Zr-2合金表面ZrO2/Cr复合膜的高温蒸汽氧化行为

doi:10.11901/1005.3093.2022.633

材料研究学报

2023, Vol. 37

Issue (10): 759-769 DOI: 10.11901/1005.3093.2022.633

研究论文

本期目录 | 过刊浏览

Zr-2合金表面ZrO₂/Cr复合膜的高温蒸汽氧化行为

王兴平¹^,²(

), 薛文斌², 王文选³

^1.兰州交通大学材料科学与工程学院兰州 730070
^2.北京师范大学核科学与技术学院射线束技术教育部重点实验室北京 100875
^3.兰州交通大学机电工程学院兰州 730070

High Temperature Steam Oxidation Behavior of Zr-2 Alloy with ZrO₂/Cr Composite Coating

WANG Xingping¹^,²(

), XUE Wenbin², WANG Wenxuan³

^1.School of Materials Science and Engineering, Lanzhou Jiaotong University, Lanzhou 730070, China
^2.Key Laboratory of Beam Technology of Ministry of Education, College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875, China
^3.School of Mechanical Engineering, Lanzhou Jiaotong University, Lanzhou 730070, China

引用本文:

王兴平, 薛文斌, 王文选. Zr-2合金表面ZrO₂/Cr复合膜的高温蒸汽氧化行为[J]. 材料研究学报, 2023, 37(10): 759-769.
Xingping WANG, Wenbin XUE, Wenxuan WANG. High Temperature Steam Oxidation Behavior of Zr-2 Alloy with ZrO₂/Cr Composite Coating[J]. Chinese Journal of Materials Research, 2023, 37(10): 759-769.

全文: PDF(15803 KB) HTML

摘要:

用微弧氧化(MAO)和磁过滤阴极真空弧离子镀(FCVAD)在Zr-2合金表面制备ZrO₂/Cr复合膜，用热重分析仪(TGA)评估了Zr-2合金基体和ZrO₂/Cr复合膜在900~1100℃蒸汽环境中的抗氧化性能，并分析其氧化后氧化层的截面结构、相组成和成分深度分布。结果表明，在900、1000和1100℃蒸汽环境中分别氧化3600 s后，ZrO₂/Cr复合膜试样单位面积增重约为Zr-2合金基体的3/8、1/4和2/5。在高温蒸汽环境中，ZrO₂/Cr复合膜表面氧化生成的致密Cr₂O₃膜能抑制氧向内扩散，提高锆合金的抗蒸汽氧化性能，阻止锆试样在1000℃蒸汽环境中出现分离氧化。ZrO₂/Cr复合膜的表面Cr层完全消耗前，Cr涂层的氧化主要取决于铬向外扩散，而不是氧向内扩散。在蒸汽氧化过程中，MAO膜的中间层能抑制氢渗透进入锆合金基体。

关键词 ：金属材料, Zr-2合金, ZrO₂/Cr复合膜, 高温蒸汽氧化, 氧化动力学, 分离氧化

Abstract：

A ZrO₂/Cr composite coating on Zr-2 alloy was prepared by micro-arc oxidation (MAO) and filtered cathodic vacuum arc deposition (FCVAD) treatments. The oxidation resistance of bare and ZrO₂/Cr-coated Zr alloys was estimated in 900~1100°C steam environment using a thermogravimetric analyzer (TGA) and their cross-sectional structures, phase constituents and composition depth profiles before and after steam oxidation were analyzed. The results showed that the mass gain per unit area of ZrO₂/Cr-coated Zr alloy was about 3/8, 1/4 and 2/5 of that of bare Zr alloy after 3600 s steam oxidation at 900, 1000 and 1100℃, respectively. In high temperature water vapor, the dense Cr₂O₃ film formed on the surface of ZrO₂/Cr-coated one suppressed the inward oxygen diffusion, which improved the steam oxidation resistance of Zr-2 alloy and inhibited the occurrence of breakaway oxidation at 1000°C. Before the Cr layer of ZrO₂/Cr composite coating was completely oxidized into Cr₂O₃, the oxidation of Cr layer was principally controlled by the outward chromium diffusion rather than inward oxygen diffusion. The MAO interlayer restrained hydrogen permeation into Zr alloy substrate during the steam oxidation.

Key words： metallic materials Zr-2 alloy ZrO₂/Cr composite coating high-temperature steam oxidation oxidation kinetics breakaway

收稿日期: 2022-11-28

ZTFLH:

TG174.442

基金资助:北京市自然科学基金(2172029);国家自然科学基金(51671032);甘肃省科技计划(20JR10RA269);甘肃省教育厅创新基金(2021B-099);兰州交通大学青年基金(2023002)

通讯作者: 王兴平，wangxplju@163.com，研究方向为金属表面处理

Corresponding author: WANG Xingping, Tel: 18298491716, E-mail: wangxplju@163.com

作者简介: 王兴平，男，1992年生，博士

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图1 Zr-2合金表面微弧氧化膜的形貌、结构和相组成

图2 Zr-2合金表面ZrO2/Cr复合膜的结构、成分和相组成

图3 Zr-2合金及ZrO2/Cr复合膜在不同温度蒸汽中的氧化动力学曲线

表1 Zr-2合金及ZrO2/Cr复合膜在不同温度蒸汽中氧化动力学参数

图4 Zr-2合金在不同温度蒸汽中氧化3600 s后截面的结构和GDOES成分深度分布

图5 ZrO2/Cr复合膜在不同温度蒸汽中氧化3600 s后的截面结构和GDOES成分深度分布

表2 ZrO2/Cr复合膜试样1100℃蒸汽氧化3600 s后的截面成分

图6 Zr-2合金和ZrO2/Cr复合膜在不同温度蒸汽中氧化3600 s后截面的金相组织

图7 Zr-2合金和ZrO2/Cr复合膜在不同温度的蒸汽中氧化3600 s后的XRD谱

图8 扩散系数与温度的关系

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