振荡压力烧结法制备高致密度细晶粒氧化锆陶瓷

doi:10.15541/jim20150385

无机材料学报 ›› 2016, Vol. 31 ›› Issue (2): 207-212.DOI: 10.15541/jim20150385

振荡压力烧结法制备高致密度细晶粒氧化锆陶瓷

李双^1,2, 谢志鹏¹

(1. 清华大学材料学院, 新型陶瓷与精细工艺国家重点实验室, 北京100084; 2. 山东理工大学资源与环境工程学院, 淄博255049)

收稿日期:2015-08-17 修回日期:2015-09-30 出版日期:2016-02-20 网络出版日期:2016-01-15
作者简介:李双(1981–), 男, 博士, 讲师. E-mail: shuangli1981@gmail.com
基金资助:
国家自然科学基金项目(51427802)

Preparation of Zirconia Ceramics with High Density and Fine Grains by Oscillatory Pressure Sintering

LI Shuang^1,2, XIE Zhi-Peng¹

(1. State Key Laboratory of New Ceramics and Fine Processing, School of Materials Science and Engineering, Tsinghua University, Beijing 100084, China; 2. School of Resources and Environmental Engineering, Shandong University of Technology, Zibo 255049, China)

Received:2015-08-17 Revised:2015-09-30 Published:2016-02-20 Online:2016-01-15
About author:LI Shuang. E-mail: shuangli1981@gmail.com
Supported by:
National Natural Science Foundation of China (51427802)

摘要/Abstract

摘要：

针对重大工程和关键技术对高强韧性、高可靠性陶瓷部件的迫切需求, 本研究提出了适用于高性能陶瓷制备的振荡压力烧结(Oscillatory Pressure Sintering, OPS)新方法, 并采用此种方法制备了高致密度、细晶粒、高强度和高可靠性的氧化锆陶瓷。作为对比, 在相同的温度条件下分别采用无压烧结(Pressureless Sintering, PS)和热压烧结(Hot Pressing, HP)制备了氧化锆陶瓷。SEM研究表明振荡压力抑制了高温下氧化锆晶粒的快速生长, 统计表明OPS氧化锆的平均晶粒尺寸为251 nm, 而PS氧化锆、HP氧化锆的平均晶粒尺寸分别为451 nm和298 nm。另外, 振荡压力引发的晶粒塑性形变和晶界滑移促进了晶界处闭气孔的排出, 使OPS氧化锆的体积密度提高到99.7%。氧化锆致密度的提高及晶粒细化使其断裂强度从1003 MPa提高到1572 MPa, Weibull模数从13提高到32。另外, 低温老化实验表明OPS氧化锆的抗老化性能也得到显著提高。

关键词: 振荡压力, 晶粒细化, 强度韧性, 致密度

Abstract:

To fulfill the demands of ceramic components with high strength, high toughness and high reliability in key projects, a novel oscillatory pressure sintering (OPS) method was proposed in this study. With this new method, zirconia ceramics with high relative density, fine grains, high fracture strength, and excellent reliability, were prepared. As a comparison, zirconia ceramics were sintered by pressure-less sintering (PS) method and hot pressing (HP) method at same temperature. SEM analysis shows that the oscillatory pressure inhibits the rapid grain growth of zirconia at high temperature. Statistic results indicate that the OPS zirconia presents fine grain size at 251 nm, while the average sizes of PS and HP zirconia are 451 and 298 nm, respectively. In addition, the oscillatory pressure induces plastic deformation of grains and sliding of grain boundaries, facilitating elimination of closed pores at grain boundaries. As a result, the relative density of OPS zirconia reaches approximately 99.7%. Due to the refinement of grains and the increase in relative density, the OPS zirconia presents an increase from 1003 MPa to 1572 MPa in flexural strength, and an increase from 13 to 32 in Weibull modulus. Furthermore, its resistance to low temperature degradation is also improved because of the microstructure evolution.

Key words: oscillatory pressure, grain refinement, strength and toughness, relative density

中图分类号:

TB332

李双, 谢志鹏. 振荡压力烧结法制备高致密度细晶粒氧化锆陶瓷[J]. 无机材料学报, 2016, 31(2): 207-212.

LI Shuang, XIE Zhi-Peng. Preparation of Zirconia Ceramics with High Density and Fine Grains by Oscillatory Pressure Sintering[J]. Journal of Inorganic Materials, 2016, 31(2): 207-212.

图/表 8

图1 氧化锆粉体的TEM照片

Fig. 1 TEM images of zirconia particles

图2 振荡压力耦合装置示意图(a)振荡压力耦合原理示意图(b)

Fig. 2 Schematic of the coupling apparatus for oscillatory pressure (a) and the coupling mechanism for oscillatory pressure (PT)

图3 氧化锆的显微结构照片

Fig. 3 Morphologies of zirconia ceramics (a) PS zirconia, fracture surface; (b) HP zirconia, fracture surface; (c) OPS zirconia, fracture surface; (d) OPS zirconia, polished surface

图4 不同烧结方法所制备氧化锆陶瓷的相对密度变化

Fig. 4 Variation of relative density of zirconia sintered by different methods

图5 不同烧结方法制备氧化锆的抗弯强度变化

Fig. 5 Variation of flexural strength of zirconia by different sintering methods

图6 不同烧结方法制备氧化锆的Weibull模数变化

Fig. 6 Variation of Weibull modulus of zirconia by different sintering methods

图7 HP氧化锆和OPS氧化锆的断裂强度随老化时间的变化

Fig. 7 Variation of flexural strength with increase of aging time of zirconia by different sintering methods

图8 恒定压力与振荡压力下陶瓷材料烧结路径示意图

Fig. 8 Schematic of sintering routes of ceramics under constant pressure and oscillatory pressure

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振荡压力烧结法制备高致密度细晶粒氧化锆陶瓷

Preparation of Zirconia Ceramics with High Density and Fine Grains by Oscillatory Pressure Sintering

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