预氧化处理对G115钢高温蒸气氧化行为的影响

doi:10.11900/0412.1961.2017.00377

金属学报

2018, Vol. 54

Issue (6): 895-904 DOI: 10.11900/0412.1961.2017.00377

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预氧化处理对G115钢高温蒸气氧化行为的影响

白银^1,², 刘正东¹(

), 谢建新², 包汉生¹, 陈正宗¹

1 钢铁研究总院北京 1000812 北京科技大学材料科学与工程学院北京 100083

Effect of Pre-Oxidation Treatment on the Behavior of High Temperature Oxidation in Steam of G115 Steel

Yin BAI^1,², Zhengdong LIU¹(

), Jianxin XIE², Hansheng BAO¹, Zhengzong CHEN¹

1 Central Iron and Steel Research Institute, Beijing 100081, China
2 School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083, China

引用本文:

白银, 刘正东, 谢建新, 包汉生, 陈正宗. 预氧化处理对G115钢高温蒸气氧化行为的影响[J]. 金属学报, 2018, 54(6): 895-904.
Yin BAI, Zhengdong LIU, Jianxin XIE, Hansheng BAO, Zhengzong CHEN. Effect of Pre-Oxidation Treatment on the Behavior of High Temperature Oxidation in Steam of G115 Steel[J]. Acta Metall Sin, 2018, 54(6): 895-904.

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摘要:

以Ar气为保护环境,对G115马氏体耐热钢进行了预氧化处理。通过循环蒸气氧化实验,研究了未预氧化处理和预氧化处理2种试样在650 ℃水蒸气中的高温氧化行为。采用分析天平测量氧化增重,得到了氧化增重动力学曲线。通过SEM及附带的EDS分析了氧化皮的形貌和结构,采用XRD结合EDS对氧化产物进行了相鉴定。实验结果表明,预氧化处理明显降低G115钢1800 h以内的氧化增重。预氧化处理后,G115钢的蒸气氧化动力学由立方型转变为直线型,氧化皮结构由典型的双层结构转变为多层结构。预氧化处理试样的氧化皮最外层为由Fe向外扩散形成的富Fe层,中层为Cr含量达46% (质量分数)的富Cr层,最内层由金属基体转变而成。其中氧化皮中层由于Cr含量高而具有良好的保护性,是整体氧化过程的控制步骤。另外该层厚度接近常数,使得预氧化处理试样的氧化动力学呈直线型。以氧化皮结构和氧化过程机制为根据,对预氧化处理的长期效果进行了评估。

关键词 ：耐热钢, 高温氧化, 氧化动力学, 预氧化

Abstract：

In order to improve the steam oxidation resistance of G115 steel (9Cr3W3CoVNbCuBN) at 650 ℃, pre-oxidation treatment was carried out in argon environment with low oxygen partial pressure. The oxidation behaviors of the pre-oxidized and untreated samples were simultaneously investigated by a cyclic oxidation experiment. Weight gains of samples were measured by analytical balance, phases of oxide products were identified by XRD and EDS, morphology and structure of scales were characterized by SEM and EDS. The result showed that pre-oxidation treatment significantly decrease oxidation weight gains in 1800 h. After pre-oxidation treatment, the oxidation kinetics transformed from cubic into linear form, and the scale structures transformed from duplex layers into triple layers. In the scale of pre-oxidized samples, the outermost layer was enriched in Fe, the middle layer was enriched in Cr, and the innermost layer was transformed from the matrix metal. The middle layer had chromium content as high as 46% (mass fraction) and was considered to be conformed of chromite (FeCr₂O₄). This layer was the most protective layer due to its highest Cr content, and the diffusion of O and Fe though it was the main controlling process of the whole oxidation. It suggested that the stable structure of the middle layer improved the oxidation resistance of pre-oxidation samples. The thickness of the middle layer nearly kept constant during the whole oxidation process, which was the main reason why the pre-oxidized sample had linear oxidation kinetics. The long term effect of the pre-oxidation treatment was evaluated based on the scale structure and oxidation mechanism.

Key words： heat-resistant steel high temperature oxidation oxidation kinetics pre-oxidation

收稿日期: 2017-09-08

ZTFLH:

TG172.5

基金资助:国家重点研发计划项目No.2017YFB0305200

作者简介:

作者简介白银,男,1987年生,博士生

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https://www.ams.org.cn/CN/10.11900/0412.1961.2017.00377 或 https://www.ams.org.cn/CN/Y2018/V54/I6/895

图1 高温蒸气氧化实验平台示意图

图2 未预氧化处理和预氧化处理的G115试样650 ℃蒸气氧化后增重与时间的关系

图3 未预氧化处理试样在650 ℃蒸气氧化100和800 h后表层氧化物形貌的SEM像

图4 未预氧化试样在蒸气中氧化200 h后表层氧化物的XRD谱

图5 预氧化后试样的表层氧化物形貌的SEM像、XRD谱和EDS分析

图6 预氧化处理试样在650 ℃水蒸气中氧化不同时间后表层形貌的SEM像

图7 图6a中底层氧化物和晶须顶端组织及图6b中晶须处的EDS分析结果

图8 未预氧化试样蒸气氧化400 h后截面形貌的SEM像

图9 经Ar气预氧化的G115钢试样在650 ℃水蒸气中氧化后氧化层截面形貌的SEM像

图10 预氧化处理试样氧化400 h后氧化皮内元素分布图

图11 预氧化试样氧化皮中层厚度与氧化时间的关系

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