溶胶-凝胶法制备硅酸锆的工艺研究
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摘要
以正硅酸乙酯[Si(OC2H5)4]和氧氯化锆(ZrOCl2·8H2O)为原料,乙醇和去离子水作溶剂,NaF作矿化剂,采用溶胶-凝胶法合成硅酸锆粉体,研究制备工艺对其合成的影响,并利用XRD、SEM等测试手段分析了硅酸锆的晶相组成及其微观形貌。结果表明:样品中没有添加矿化剂时,ZrSiO4的初始合成温度高达1250℃以上,样品中加入矿化剂Na F后,经550℃热处理后就开始出现ZrSiO4的衍射峰,当温度逐渐上升至800℃时,硅酸锆的结晶程度良好并且其合成率也很高。
Zircon powders were prepared by sol-gel method using zirconium oxychloride and tetraethoxysilane as raw materials, NaF as a mineralizer, deionized water and ethanol as dissolvant to promote crystallization of zircon.The influences of sol-gel synthesis parameters on preparing zircon particles were researched by means of XRD and SEM as well. The results show that the synthesis temperature of zircon is as high as 1250 ℃ without the introduction of any mineralizers to precursor sols and that after adding sodium fluoride as mineralizer to the sols, the diffraction peak of zircon appears at 550 ℃, and the zircon synthesized at 800 ℃ not only shows good crystal growth, but also has high synthesis rate, indicating the successful synthesis of zircon at low temperatures.
Zircon powders were prepared by sol-gel method using zirconium oxychloride and tetraethoxysilane as raw materials, NaF as a mineralizer, deionized water and ethanol as dissolvant to promote crystallization of zircon.The influences of sol-gel synthesis parameters on preparing zircon particles were researched by means of XRD and SEM as well. The results show that the synthesis temperature of zircon is as high as 1250 ℃ without the introduction of any mineralizers to precursor sols and that after adding sodium fluoride as mineralizer to the sols, the diffraction peak of zircon appears at 550 ℃, and the zircon synthesized at 800 ℃ not only shows good crystal growth, but also has high synthesis rate, indicating the successful synthesis of zircon at low temperatures.
引文
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[7]陆彩飞,王秀峰,等.纳米硅酸锆的水热合成[J].硅酸盐学报,2000,28(7):87-90.
[8]陆彩飞,王秀峰,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.
[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.
[2]KubotaY,YamamooS,MoriT.Changes of microstructural and high temperature strength of ceramic composite in the mullite-ZrO_2-Al_2O_3 system using an in situ reaction between synthetic zircon and AIO.J.Ceram.Soc.J pn.1994.102(1):94.
[3]SHI Y,HUANG X X,Y AND S.Preparation and characterization of highly pure fine zircon powder[J].Eur Ceram Soc,1994,13(2):113-119.
[4]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.
[5]KANNO Y.T hermody namic and crystallographic discussion of the formation and dissociation of zircon[J].Mater Chem,1989,24:2415-2420.
[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.
[7]陆彩飞,王秀峰,等.纳米硅酸锆的水热合成[J].硅酸盐学报,2000,28(7):87-90.
[8]陆彩飞,王秀峰,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.
[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.