阶段占空比对ZrH1.8表面微弧氧化陶瓷层性能的影响

doi:10.15541/jim20190578

无机材料学报 ›› 2020, Vol. 35 ›› Issue (10): 1112-1116.DOI: 10.15541/jim20190578 CSTR: 32189.14.10.15541/jim20190578

所属专题：结构陶瓷论文精选(2020)

阶段占空比对ZrH_1.8表面微弧氧化陶瓷层性能的影响

杨少辉¹(),闫淑芳^1,²(),李世江¹,陈伟东^1,²,杜培¹,马文^1,²

内蒙古工业大学 1. 材料科学与工程学院
^2. 内蒙古自治区薄膜与涂层重点实验室, 呼和浩特 010051

收稿日期:2019-11-14 修回日期:2019-12-26 出版日期:2020-10-20 网络出版日期:2020-01-20
作者简介:杨少辉(1996-), 男, 硕士研究生. E-mail:18447071525@163.com
基金资助:
国家自然科学基金(51964035);内蒙古自然科学基金(2019MS05020)

Effect of Phase Duty Cycle on the Properties of ZrH_1.8 Surface Micro-arc Oxidized Ceramic Layer

YANG Shaohui¹(),YAN Shufang^1,²(),LI Shijiang¹,CHEN Weidong^1,²,DU Pei¹,MA Wen^1,²

^1. College of Materials Science and Engineering, Inner Mongolia University of Technology, Hohhot 010051, China
^2. Inner Mongolia Key Laboratory of Thin Film and Coatings, Inner Mongolia University of Technology, Hohhot 010051, China

Received:2019-11-14 Revised:2019-12-26 Published:2020-10-20 Online:2020-01-20
About author:YANG Shaohui (1996-) male, Master candidate. E-mail:18447071525@163.com
Supported by:
National Natural Science Foundation of China(51964035);Natural Science Foundation of Inner Mongolia Autono mous Region(2019MS05020)

摘要/Abstract

摘要：

为了提高氢化锆表面微弧氧化陶瓷层的致密性及阻氢性能, 采用恒压模式对氢化锆基体进行微弧氧化处理, 在磷酸盐电解液体系下, 研究阶段占空比分别为40%-50%-60%、50%-60%-40%和60%-50%-40%三种情况下陶瓷层的生长过程。利用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、膜层测厚仪分析陶瓷层的形貌、相结构及厚度; 通过真空脱氢实验评价不同阶段占空比模式下获得陶瓷层的阻氢性能。研究结果表明: 不同阶段占空比模式下在ZrH_1.8表面可制得厚度分别为162.6、175.9、158.7 μm的氧化锆陶瓷层, 且所制微弧氧化陶瓷层均由M-ZrO₂、T-ZrO₂以及Zr_0.95Ce_0.05O₂三种物相组成, 阶段占空比对陶瓷层物相组成无显著影响; 阶段占空比为40%-50%-60%条件下, 氢化锆表面所制陶瓷层厚度达到162.6 μm, 氢渗透降低因子(Permeation Reduction Factor, PRF)达到12.5, 阻氢性能较佳。

关键词: 微弧氧化, 氢化锆, 占空比, 陶瓷层

Abstract:

To study the respective growths of micro-arc oxidation (MAO) ceramic coatings under three phase duty cycles of 40%-50%-60%, 50%-60%-40%, and 60%-50%-40%, and to thereby improve the compactness and hydrogen permeation resistance of the MAO ceramic coatings on the surface of zirconium hydride, the zirconium hydride matrix went through MAO treatment under constant voltage in the phosphate electrolyte system. On the one hand, the morphology, phase structure, and thickness of the ceramic coatings were analyzed by using scanning electron microscope (SEM), X-ray diffractometer (XRD), and film thickness meter. On the other hand, the hydrogen permeation resistance of the ceramic coatings under the different phase duty cycle was obtained through a vacuum dehydrogenation experiment. The research results indicate that under three phase duty cycle, the accumulated thickness of zirconium oxide ceramic coatings on the surface of ZrH_1.8 are 162.6, 175.9, and 158.7 μm, respectively; all of the produced MAO ceramic coatings consist of three phases, namely M-ZrO₂, T-ZrO₂, and Zr_0.95Ce_0.05O₂. Phase duty cycle has no significant effect on the phase composition of ceramic coatings. Under the phase duty cycle of 40%-50%-60%, the ceramic coating achieves on the surface of zirconium hydride has the thickness of 162.6 μm and the Permeation Reduction Factor (PRF) value of 12.5, indicating a relatively satisfactory hydrogen permeation resistance.

