石墨烯浓度对ZrH1.8表面微弧氧化陶瓷层的影响

doi:10.15541/jim20190037

摘要/Abstract

摘要：

在Na₅P₃O₁₀-KOH-Na₂EDTA电解液中, 以石墨烯为添加剂, 在恒压模式下对ZrH_1.8表面进行微弧氧化处理。采用涂层划痕仪测试陶瓷层与基体的结合力, 通过真空脱氢实验来评价陶瓷层的阻氢性能。电解液中添加石墨烯后, ZrH_1.8表面微弧氧化陶瓷层均由内层致密层和外层疏松层构成, XRD图谱显示, 所制陶瓷层主要由M-ZrO₂和T-ZrO₂相组成。随着石墨烯浓度的增加, 陶瓷层的氢渗透降低因子(Permeation Reduction Factor, PRF)呈先增大后减小的趋势。当石墨烯浓度为0.10 g/L时, 陶瓷层的厚度约为66.5 μm, 表面孔洞和裂纹较少, 陶瓷层较致密, PRF值为13.2, 阻氢性能较好。

关键词: 氢化锆, 微弧氧化, 石墨烯, 陶瓷层, 阻氢性能

Abstract:

The surface of ZrH_1.8 was subjected to micro-arc oxidation treatment in a constant pressure mode using graphene as an additive in Na₅P₃O₁₀-KOH-Na₂EDTA electrolyte. Adhesion of the ceramic layer to the substrate was tested using a coating scratch tester. Hydrogen barrier property of the ceramic layer were evaluated by vacuum dehydrogenation experiments. After adding graphene to the electrolyte, the micro-arc oxidation ceramic layer on the ZrH_1.8 surface is composed of an inner dense layer and a loose outer layer. XRD pattern shows that the ceramic layer is mainly composed of M-ZrO₂ and T-ZrO₂ phases. As the concentration of graphene increases, the permeation reduction factor (PRF) of the ceramic layer increases firstly and then decreases. When the concentration of graphene is 0.10 g/L, the thickness of the ceramic layer is about 66.5 μm, with less surface pores and cracks, denser ceramic layer, PRF at 13.2, and better hydrogen barrier performance.

Key words: zirconium hydride, micro-arc oxidation, graphene, ceramic layer, hydrogen barrier performance

中图分类号:

TG174

杜培, 闫淑芳, 陈伟东, 李世江, 马文. 石墨烯浓度对ZrH_1.8表面微弧氧化陶瓷层的影响[J]. 无机材料学报, 2019, 34(11): 1175-1180.

DU Pei, YAN Shu-Fang, CHEN Wei-Dong, LI Shi-Jiang, MA Wen. Graphene Concentration on Micro-arc Oxidation Ceramic Layer of ZrH_1.8 Surface[J]. Journal of Inorganic Materials, 2019, 34(11): 1175-1180.

图/表 8

表1 电解液组成及微弧氧化实验参数

Table 1 Electrolyte composition and micro-arc oxidation experimental parameters

Graphene concentration/(g·L^-1)	Anode voltage/V	Cathode voltage/V	Frequency/Hz	Duty cycle	Time/min	Electrolyte composition
0	430	150	150	50	15	Na₅P₃O₁₀ KOH Na₂EDTA
0.05
0.10
0.15
0.20

图1 不同石墨烯浓度时微弧氧化陶瓷层的表面形貌

Fig. 1 Surface morphologies of micro-arc oxidation ceramic layer at different graphene concentrations (a) Without graphene; (b) 0.05 g/L; (c) 0.10 g/L; (d) 0.15 g/L; (e) 0.20 g/L

图2 不同石墨烯浓度时微弧氧化陶瓷层的截面形貌

Fig. 2 Cross-section morphologies of micro-arc oxidation ceramic layer at different graphene concentrations (a) Without graphene; (b) 0.05 g/L; (c) 0.10 g/L; (d) 0.15 g/L; (e) 0.20 g/L

图3 不同石墨烯浓度时微弧氧化陶瓷层的XRD图谱

Fig. 3 XRD patterns of micro-arc oxidation ceramic layer at different graphene concentrations (a) Without graphene; (b) 0.05 g/L; (c) 0.10 g/L; (d) 0.15 g/L; (e) 0.20 g/L

图4 不同石墨烯浓度时微弧氧化陶瓷层的XPS图谱

Fig. 4 XPS spectra of micro-arc oxidation ceramic layer at different graphene concentrations (a) Without graphene; (b) 0.10 g/L

图5 图4(b)中检测到的元素的XPS高分辨率光谱

Fig. 5 XPS high resolution spectra of elements detected in Fig. 4(b) (a) C; (b) O; (c) Zr

图6 不同石墨烯浓度时微弧氧化陶瓷层与ZrH1.8基体的结合力

Fig. 6 Bonding force between micro-arc oxidation ceramic layer and ZrH1.8 matrix at different graphene concentrations

图7 不同石墨烯浓度时微弧氧化陶瓷层的PRF值

Fig. 7 PRF value of micro-arc oxidation ceramic layer at different graphene concentrations

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