸锆的晶相含量已经很高,结晶程度很好。
Zircon powders were prepared by sol-gel method at low temperature using zirconium oxychloride and tetraethoxysilane as raw materials, deionized water and ethanol as dissolvants, NaF as a mineralizer to promote crystallization of zircon powder. The characterization techniques such as XRD and SEM are used to analyze the phase composition and the microstructures. The results show that the original synthesis temperature of zircon is as high as 1250 ℃ without the introduction of any mineralizers to precursor sols, when the temperature is raised up to 1500 ℃, the synthesis ratio of zircon powder is not very high, however, by adding sodium fluoride as a mineralizer to the sols, the crystalline phase of zircon appears at 550 ℃ and the zircon powder which is calcined at the temperature of 800 ℃ not only has a high synthesis ratio, but also shows good crystallinity.
Zircon powders were prepared by sol-gel method at low temperature using zirconium oxychloride and tetraethoxysilane as raw materials, deionized water and ethanol as dissolvants, NaF as a mineralizer to promote crystallization of zircon powder. The characterization techniques such as XRD and SEM are used to analyze the phase composition and the microstructures. The results show that the original synthesis temperature of zircon is as high as 1250 ℃ without the introduction of any mineralizers to precursor sols, when the temperature is raised up to 1500 ℃, the synthesis ratio of zircon powder is not very high, however, by adding sodium fluoride as a mineralizer to the sols, the crystalline phase of zircon appears at 550 ℃ and the zircon powder which is calcined at the temperature of 800 ℃ not only has a high synthesis ratio, but also shows good crystallinity.
引文
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[2]KUBOTA Y,YAMAMOO S,MORI T.Changes of microstructural and high temperature strength of ceramic composite in the mullite-Zr O2-Al2O3 system using an in situ reaction between synthetic zircon and Al O.J.Ceram.Soc.Jpn.,1994,102(1):94.
[3]SHI Y,HUANG X X YAN D S.Preparation and characterization of highly pure fine zircon powder[J].J.Eur.Ceram.Soc.,1994,13(2):113-119.
[4]陆彩飞,王秀峰,苗鸿雁,等.纳米硅酸锆的水热合成[J].硅酸盐学报,2000,28(7):87-90.LU Caifei,et al.Journal of the Chinese Ceramic Society,2000,28(7):87-90.
[5]陆彩飞,王秀峰,苗鸿雁,等.水热合成纳米硅酸锆工艺因素分析[J].中国粉体技术,1999,26(5):21-23.LU Caifei,et al.China Powder Science and Technology,1999,26(5):21-23.
[6]江伟辉,周艳华,魏恒勇,等.非水解溶胶-凝胶法低温合成硅酸锆粉体[J].中国陶瓷,2009,44(7):20-22.JIANG Weihui,et al.China Ceramics,2009,44(7):20-22.
[7]杜春生,葛志平,杨正方,等.溶胶-凝胶法合成高纯锆英石粉[J].硅酸盐学报,1999,27(3):346-350.DU Chunsheng,et al.Journal of the Chinese Ceramic Society,1999,27(3):346-350.
[8]KANNO Y.Thermodynamic and crystallographic discussion of the formation and dissociation of zircon[J].Mater.Chem.,1989,24:2415-2420.
[9]方培育,吴建清.低温水热法合成高纯的硅酸锆粉体[J].硅酸盐学报,2009,37(4):305-319.FANG Peiyu,et al.Journal of the Chinese Ceramic Society,2009,37(4):305-319.
[10]董雪亮,滕元成,曾冲盛,等.溶胶-凝胶法合成硅酸锆[J].中国粉体技术,2010,16(6):4-7.DONG Xueliang,et al.China Powder Science and Technology,2010,16(6):4-7.
[11]江伟辉,程思,朱庆霞,等.氯化钠抑制硅酸锆纳米粉体团聚的研究[J].陶瓷学报,2012,33(4):420-424.JIANG Weihui,et al.Journal of Ceramics,2012,33(4):420-424.
[12]朱庆霞,江伟辉,杨延辉,等.非水解溶胶-凝胶法制备锆铁红色料影响因素的研究[J].人工晶体学报,2014,43(1):116-121.ZHU Qingxia,et al.Journal of Synthetic Crystals,2014,43(1):116-121.
[13]包启富,常启兵,王霞,等.溶胶-凝胶法制备包裹炭黑色料及表征[J].陶瓷学报,2013,34(4):421-424.BAO Qifu,et al.Journal of Ceramics,2013,34(4):421-424.