以无机盐氧氯化锆(ZrOCl2·8H2O)为原料, H2O2为水解促进剂, 乙醇为溶剂, 低pH值条件下制备了纤维状ZrO2水合物. 运用FT-IR、TG、XRD研究了ZrO2水合物的组成、结构和热稳定性, 用光学显微镜、FESEM对ZrO2水合物的形貌及其形成机理进行了分析. 结果表明, ZrO2水合物分子简式为Zr(μ-OH)2(OH)2·2H2O; 经80℃干燥的ZrO2水合物为非晶态, 随热处理温度的升高, 物相结构由亚稳四方相向单斜相转变; ZrO2水合物是由尺寸较小的短纤维通过表面羟基的氢键作用, 按一定方式聚集而成的尺寸较大的纤维簇.
Hydrous zirconia was prepared at low pH values with ZrOCl2·8H2O as raw material, H2O2 as hydrolysis promoter and ethanol as solvent. FT-IR, TG and XRD were applied to study the components, structure and heat-stabilization of hydrous zirconia. Light microscope and FESEM were used to analyze the microcosmic structure of hydrous zirconia, its formation mechanism was also discussed. The results show that the molecular formula of hydrous zirconia is Zr(μ-OH)2(OH)2·2H2O. The hydrous zirconia is amorphous, and as the treating temperature rising, it will turn from metastable tetragonal phase to monoclinic phase. The hydrous zirconia is fiber cluster composed of small short fibers via hydrogen bonds.
[1] 郑文裕, 陈潮钿, 陈仲丛(ZHENG Wen-Yu, et al). 无机盐工业(Inorganic Chemicals Industry), 2000, 32 (1): 18--20.
[2] Reddy B M, Sreekanth P M, Reddy V R. Journal of Molecular Catalysis A : Chemical, 2005, 225 (1): 71--78.
[3] Stefanic G, Music S, Grzeta B, et al. Journal of Physics Chemistry of Solids, 1988, 59 (6): 879--885.
[4] 王昕, 李镇江, 杨丰科, 等(WANG Xin, et al). 化工学报(Journal of Chemical Industry and Engineering), 1999, 50 (4): 519--523.
[5] 汤皎宁, 靳喜海, 高濂(TANG Jiao-Ning, et al). 无机材料学报(Journal of Inorganic Materials), 2003, 18 (6): 1367--1371.
[6] 李懋强(LI Mao-Qiang). 中国粉体技术(China Powder Science and Technology), 2000, 6 (5): 13--18.
[7] Matsui K, Ohgai M. Journal of the American Ceramic Society, 2001, 84 (10): 2303--2312.
[8] Matsui K, Ohgai M. Journal of the American Ceramic Society, 2000, 83 (6): 1386--1392
[9] Amit S, Louis M T, Gregory B, et al. Journal of Colloid and Interface Science, 1997, 194 (2): 470--481.
[10] 周彩华, 何超, 胡行方, 等(ZHOU Cai-Hua, et al). 玻璃与搪瓷(Glass and Porcelain Enamel), 2001, 29 (4): 41--44.
[11] Guo G Y, Chen Y L, Ying W J. Materials Chemistry and Physics, 2004, 84 (2-3): 308--314.
[12] 王大志, 罗毅, 杨兰, 等(WANG Da-Zhi, et al). 化学物理学报(Chinese Journal of Chemical Physics), 2000, 13 (4): 481--486.
[13] Jones S L, Norman C J. Journal of the American Ceramic Society, 1988, 71 (4): 190--191.
[14] Liang J L, Jiang X, Liu G, et al. Materials Research Bulletin, 2003, 38 (1): 161--168.
[15] Guo G Y, Chen Y L. Journal of Solid State Chemistry, 2005, 178 (5): 1675--1682.
[16] Stanley L J, Colin J N. Journal of the American Ceramic Society, 1988, 71 (4): 190--191.
[17] Huang C Y, Tang Z L, Zhang Z T. Journal of the American Ceramic Society, 2001, 84 (7): 1637--1638.
[18] 郭祝昆, 林祖纕, 严东生(KUO Zhu-Kun, et al). 高温相平衡和相图, 第1版. 上海: 上海科学技术出版社, 1987. 208--213.