微乳液-水热法合成超细球形硅酸锆的研究
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摘要
硅酸锆具有优良的耐腐蚀性和良好的热稳定性等优点。但是,硅酸锆粉体的大晶粒尺寸和高烧结温度限制了它的应用。采用微乳液-水热法合成超细球形硅酸锆粉体,研究了超细球形硅酸锆合成机理和工艺条件。实验结果表明:采用微乳液-水热法获得硅酸锆前驱体。在前驱体中加入1 wt%的氟化锂(LiF),经900℃煅烧0.5 h能够合成晶粒尺寸为50 nm,平均粒径约为300 nm的超细球形硅酸锆粉体。
ZrSiO_4 ceramics have many benefits, such as excellent corrosion resistance and good thermal stability. However, the large grain size and high sintering temperature of ZrSiO_4 powder have restricted their application. In this paper, ultrafine spherical ZrSiO_4 powder was synthesized by microemulsion-hydrothermal method. The synthesis mechanism and process conditions of ultrafine spherical ZrSiO_4 were studied. The experimental results show that the ZrSiO_4 precursor was obtained by microemulsion-hydrothermal method. Adding 1 wt% of LiF to the precursor and calcining at 900 ℃ for 0.5 h can synthesize ultrafine spherical ZrSiO_4 powder with crystallite size of 50 nm and average particle size of about 300 nm.
ZrSiO_4 ceramics have many benefits, such as excellent corrosion resistance and good thermal stability. However, the large grain size and high sintering temperature of ZrSiO_4 powder have restricted their application. In this paper, ultrafine spherical ZrSiO_4 powder was synthesized by microemulsion-hydrothermal method. The synthesis mechanism and process conditions of ultrafine spherical ZrSiO_4 were studied. The experimental results show that the ZrSiO_4 precursor was obtained by microemulsion-hydrothermal method. Adding 1 wt% of LiF to the precursor and calcining at 900 ℃ for 0.5 h can synthesize ultrafine spherical ZrSiO_4 powder with crystallite size of 50 nm and average particle size of about 300 nm.
引文
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[14]郭威威.半导体金属氧化物ZnO的水热合成及气敏性能研究[D].重庆:重庆大学,2013.
[2]C.Veytizou,J.F.Quinson,Y.Jorand.Preparation of zircon bodies from amorphous precursor powder synthesized by sol-gel processing[J]。Journal of the European Ceramic Society,2002,22(16):2901-2909.
[3]Q.B.Chang,X.Wang,Y.Q.Wang,et al.Encapsulated carbon black prepared by sol-gel-spraying:A new black ceramic pigment[J].J.Eur.Ceram.Soc.,2014,34(13):3151-3157.
[4]康厚军,王晓丽,卢喜瑞,张东,崔春龙,唐敬友.锆英石微粉高温固相合成研究[J].成都理工大学学报(自然科学版),2010,37(03):332-335.
[5]王衍行,周鹏,祖成奎,等.硅酸锆粉体的合成研究[J].功能材料,2015,46(S2):8-12.
[6]喻佑华,刘建磊,熊甜甜.溶胶-凝胶法低温合成硅酸锆粉体的研究[J].陶瓷学报,2017,38(3):382-385.
[7]江伟辉,张缇,朱庆霞,等.非水解凝胶化工艺对低温合成硅酸锆的影响[J].硅酸盐学报,2011,39(3):383-386.
[8]Shi Y,Huang X X,Yan D S.Preparation and characterization of highly pure fine zircon powder[J].Journal of the European Ceramic Society,1994,13(2):113-119.
[9]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(1):87-90.
[10]Tartaj P.Zircon Formation from Nanosized Powders Obtained by a Reverse Micelle Process[J].Journal of the American Ceramic Society,2005,88(1):222-224.
[11]Muhammad Faizan Nazar,Olesya Myakonkaya,Syed Sakhawat Shah,Julian Eastoe,Separating nanoparticles from microemulsions,Journal of Colloid and Interface Science.2011,354(2):624-629.
[12]王三海,江伟辉,冯果,等.非水解溶胶-凝胶法制备硅酸锆晶须初探[J].人工晶体学报,2014,43(05):1206-1211.
[13]武海虹,张文燕,路绍琰,等.微乳液法在无机纳米材料制备中的应用研究[J].盐科学与化工,2017,46(05):17-20.
[14]郭威威.半导体金属氧化物ZnO的水热合成及气敏性能研究[D].重庆:重庆大学,2013.