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采用共沉淀法制备纳米氧化钇稳定的四方氧化锆(yttria stabilized tetragonal zirconia,3Y-TZP)粉体。利用X射线衍射、N2吸附–脱附等温线,透射电子显微镜对3Y-TZP粉体的物理性能和化学性能进行表征。研究了纳米3Y-TZP粉体的烧结曲线,分析了3Y-TZP素坯在烧结过程中的致密化行为和显微结构,探讨了两步烧结工艺对3Y-TZP纳米陶瓷微观结构的影响。结果表明:采用共沉淀法,在600℃煅烧2h后,可获得晶粒尺寸为13nm、晶型发育良好、团聚较少的纳米3Y-TZP粉体;采用两步烧结法,将素坯升温至1200℃保温1min后,再降温到1050℃保温35h,可获得相对密度大于98%,晶粒尺寸约为100 nm的3Y-TZP陶瓷。两步烧结法通过控制煅烧温度和保温时间,利用晶界扩散及其迁移动力学之间的差异,使晶粒生长受到抑制,样品烧结致密化得以维持,实现在晶粒无显著生长前提下完成致密化。
Abstract：A nano-sized powder of 3%(mole fraction) yttria stabilized tetragonal zirconia(3Y-TZP) was prepared by a co-precipitation method.The physical and chemical properties of 3Y-TZP powders were characterized by X-ray diffraction,N2 adsorption–desorption iso-therms and transmission electron microscope,respectively.The sintering curve of the nano-sized powder of 3Y-TZP,the densification behav-ior and microstructure of the sintered bulk were analyzed,and the influence of two-step sintering on the microstructure of the 3Y-TZP ceram-ics was discussed.The results show that the well-developed crystal and agglomeration-free nano-sized powder with the grain size of 13 nm was obtained by co-precipitation method and the subsequent calcination at 600 ℃ for 2 h.The relative density of the 3Y-TZP ceramics was >98% and the grain size was 100 nm when the green body was calcined at 1 200 ℃ for 1 min and then decreased to 1 050 ℃ for 35 h using two-step sintering method.It was found that the grain growth was inhibited and the densification of the samples was achieved through controlling the calcining temperature and holding time in the two-step sintering process utilizing the different migration kinetics between the grain boundary diffusion and the grain boundary migration.Finally,the sintered body had a full density without any grain growth.
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基本信息:
DOI：10.14062/j.issn.0454-5648.2012.03.024
中图分类号:TB383.1
引用信息:
[1]陈静,黄晓巍,覃国恒.两步烧结法制备纳米氧化钇稳定的四方氧化锆陶瓷[J].硅酸盐学报,2012,40(03):335-339.DOI:10.14062/j.issn.0454-5648.2012.03.024.
基金信息:
福建省自然科学基金(2008J0146)资助項目
2012-02-17
2012-02-17
2012-02-17