口腔医学研究 ›› 2017, Vol. 33 ›› Issue (3): 331-335.DOI: 10.13701/j.cnki.kqyxyj.2017.03.024

• 临床研究论著 • 上一篇    下一篇

口腔氧化锆纳米粉体的制备及性能研究

郑迎秋1,郭晓瑨2,王健1,许冉冉1,吴文慧1*   

  1. 1. 华北理工大学口腔医学院 河北 唐山 063000;
    2. 北京市通州区新华医院口腔科 北京 101100
  • 收稿日期:2016-08-22 出版日期:2017-03-20 发布日期:2017-03-22
  • 通讯作者: 吴文慧,E-mail:wuwenhui120@163.com
  • 作者简介:郑迎秋(1989~ ),女,河北唐山市人,硕士,主要从事氧化锆粉体的制备及性能的研究。

Preparation and Properties of Zirconia Nano-powders.

ZHENG Ying-qiu1, GUO Xiao-jin2, WANG Jian1, XU Ran-ran1, WU Wen-hui1*   

  1. 1. College of Stomatology, North China University of Science and Technology, Tangshan 063000, China;
    2. Department of Stomatology, Beijing Tongzhou Xinhua Hospital, Beijing 101100, China
  • Received:2016-08-22 Online:2017-03-20 Published:2017-03-22

摘要: 目的:探讨盐助溶液燃烧法(Salt-assisted solution Combustion Synthesis ,SSCS)的工艺条件,制备性能优良的3mol%氧化钇(Y2O3)稳定四方相多晶体氧化锆(3Y-TZP)纳米粉体。方法:以硝酸氧锆和尿素为原料,采用SSCS法和冷冻干燥法制备3Y-TZP纳米粉体。利用热重-差热分析(TG-DTA)、 X射线衍射仪(XRD)和透射电镜(TEM)检测分析粉体表征。采用正交试验考察了锆离子的浓度(A)、尿素和金属硝酸盐摩尔比(B)、KCL和金属硝酸盐摩尔比(C)、前驱体的引燃温度(D)对粉体晶粒度的影响。结果:前驱体引燃温度和尿素加入量是最重要的影响因素,最佳的工艺条件是A:0.085 mol/L ,B:1,C:3,D:400 ℃。产物经XRD检测分析为四方相多晶体氧化锆,晶粒度(DXRD)为2.9~9.0 nm。TEM观察在最优工艺水平下制备的粉体形貌为球形、高分散的、低团聚的、平均粒径约为5.38 nm的纳米粉体,与DXRD基本一致。并且随着引燃温度的增加粉体粒径变大,而且团聚加重。结论:通过盐助溶液燃烧法可以制备性能良好的3Y-TZP纳米粉体。

关键词: 盐助溶液燃烧法, 3Y-TZP, 纳米粉体

Abstract: Objective: To prepare the 3mol% yttria-stabilized tetragonal polycrystalline zirconia (3Y-TZP) nano-powders by using salt-assisted solution combustion synthesis (SSCS) method. Methods: 3Y-TZP nano-powders were prepared via the SSCS and freeze drying method. Thermogravimetry differential thermal analysis (TG-DTA), x-ray diffraction (XRD) and transmission electron microscopy (TEM) were employed to evaluate the ignition temperature of the precursors, the phase structure, the crystallite size, morphology, and size distribution of 3Y-TZP nano-powders. Effects of the density of zirconium ion, the ignition temperature of the precursors, the molar ratios of metal ion to urea and metal ion to KCL on size of powders were determined by orthogonal test. Results: The optimal conditions were determined as follows: 0.085 mol/L zirconium ion, 1 molar ratio of metal ion to urea, 3 molar ratio of metal ion to KCL, and ignition temperature 400℃.The products were tetragonal polycrystalline zirconia and 2.9~9.0nm in crystalline size analyzed via XRD. Under the optimal conditions, the micrographs of nano-particles were sphericity, well dispersion and low-agglomeration. The particle size was 5.38nm on the average. Conclusion: 3Y-TZP nano-powders can be prepared by the SSCS method and have high-purity, small crystalline size, narrow size distribution and low-agglomeration.

Key words: Salt-assisted solution, Combustion, 3Y-TZP , Nano-powders

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