铝酸盐体系下反应时间对ZrH1.8表面阻氢膜层制备的影响

doi:10.15541/jim20170179

无机材料学报 ›› 2018, Vol. 33 ›› Issue (3): 284-288.DOI: 10.15541/jim20170179

铝酸盐体系下反应时间对ZrH_1.8表面阻氢膜层制备的影响

张鹏飞^{1, 2}, 闫淑芳¹, 陈伟东¹, 李世江¹, 赵丽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:2017-04-17 修回日期:2017-06-06 出版日期:2018-03-20 网络出版日期:2018-03-12
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)

Influence of Reaction Time on Hydrogen Resistance Film on the Surface of ZrH_1.8 in Aluminate System

ZHANG Peng-Fei^{1, 2}, YAN Shu-Fang¹, CHEN Wei-Dong¹, LI Shi-Jiang¹, ZHAO Li¹, 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:2017-04-17 Revised:2017-06-06 Published:2018-03-20 Online:2018-03-12
About author:ZHANG Peng-Fei. E-mail: pfzhang.kk@foxmail.com
Supported by:
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)

摘要/Abstract

摘要：

采用微弧氧化技术在NaAlO₂电解液体系下制备ZrH_1.8表面阻氢膜层, 采用场发射扫描电子显微镜(FE-SEM), X射线衍射(XRD), 真空脱氢实验对膜层进行表征, 考察不同反应时间对ZrH_1.8表面阻氢膜层的厚度、形貌、相结构以及阻氢性能的影响规律。研究结果表明：当反应时间在7.5~15 min变化时, 膜层厚度由78.4 μm增大至152.8 μm。膜层由单斜相M-ZrO₂、四方相T-ZrO₂以及立方相C-ZrO₂组成, 反应时间对膜层的相组成并无明显影响。阻氢膜层由致密层和疏松层构成, 膜层外侧为疏松层, 靠近基体一侧为致密层。当反应时间为10 min时, 获得的膜层表面平整, 致密性较好, 厚度适中, 膜层的氢渗透降低因子PRF值为20。

关键词: ZrH_1.8, 微弧氧化技术, 反应时间, 氧化膜

Abstract:

Micro-arc oxidation process was conducted on ZrH_1.8 in the electrolyte composed of NaAlO₂ to fabricate hydrogen resistance film. The as-prepared film was then characterized by field emission scanning electron microscope (FE-SEM), X-ray diffraction (XRD), and vacuum dehydrogenation experiment. The influences of reaction time on thickness, micro-morphology, structure, and hydrogen resistance properties of the hydrogen resistance film on the surface of ZrH_1.8 were investigated. The results show that the thickness of the surface film increases from 78.4 μm to 152.8 μm with the oxidation time changing from 7.5 min to 15 min. The film is composed of M-ZrO₂, T-ZrO₂ and C-ZrO₂, and the oxidation time has no obvious influence on its structure. The film comprises of an exterior loose layer and an interior layer by substrate. When the oxidation time is 10 min, the obtained film is compact and uniform, and has a moderate thickness, showing an excellent hydrogen permeation resistance, of which the Permeation Reduction Factor (PRF) value reaches up to the maximum of 20.

Key words: zirconium hydride, micro-arc oxidation technology, reaction time, oxide film

中图分类号:

TQ174

张鹏飞, 闫淑芳, 陈伟东, 李世江, 赵丽, 王宏兴. 铝酸盐体系下反应时间对ZrH_1.8表面阻氢膜层制备的影响[J]. 无机材料学报, 2018, 33(3): 284-288.

ZHANG Peng-Fei, YAN Shu-Fang, CHEN Wei-Dong, LI Shi-Jiang, ZHAO Li, WANG Hong-Xing. Influence of Reaction Time on Hydrogen Resistance Film on the Surface of ZrH_1.8 in Aluminate System[J]. Journal of Inorganic Materials, 2018, 33(3): 284-288.

图/表 6

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/(g•L^-1)
1	7.5	375	120	NaAlO₂(18) NaOH (1.5) Na₂EDTA (2)
2	10.0
3	12.5
4	15.0

图1 不同反应时间下膜层的表面形貌

Fig. 1 Surface morphologies of the films prepared with different reaction time(a) 7.5 min; (b) 10 min; (c) 12.5 min; (d) 15 min

图2 不同反应时间下膜层的截面形貌

Fig. 2 Cross-section morphologies of the films prepared with different reaction time(a) 7.5 min; (b) 10 min; (c) 12.5 min; (d) 15 min

图3 反应时间对微弧氧化膜层的厚度和生长速率的影响

Fig. 3 Effects of reaction time on the thickness and growth rate of micro-arc oxidation coating

图4 不同反应时间下氧化膜层的XRD图谱

Fig. 4 XRD patterns of the oxide films under different reaction time

图5 氧化膜层氢渗透降低因子与反应时间关系

Fig. 5 Relationship between permeation reduction factor of oxide films and reaction time

参考文献 21

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铝酸盐体系下反应时间对ZrH_1.8表面阻氢膜层制备的影响

Influence of Reaction Time on Hydrogen Resistance Film on the Surface of ZrH_1.8 in Aluminate System

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铝酸盐体系下反应时间对ZrH1.8表面阻氢膜层制备的影响

Influence of Reaction Time on Hydrogen Resistance Film on the Surface of ZrH1.8 in Aluminate System

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铝酸盐体系下反应时间对ZrH_1.8表面阻氢膜层制备的影响

Influence of Reaction Time on Hydrogen Resistance Film on the Surface of ZrH_1.8 in Aluminate System