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不同锆源对聚丙烯酰胺凝胶法制备氧化锆纳米粉体的影响
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内蒙古工业大学

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国家自然科学基金资助(51164023,51364026);内蒙古自然科学基金资助(2016MS0505);内蒙古工业大学科学研究项目(X201410)资助


Effect of Zirconium Salts on Preparation of Zirconia Nanopowders via Polyacrylamide Gel Route
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Inner Mongolia University of Technology

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    摘要:

    采用聚丙烯酰胺凝胶法,分别以氧氯化锆、硫酸锆和硝酸氧锆为锆源制备ZrO2纳米粉体,利用热重-差热同步分析仪(TG-DSC)、X射线衍射仪(XRD)和扫描电子显微镜(SEM) 分别对凝胶的热分解过程及氧化锆粉体的物相组成和形貌进行分析和表征,研究了不同锆源对聚丙烯酰胺凝胶法所制备的ZrO2纳米粉体相转变、物相组成及粉体形貌的影响。结果表明,锆盐影响聚丙烯酰胺凝胶的热分解完全温度,以硝酸氧锆为前驱体制得的凝胶热分解完全温度最低,约为530 ℃,以硫酸锆和氧氯化锆为前驱体制得的凝胶热分解完全温度分别为573 ℃和580 ℃。锆盐影响氧化锆的晶化温度,但氧化锆的相转变过程相似,均是由无定型氧化锆转变为四方相氧化锆,并在900 ℃时完全转变为单斜相氧化锆。氧化锆的晶化温度越高,平均粒径越小,团聚程度越高,以上述三种锆源为前驱体均可制备出近似球形的纳米氧化锆粉体,粉体粒径分布在52~97.4 nm范围内。

    Abstract:

    Zirconia nanopowders were prepared via polyzcrylamide gel route with different zirconium salt, including ZrOCl2·8H2O, Zr(SO4)2·4H2O and ZrO(NO3)2·2H2O. Thermogravimetric analysis (TG), differential scanning calorimetry analysis (DSC), X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to characterize the thermal decomposition process of xerogel, phase compositions and morphologies of zirconia nanopowders. The influence of different zirconium salts on the phase transformation, phase compositions and morphologies of the as-prepared zirconia nanopowders by polyacrylamide gel route were studied. The results demonstrate that zirconium salt affects thermo-decomposing temperature of polyacrylamide gel. When precursor is zirconium oxynitrate, the thermo-decomposing temperature of xerogel is the lowest which is around 530 ℃. When precursors are zirconium sulfate and zirconium oxychloride, the thermo-decomposing temperatures of xerogels are around 573 ℃ and 580 ℃, respectively. Zirconium salt affects the crystallization temperature of zirconia, but the phase transformation of zirconia is similar, which transforms from amorphous to tetragonal and completely converts to monoclinic at 900 ℃. The higher the crystallization temperature of zirconia, the smaller the mean particle size, the more particle agglomeration. The nearly spherical zirconia nanopowders can be prepared and the particle size distribution is within the range of 52~97.4 nm with the above three zirconium salts as precursors.

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刘婷,陈伟东,鞠红民,闫淑芳,马文.不同锆源对聚丙烯酰胺凝胶法制备氧化锆纳米粉体的影响[J].稀有金属材料与工程,2019,48(6):2044~2048.[Liu Ting, Chen Weidong, Ju Hongmin, Yan Shufang, Ma Wen. Effect of Zirconium Salts on Preparation of Zirconia Nanopowders via Polyacrylamide Gel Route[J]. Rare Metal Materials and Engineering,2019,48(6):2044~2048.]
DOI:10.12442/j. issn.1002-185X.20171201

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  • 收稿日期:2017-12-26
  • 最后修改日期:2018-02-23
  • 录用日期:2018-03-12
  • 在线发布日期: 2019-07-30
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