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出 处:《应用化学》2008年第6期637-641,共5页Chinese Journal of Applied Chemistry
基 金:国家自然科学基金资助项目(50373010)
摘 要:以氯氧化锆为原料,异丙醇为溶剂,双氧水为水解促进剂,乙酰丙酮为配位剂,采用溶胶-凝胶法制备了ZrO2前驱体连续纤维,经800℃热处理后得ZrO2连续纤维。用FT-IR、TGA、元素分析和SEM等分析技术表征了纤维的化学结构和形貌观察,研究了可纺性ZrO2溶胶的制备条件和影响因素。结果表明,当n(氯氧化锆)∶n(双氧水)=1∶3,反应时间6 h,陈化温度15℃时可得纺丝性能良好的锆溶胶,ZrO2前驱体连续纤维的成分是部分经乙酰丙酮配位的ZrO2水合物,热处理后ZrO2纤维的平均直径为15μm左右,纤维体中存在大量纳米级气孔,但没有发现明显裂纹。Continuous ZrO2 precursor fibers were prepared by the sol-gel method with zirconium oxychlorid as raw material, 2-propyl as solvent, acetylacetone as complex, and then continuous ZrO2 fibers were obtained by sintering the precursor at 800 ℃. The chemistry structure and morphology of the fibers were studied by FT-IR, TGA, elemental analysis and SEM. The process and related influencing factors of the preparation of spinnable zirconium sol were studied. The results show that the zirconium sol has a good spinnability when n( zirconium oxychlorid) : n(dioxogen) = 1 : 3, reaction time is 6 h and aging temperature is 15 ℃. The main component of the ZrO2 precursor fibers is hydrous zirconia chelated by acetyl acetone. The mean diameter of the sintered ZrO2 fibers is About 15 μm; there are lots of nanometer pores in ZrO2 fibers, and cracks are found.
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