正向电压对氢化锆微弧氧化阻氢膜层性能的影响

doi:10.15541/jim20170328

无机材料学报 ›› 2018, Vol. 33 ›› Issue (7): 793-797.DOI: 10.15541/jim20170328 CSTR: 32189.14.10.15541/jim20170328

正向电压对氢化锆微弧氧化阻氢膜层性能的影响

张鹏飞^1,2, 闫淑芳¹, 陈伟东¹, 李世江¹, 耿艳花¹, 王宏兴²

1. 内蒙古工业大学材料科学与工程学院, 呼和浩特 010051;
2. 西安交通大学宽禁带半导体材料与器件研究中心, 西安 710049

收稿日期:2017-07-05 修回日期:2017-09-06 出版日期:2018-07-10 网络出版日期:2018-06-19
作者简介:张鹏飞(1992-), 男, 硕士研究生. E-mail: pfzhang.kk@foxmail.com
基金资助:
国家自然科学基金(51164023, 51364026);内蒙古自然科学基金(2016MS0505);内蒙古工业大学科学研究项目(X201410);National Natural Science Foundation of China (51164023, 51364026);Natural Science Foundation of Inner Mongolia Autonomous Region (2016MS0505);Science Project of Inner Mongolia University of Technology (X201410)

Anode Voltage on Hydrogen Permeation Barrier Performance of Zirconium Hydride with Micro-arc Oxidation

ZHANG Peng-Fei^1,2, YAN Shu-Fang¹, CHEN Wei-Dong¹, LI Shi-Jiang¹, GENG Yan-Hua¹, Wang Hong-Xing²

1. College of Materials Science and Engineering, Inner Mongolia University of Technology, Hohhot 010051, China;
2. Institute of Wide Band Gap Semiconductors, Xi'an Jiaotong University, Xi'an 710049, China

Received:2017-07-05 Revised:2017-09-06 Published:2018-07-10 Online:2018-06-19
About author:ZHANG Peng-Fei. E-mail: pfzhang.kk@foxmail.com

摘要/Abstract

摘要：

在偏铝酸钠-氢氧化钠-EDTA混合溶液中, 采用恒压模式对氢化锆表面进行微弧氧化处理。借助场发射扫描电镜(FE-SEM)、X射线衍射仪(XRD)及真空脱氢实验, 研究了不同正向电压(350~425 V)对微弧氧化膜层表面、截面、相结构及阻氢渗透性能的影响。分析结果表明: 微弧氧化过程大致由阳极氧化、火花放电、微弧氧化和熄弧四个阶段组成。制备的膜层分为致密层和疏松层, 致密层所占比例约为80%。随着正向电压的增大, 晶粒尺寸增大, 晶面间距减小, 氢化锆表面微弧氧化膜层厚度由122 μm增加至150 μm, 膜层的增长速度也随正向电压的增大而加快。但正向电压的改变对膜层的相结构并无显著影响, 膜层由单斜相氧化锆和四方相氧化锆组成, 当正向氧化电压为400 V时, 氧化膜的PRF值达到最大值20。

关键词: 氢化锆, 微弧氧化, 正向电压, 阻氢渗透层

Abstract:

Technology of micro-arc oxidation was applied on ZrH_1.8in the electrolyte composed of NaAlO₂+NaOH+ Na₂EDTA in constant voltage mode. The film was characterized by field emission scanning electron microscope (FE-SEM), X-ray diffraction (XRD), and vacuum dehydrogenation experiment, respectively. The influences of anode voltage (350 to 425 V) on surface and cross-sectional morphology, structure, and hydrogen resistance properties of the hydrogen resistance film on the surface of ZrH_1.8 were investigated. The micro-arc oxidation process can be divided into four stages: anodic oxidation, spark discharge, micro-arc oxidation and flameout. The results reveal that film obtained in the electrolyte is composed of inner dense layer and outer loose layer, and proportion of the dense layer is about 80%. Grain sizes and growth rate of the film increase while the d-spacing decreases with the increase of the anode voltage, and the thickness of the film is increased from 122 to 150 μm. However, anode voltage has no obvious influence on the structure of the film. The prepared film is composed of M-ZrO₂ and T-ZrO₂. When the anode voltage is 400 V, the permeation reduction factor value reaches the maximum of 20.

Key words: zirconium hydride, micro-arc oxidation, anode voltage, hydrogen permeation barrier

中图分类号:

TQ174

张鹏飞, 闫淑芳, 陈伟东, 李世江, 耿艳花, 王宏兴. 正向电压对氢化锆微弧氧化阻氢膜层性能的影响[J]. 无机材料学报, 2018, 33(7): 793-797.

ZHANG Peng-Fei, YAN Shu-Fang, CHEN Wei-Dong, LI Shi-Jiang, GENG Yan-Hua, Wang Hong-Xing. Anode Voltage on Hydrogen Permeation Barrier Performance of Zirconium Hydride with Micro-arc Oxidation[J]. Journal of Inorganic Materials, 2018, 33(7): 793-797.

图/表 7

表1 微弧氧化实验参数

Table 1 Experimental parameters of micro-arc oxidation

No.	Time/min	Anode voltage/V	Cathode voltage/V	Electrolyte composition
1	10	350	120	NaAlO₂ NaOH Na₂EDTA
2		375
3		400
4		425

图1 铝酸盐体系下MAO过程中正向电流随反应时间变化的曲线

Fig. 1 Anodic current-time responses during MAO process in NaAlO2 electrolyte

图 2 不同正向电压制备得到的氢化锆 MAO 膜层的 XRD图谱

Fig. 2 XRD patterns of the MAO coatings on the surface of ZrH1.8 prepared at different anode voltages

表2 不同正向电压下氢化锆MAO膜层的晶粒尺寸和晶面间距

Table 2 Grain size and d-spacing of MAO coatings on the surface of ZrH1.8 prepared at different anode voltages

Voltage/V	2θ/(°)	d-spacing/nm	FWHM/(°)	Grain size/nm
350	30.194	0.29575	0.314	27.7
375	30.214	0.29556	0.293	29.9
400	30.293	0.29480	0.286	30.8
425	30.332	0.29443	0.262	34.4

图3 不同正向电压下制备的膜层的表面SEM照片

Fig. 3 Surface morphologies of oxide films prepared at different anode voltages(a) 350 V; (b) 375 V; (c) 400 V; (d) 425 V

图4 不同正向电压下制备得到的膜层的截面形貌

Fig. 4 Cross-section morphologies of oxide films prepared at different anode voltages(a) 350 V; (b) 375 V; (c) 400 V; (d) 425 V and magnified image of selected area in (a) (e)

图5 不同正向电压下制备得到的膜层厚度、生长速率及氢渗透降低因子变化关系

Fig. 5 Thickness, growth rate and permeation reduction factor of oxide films prepared at different anode voltages

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正向电压对氢化锆微弧氧化阻氢膜层性能的影响

Anode Voltage on Hydrogen Permeation Barrier Performance of Zirconium Hydride with Micro-arc Oxidation

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