微米晶单斜氧化锆高压相变制备亚微米四方多晶氧化锆

董丙舜 王海阔 仝斐斐 侯志强 李振 刘童 臧金浩 杨西贵

董丙舜, 王海阔, 仝斐斐, 侯志强, 李振, 刘童, 臧金浩, 杨西贵. 微米晶单斜氧化锆高压相变制备亚微米四方多晶氧化锆[J]. 高压物理学报, 2019, 33(2): 020104. doi: 10.11858/gywlxb.20190709
引用本文: 董丙舜, 王海阔, 仝斐斐, 侯志强, 李振, 刘童, 臧金浩, 杨西贵. 微米晶单斜氧化锆高压相变制备亚微米四方多晶氧化锆[J]. 高压物理学报, 2019, 33(2): 020104. doi: 10.11858/gywlxb.20190709
DONG Bingshun, WANG Haikuo, TONG Feifei, HOU Zhiqiang, LI Zhen, LIU Tong, ZANG Jinhao, YANG Xigui. Fabrication of Submicron Tetragonal Polycrystalline ZrO2 by the Transformation of Micro Monoclinic ZrO2 under High Pressure[J]. Chinese Journal of High Pressure Physics, 2019, 33(2): 020104. doi: 10.11858/gywlxb.20190709
Citation: DONG Bingshun, WANG Haikuo, TONG Feifei, HOU Zhiqiang, LI Zhen, LIU Tong, ZANG Jinhao, YANG Xigui. Fabrication of Submicron Tetragonal Polycrystalline ZrO2 by the Transformation of Micro Monoclinic ZrO2 under High Pressure[J]. Chinese Journal of High Pressure Physics, 2019, 33(2): 020104. doi: 10.11858/gywlxb.20190709

微米晶单斜氧化锆高压相变制备亚微米四方多晶氧化锆

doi: 10.11858/gywlxb.20190709
基金项目: 国家自然科学基金青年科学基金(11504087,11804307);郑州市科技重大专项(174PZDZX567)
详细信息
    作者简介:

    董丙舜(1992-),男,硕士研究生,主要从事高压下陶瓷材料的合成和物性研究. E-mail: bingshun219@163.com

    通讯作者:

    王海阔(1984-),男,博士,副教授,主要从事超硬材料合成、大腔体静高压技术和高压下材料物性研究. E-mail: haikuo_wang@haut.edu.cn

    杨西贵(1990-),男,博士,主要从事高压下碳材料的新结构和新性质研究. E-mail: yangxg@zzu.edu.cn

  • 中图分类号: O521.2

Fabrication of Submicron Tetragonal Polycrystalline ZrO2 by the Transformation of Micro Monoclinic ZrO2 under High Pressure

  • 摘要: 高压相变已逐渐发展成为一种制备纳米/亚微米多晶陶瓷块体材料的有效方法。高压可以抑制原子的长程扩散进而抑制晶粒长大,高压下截获的新相不受初始材料晶粒尺寸的制约,通过热力学调控可以得到晶粒尺寸更小的多晶块体材料。陶瓷材料在特定热力学条件下通常会发生相变,新相的形成要经历形核、生长的过程。采用晶粒尺寸为2 $ {\text{μ}} $m的单斜ZrO2与晶粒尺寸为50 nm的Y2O3以97 : 3的摩尔比混合,在5.5 GPa、800~1700 ℃温压区间内对初始材料进行烧结,采用X射线衍射、扫描电镜、透射电镜对所得样品进行表征。研究结果表明:高压下截获了单斜相和亚微米四方相复合的多晶ZrO2块体材料,1200、1400、1600和1700 ℃温度下获得的四方相的平均晶粒尺寸为(145±62) nm、(246±165) nm、(183±62) nm和(245±107) nm。利用高压相变以微米晶制备细晶粒多晶块体材料,可以避免常规方法中以纳米粉末为初始材料制备细晶粒多晶块体材料存在的团聚、吸附及晶粒长大的问题,进而发展一种以微米晶为初始材料通过高压相变制备高性能细晶粒多晶块体材料的方法。

     

  • 图  组装示意图

    Figure  1.  Schematic diagram of assembly

    图  亚微米原料和微晶ZrO2的XRD图谱(插图为ZrO2单斜相特征峰XRD图谱)

    Figure  2.  XRD pattern of submicron and microcrystalline ZrO2 (Inset: XRD pattern of the characteristic diffraction peaks of monoclinic ZrO2)

    图  亚微米晶ZrO2(a)和微米晶ZrO2(b)的SEM照片

    Figure  3.  SEM images of submicron (a) and microcrystalline ZrO2 (b)

    图  5.5 GPa不同温度条件下样品的XRD图谱(a)、单斜相和四方相的特征峰放大图谱(b)以及(a)中方框标记的800和1000 ℃条件下合成样品的XRD图谱(c)

    Figure  4.  (a) XRD pattern of samples sintered at 5.5 GPa and different temperatures; (b) magnified range of the characteristic diffraction peaks of monoclinic and tetragonal phases from (a); (c) XRD patterns of samples sintered at 800 and 1000 ℃ marked with dotted line in (a)

    图  (a) 1400 ℃温度条件下样品中亚微米晶粒的SEM照片,(b) (a)中箭头所指亚微米晶粒的EDS能谱,(c) 1700 ℃温度条件下样品中亚微米晶粒的SEM照片,(d) (c)中箭头所指亚微米晶粒的EDS能谱

    Figure  5.  (a) SEM images of submicron grains in the sample sintered at 1400 ℃; (b) EDS spectra of the submicron grain directed by the arrow; (c) SEM images of submicron grains in the sample sintered at 1700 ℃; (d) EDS spectra of the submicron grain directed by the arrow

    图  5.5 GPa、不同温度下合成样品的SEM照片

    Figure  6.  SEM images of samples sintered at the condition of 5.5 GPa and different temperatures

    图  5.5 GPa不同温度下合成样品中亚微米晶粒的晶粒尺寸分布

    Figure  7.  Grain size distribution of submicron grains in samples sintered at 5.5 GPa and different temperatures

    图  5.5 GPa、1700 ℃合成样品的TEM照片((a)样品中亚微米晶粒的低倍TEM照片;(b)样品中亚微米晶粒的HRTEM照片,插图为虚线椭圆部位的放大图)

    Figure  8.  TEM images of the sample sintered at 5.5 GPa and 1700 ℃ ((a) Low-magnification TEM image of submicron grains in the sample; (b) HRTEM image of submicron grains in the sample. Inset: Magnified HRTEM image marked with the dotted ellipse in (b))

    表  1  室温下稳定四方相氧化锆的晶胞参数

    Table  1.   Unit-cell parameters of tetragonal zirconia stabilized at room temperature

    Sample Processing temperature/℃ a/nm c/nm Test method
    Tetragonal zirconia 1400 0.3607(6) 0.5219(8) XRD
    Tetragonal zirconia 1700 0.3615(5) 0.5168(3) XRD
    ZrO2[42] 0.3591(1) 0.5169(1) Neutron diffraction
    Zr0.94Y0.06O1.97[43] 0.3610 0.5168 XRD
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  • 收稿日期:  2019-01-10
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