Key words: micro-arc oxidation, zirconium hydride, duty cycle, ceramic layer

中图分类号:

TQ174

杨少辉, 闫淑芳, 李世江, 陈伟东, 杜培, 马文. 阶段占空比对ZrH_1.8表面微弧氧化陶瓷层性能的影响[J]. 无机材料学报, 2020, 35(10): 1112-1116.

YANG Shaohui, YAN Shufang, LI Shijiang, CHEN Weidong, DU Pei, MA Wen. Effect of Phase Duty Cycle on the Properties of ZrH_1.8 Surface Micro-arc Oxidized Ceramic Layer[J]. Journal of Inorganic Materials, 2020, 35(10): 1112-1116.

图/表 6

表1 微弧氧化实验电参数

Table 1 Electrical parameters of micro-arc oxidation

No.	Anode voltage/V	Cathode voltage/V	Frequency/ Hz	Duty cycle
Ⅰ	350	120	100	40%-50%-60%
Ⅱ	350	120	100	50%-60%-40%
Ⅲ	350	120	100	60%-50%-40%

图1 不同阶段占空比模式下正向电流(a)与正向电阻(b)随时间的变化曲线

Fig. 1 Forward current (a) and forward resistance (b) changed with time under different phase duty cycle modes

图2 不同阶段占空比模式下ZrH1.8微弧氧化陶瓷层表面SEM照片

Fig. 2 Micromorphology of ZrH1.8 micro-arc oxidation ceramic layer under different phase duty cycles (a) 40%-50%-60%; (b) 50%-60%-40%; (c) 60%-50%-40%

图3 不同阶段占空比模式下ZrH1.8微弧氧化陶瓷层截面SEM照片

Fig. 3 Cross-micromorphology of ZrH1.8 micro-arc oxidation ceramic layers under different phase duty cycle modes (a) 40%-50%-60%; (b) 50%-60%-40%; (c) 60%-50%-40%

图4 不同阶段占空比模式下ZrH1.8表面陶瓷层的相结构

Fig. 4 XRD patterns of ZrH1.8 surface ceramic layers under different phase duty cycle modes

表2 不同阶段占空比条件下微弧氧化陶瓷层厚度及氢渗透降低因子

Table 2 Thicknesses and permeation reduction factors of micro-arcoxidation ceramic layers under different phase duty cycle modes

No.	Duty cycle/%	Thickness /μm	H_PRF
Ⅰ	40%-50%-60%	162.6	12.5
Ⅱ	50%-60%-40%	175.9	7.1
Ⅲ	60%-50%-40%	158.7	10.5

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阶段占空比对ZrH_1.8表面微弧氧化陶瓷层性能的影响

Effect of Phase Duty Cycle on the Properties of ZrH_1.8 Surface Micro-arc Oxidized Ceramic Layer

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阶段占空比对ZrH1.8表面微弧氧化陶瓷层性能的影响

Effect of Phase Duty Cycle on the Properties of ZrH1.8 Surface Micro-arc Oxidized Ceramic Layer

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阶段占空比对ZrH_1.8表面微弧氧化陶瓷层性能的影响

Effect of Phase Duty Cycle on the Properties of ZrH_1.8 Surface Micro-arc Oxidized Ceramic Layer