硅酸盐学报

以钼酸钠为熔盐制备硅酸锆晶须

单位：1. 景德镇陶瓷学院材料科学与工程学院江西景德镇 333000 2. 江西省先进陶瓷材料重点实验室江西景德镇 333001

关键词：硅酸锆晶须非水解溶胶-凝胶工艺熔盐法

分类号：TQ 174

出版年,卷(期):页码：2015,43(3):798-802

DOI：10.14062/j.issn.0454-5648.2015.06.15

摘要：

以无水四氯化锆为锆源、正硅酸乙酯为硅源、无水乙醇为溶剂、钼酸钠为熔盐介质，采用非水解溶胶-凝胶工艺结合熔盐法制备硅酸锆晶须，研究熔盐存在条件下硅酸锆干凝胶的物相转变以及熔盐的引入、热处理温度及保温时间等对硅酸锆晶体一维择优生长的影响。熔盐的加入不仅降低了硅酸锆的合成温度，而且对其一维生长有明显促进作用；热处理温度过高或过低、保温时间过长或过短均不利于硅酸锆晶须的形成。850 ℃保温3 h能制备出产率高、直径在50~100 nm，长径比为20~30、沿[001]方向择优生长的硅酸锆晶须。

Zircon whiskers were synthesized by a non-hydrolytic sol-gel process combined with a molten salt method with anhydrous zirconium tetrachloride as zirconium source, tetraethylorthosilicate (TEOS) as silicon source, anhydrous ethanol as a solvent, sodium molybdate as a molten salt. The phase transition of zircon dry gel in the presence of the molten salt as well as the influences of molten salt, heat treatment temperature and holding time on the one- dimensional preferential growth of zircon crystal were investigated. The results show that the presence of molten salt can reduce the synthesis temperature of zircon and promote the one-dimensional growth of zircon. The zircon whiskers along the growth direction of [001], the diameter of 50–100 nm and the aspect ratio of 20–30 can be synthesized at 850 ℃ for 3 h.

基金项目：

国家自然科学基金(51162013，51362014)；江西省主要学科学术和技术带头人培养计划(20113BCB22009)；江西省博士后研究人员择优资助项目(2013KY34)资助。

作者简介：

张涛(1991—)，男，硕士研究生。

参考文献：

[1] SHI Y, HUANG X X, YAN D. Preparation and characterization of highly pure fine zircon powder[J]. J Eur Ceram Soc, 1994, 13(2): 113–119.

[2] MORI T, YAMAMURA H, KOBAYASHI H, et al. Preparation of high-purity ZrSiO4 powder using sol–gel processing and mechanical properties of the sintered body[J]. J Am Ceram Soc, 1992, 75(9): 2420-2426.

[3] MORI T, YAMAMURA H, KOBAYASHI H, et al. Formation mechanism of ZrSiO4 powders[J]. J Mater Sci, 1993, 28(18): 4970-4973.

[4] KOH Y H, KIM H W, KIM H E. Microstructural evolution and mechanical properties of Si3N4–SiC (nanoparticle)–Si3N4 (whisker) composites[J]. J Mater Res, 2000, 15(02): 364-368.

[5] LEE S, CHAE H, PARK D, et al. Thermal conductivity of unidirectionally oriented Si3N4w/Si3N4 composites[J]. J Mater Sci, 2000, 35(18): 4487-4493.

[6] QIANGANG F, HEJUN L, XIAOHONG S, et al. Microstructure and growth mechanism of SiC whiskers on carbon/carbon composites prepared by CVD[J]. Mater Lett, 2005, 59(19): 2593-2597.

[7] LI S, ZHANG Y, HAN J, et al. Fabrication and characterization of SiC whisker reinforced reaction bonded SiC composite[J]. Ceram Int, 2013, 39(1): 449-455.

[8] 王三海, 江伟辉, 冯果, 等. 以炭黑为还原剂制备硅酸锆晶须的研究[J]. 无机材料学报, 2014, 29(8): 835-838. WANG Sanhai, JIANG Weihui, FENG Guo, et al. J Inorg Mater(in Chinese), 2014, 29(8): 835-838.

[9] 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(5): 1206-1211. WANG Sanhai, JIANG Weihui, FENG Guo, et al. J Synth Cryst(in Chinese), 2014, 43(5): 1206-1211.

[10] 张冰, 曹传宝, 许亚杰, 等. 熔盐法合成莫来石晶须[J]. 无机化学学报, 2005, 21(2): 277-280. ZHANG Bing, CAO Chuanbao, XU Yajie, et al. Chin J Inorg Chem(in Chinese), 2005, 21(2): 277–280.

[11] 朱伯铨, 李雪冬, 郝瑞, 等. 在硫酸钠熔盐中合成莫来石的热力学研究[J]. 硅酸盐学报, 2006, 34(1): 76-80. ZHU Boquan, LI Xuedong, HAO Rui, et al. J Chin Ceram Soc, 2006, 34(1): 76-80.

[12] ZHANG P, LIU J, DU H, et al. Molten salt synthesis of mullite whiskers from various alumina precursors[J]. J Alloys Compd, 2010, 491(1): 447-451.

[13] TESHIMA K, YUBUTA K, SUGIURA S, et al. Selective growth of calcium molybdate whiskers by rapid cooling of a sodium chloride flux[J]. Cryst Growth Des, 2006, 6(7): 1598-1601.

[14] ZHU W, ZHANG Q, XIANG L, et al. Flux-assisted thermal conversion route to pore-free high crystallinity magnesium borate nanowhiskers at a relatively low temperature[J]. Cryst Growth Des, 2008, 8(8): 2938-2945.

[15] 段玉, 路贵民, 宋兴福, 等. 高长径比硼酸镁晶须的制备及生长机理研究[J]. 无机材料学报, 2011, 26(4): 364-368. DUAN Yu, LU Guimin, SONG Xingfu, et al. Chin J Inorg Chem(in Chinese), 2011, 26(4): 364-368.

[16] TA? A C. Molten salt synthesis of calcium hydroxyapatite whiskers[J]. J Am Ceram Soc, 2001, 84(2): 295-300.

[17] 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. JIANG Weihui, ZHANG Ti, ZHU Qingxia, et al. J Chin Ceram Soc, 2011, 39(3): 383-386.

[18] 饶东生. 硅酸盐物理化学[M]. 北京: 冶金工业出版社, 1980: 60-64.

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