Fe高温浸渗法制备防静电3Y-TZP陶瓷及其性能研究

doi:10.15541/jim20130690

摘要/Abstract

摘要：

以3Y-TZP陶瓷为基体, 采用还原Fe粉包埋、高温浸渗的表面改性方法, 制备防静电性能与力学性能兼备的ZrO₂陶瓷。研究了浸渗时间、浸渗温度对ZrO₂陶瓷表面电阻率及硬度的影响, 结果表明：随着浸渗时间延长, 浸渗温度升高, 表面电阻率降低, 硬度下降。在1000℃浸渗4 h, ZrO₂防静电陶瓷表面电阻率由10¹⁴?/□以上降低至8.3×10⁷?/□, 硬度由12.7 GPa降低至11.23 GPa。采用XRD、SEM、XPS等方法对防静电ZrO₂陶瓷的显微结构、化学组成及防静电机理进行了分析。结果表明, 浸渗过程中, 发生由t-ZrO₂转变为m-ZrO₂相变; Fe元素以Fe₃O₄、FeO、单质Fe的形式存在晶界处, 从而使ZrO₂陶瓷具备了防静电性能。

关键词: 氧化锆陶瓷, 防静电, 表面电阻率, 高温浸渗

Abstract:

Antistatic ceramic with good mechanical performance has wide application in fields of aerospace, petrochemical engineering, electronics and textile. Antistatic ceramic ZrO₂was fabricated via an innovative surface modification method based on embedding Fe-infiltration into the 3Y-TZP ceramic at high temperature, which showed good antistatic and mechanical properties. In addition, microstructure and morphology of as-prepared samples were characterized by XRD, SEM and XPS. Furthermore, the antistatic mechanism of ZrO₂ ceramics was investigated. The effects of infiltration temperature and infiltration time on vickers hardness and surface resistivity of specimen were evaluated. Experimental results showed that the surface resistivity and hardness decreased with the increase of infiltration temperature and infiltration time, in which the surface resistivity decreased from more than 10¹⁴?/□ to 8.3×10⁷?/□, and the hardness of ZrO₂ ceramics decreased from 12.7 GPa to 11.23 GPa after infiltration at 1000℃ for 4 h. Analysis results indicated that there was a phase transformation of ZrO₂ from t-ZrO₂ to m-ZrO₂ in the infiltration process. It was also found that Fe, Fe₃O₄and FeO located in the interface of infiltration layer, which were attributed to the antistatic property of ZrO₂ ceramics.

Key words: zirconia ceramics, antistatic, surface resistivity, high-temperature infiltration

中图分类号:

TQ174

李勇, 徐协文, 杨现锋, 谢志鹏. Fe高温浸渗法制备防静电3Y-TZP陶瓷及其性能研究[J]. 无机材料学报, 2014, 29(10): 1099-1104.

LI Yong, XU Xie-Wen, YANG Xian-Feng, XIE Zhi-Peng. Preparation of Antistatic Ceramics Employing Fe-infiltration in Sintered Zirconia Body[J]. Journal of Inorganic Materials, 2014, 29(10): 1099-1104.

图/表 10

图1 浸渗温度(a)与浸渗时间(b)对3Y-TZP陶瓷表面电阻率的影响

Fig. 1 Effect of infiltration temperature (a) and infiltration time (b) on surface resistivity of 3Y-TZP ceramics

图2 浸渗温度(a)与浸渗时间(b)对3Y-TZP陶瓷硬度的影响

Fig. 2 Effect of infiltration temperature (a) and infiltration time (b) on toughness of 3Y-TZP ceramics

图3 不同温度浸渗4 h(a)和1000℃浸渗不同时间(b)处理前后的3Y-TZP陶瓷的XRD图谱

Fig. 3 XRD patterns of 3Y-TZP ceramic infiltrated at different temperatures for 4 h (a) and at 1000℃ for different time (b)

图4 处理前(a)和1000℃浸渗处理4 h后(b)的 3Y-TZP陶瓷横断面的SEM照片

Fig. 4 SEM images of 3Y-TZP ceramics before (a) and after (b)infiltrating at 1000℃ for 4 h

图5 防静电3Y-TZP陶瓷SEM照片及对应区域EDS分析

Fig. 5 SEM images of antistatic 3Y-TZP ceramics and corresponding EDS analyses of marked areas

图6 3Y-TZP陶瓷浸渗处理前后O1s、Zr3d、Y3d的XPS图谱

Fig. 6 XPS spectra of O, Zr and Y for 3Y-TZP ceramics before and after infiltrating at 1000℃ for 4 h

图7 3Y-TZP陶瓷处理前后XPS全谱图

Fig. 7 XPS wide spectra of 3Y-TZP ceramic before and after infiltration

图8 Fe2p XPS图谱

Fig. 8 XPS spectra of Fe2p

图9 防静电3Y-TZP陶瓷铁包覆层的XRD图谱

Fig. 9 XRD pattern of the iron layer coating on antistatic 3Y-TZP ceramics

表1 XPSFe峰位置及峰面积

Table 1 Peak position and relative area of Fe XPS spectra

Iron states	Peak position/eV				Area/%
Iron states	Fe2p_1/2	Satellite		Fe2p_3/2	Area/%
Fe	720.5	729.6	715.0	707.0	8.37
FeO	722.6			709.0	40.42
Fe₃O₄	724.0			710.6	51.21

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