聚变用低活化<strong>9Cr-ODS</strong>钢在高温高压水中的腐蚀行为及机理

doi:10.11900/0412.1961.2023.00465

金属学报

2025, Vol. 61

Issue (9): 1305-1319 DOI: 10.11900/0412.1961.2023.00465

研究论文

本期目录 | 过刊浏览

聚变用低活化9Cr-ODS钢在高温高压水中的腐蚀行为及机理

付海阳¹^,², 张家榕¹^,³(

), 李尧志¹^,², 王旗涛¹^,², 李新乐¹^,², 严伟¹^,³, 单以银¹^,³, 李艳芬¹^,³(

)

1 中国科学院金属研究所师昌绪先进材料创新中心沈阳 110016
2 中国科学技术大学材料科学与工程学院沈阳 110016
3 中国科学院金属研究所中国科学院核用材料与安全评价重点实验室沈阳 110016

Corrosion Behavior and Mechanism of Low Activation 9Cr-ODS Steel in High Temperature and High Pressure Water Environment for the Application in Fusion Reactors

FU Haiyang¹^,², ZHANG Jiarong¹^,³(

), LI Yaozhi¹^,², WANG Qitao¹^,², LI Xinle¹^,², YAN Wei¹^,³, SHAN Yiyin¹^,³, LI Yanfen¹^,³(

)

1 Shi -changxu Innovation Center for Advanced Materials, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
2 School of Materials Science and Engineering, University of Science and Technology of China, Shenyang 110016, China
3 CAS Key Laboratory of Nuclear Materials and Safety Assessment, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China

引用本文:

付海阳, 张家榕, 李尧志, 王旗涛, 李新乐, 严伟, 单以银, 李艳芬. 聚变用低活化9Cr-ODS钢在高温高压水中的腐蚀行为及机理[J]. 金属学报, 2025, 61(9): 1305-1319.
Haiyang FU, Jiarong ZHANG, Yaozhi LI, Qitao WANG, Xinle LI, Wei YAN, Yiyin SHAN, Yanfen LI. Corrosion Behavior and Mechanism of Low Activation 9Cr-ODS Steel in High Temperature and High Pressure Water Environment for the Application in Fusion Reactors[J]. Acta Metall Sin, 2025, 61(9): 1305-1319.

全文: PDF(4521 KB) HTML

摘要:

为了探究低活化9Cr氧化物弥散(9Cr-ODS)钢在设计服役环境下的氧化行为及机理，通过模拟聚变堆高温高压循环水腐蚀实验，研究了其在聚变堆设计冷却水中的腐蚀行为，并与中国低活化马氏体(CLAM)钢进行对比，阐释了腐蚀过程中表面及截面微观结构的演化和氧化产物的形成与转变过程。结果表明，在325 ℃、15.5 MPa的静态高温高压水和动态高温高压水(温度25 ℃、压力15.5 MPa、流速5 mL/min)中，9Cr-ODS钢的腐蚀增重和氧化膜厚度均比CLAM钢低。在静态水中腐蚀时，2种材料的腐蚀产物均为外层为颗粒状的Fe₃O₄、内层为连续的富Cr、Fe 的尖晶石的双层结构；随腐蚀时间从200 h增加至1000 h，氧化物颗粒尺寸和氧化膜厚度逐渐增加；然而在动态水中，2种钢的腐蚀增重及氧化膜厚度反而降低，其中CLAM钢外层氧化物的种类保持不变，但9Cr-ODS钢中除Fe₃O₄外还有少量Fe₂O₃生成。在相同腐蚀条件下，弥散的纳米氧化物、细化的晶粒以及较高的基体O含量对ODS钢耐腐蚀性能产生了积极作用，促进了保护性氧化膜内层的形成，同时也降低了腐蚀增重速率，使得9Cr-ODS钢具有比CLAM钢更优异的耐腐蚀性能。

关键词 ：低活化ODS钢, 高温高压水, 腐蚀, 氧化膜

Abstract：

The China fusion engineering test reactor is a bridge between the international thermonuclear experimental reactor and future fusion demonstration reactors. The harsh service environment of the fusion reactor, including high heat flow density, strong neutron irradiation, and high temperature and high pressure coolant corrosion, demands higher requirements on structural materials than conventional nuclear energy structural materials. Low activation oxide dispersion-strengthened (ODS) steels, which are developed based on reduced activation ferritic/martensitic steels, are considered as promising candidate fusion reactor structural materials because of their high creep strength and excellent resistance to irradiation. In this study, 9Cr-ODS steel prepared by mechanical alloying (MA) and Chinese low activated martensitic (CLAM) steel prepared by vacuum smelting were selected because of their excellent mechanical properties and superior radiation tolerance. The main difference between the two steels is the grain size: the average grain size of the 9Cr-ODS steel is 200-500 nm, whereas that of CLAM steel is 10-20 μm. Furthermore, the 9Cr-ODS steel was added with Y₂O₃ during MA, which improved its mechanical properties and thermal stability. Corrosion experiments were conducted in static and dynamic (flow rate of 5 mL/min) ultrapure water at 325 ^oC and 15.5 MPa. Ultrapure water had an electrical conductivity of 0.1 μS/cm and a dissolved oxygen content of 10 × 10^-9. The exposure time for both steels were set as 200, 500, and 1000 h. Results indicated that under static and dynamic conditions, the corrosion mass gain and oxide film thickness of the 9Cr-ODS steel were less than those of the CLAM steel. Under static conditions, the corrosion product of both materials exhibits a double-layer structure with granular Fe₃O₄ in the outer layer and continuous Cr- and Fe-rich spinel in the inner layer. As the exposure time increased from 200 h to 1000 h, the size and thickness of the oxide particles gradually increased. However, under dynamic conditions with a flow rate of 5 mL/min, the surface of the 9Cr-ODS steel formed not only Fe₃O₄ but also a small amount of Fe₂O₃, while the type of oxide in the outer layer of the CLAM steel remains unchanged. In contrast to the static condition, both steels exhibited decreased corrosion mass loss and oxide film thickness because of the dynamic water scouring effect and the buildup of H₂ on the surface caused by water decomposition through oxidation. Overall, under same corrosion conditions, the presence of dispersed oxides, grain refinement, and a high matrix oxygen concentration positively enhanced the corrosion resistance of the 9Cr-ODS steel. This enhancement facilitated the formation of a protective inner oxide layer and reduced the corrosion mass loss rate, thereby demonstrating the superior corrosion resistance of the 9Cr-ODS steel under high temperature and high pressure water environments compared with the CLAM steel.

Key words： low activation ODS steel high temperature and high pressure water corrosion oxide film

收稿日期: 2023-11-29

ZTFLH:

TG172.82

基金资助:国家自然科学基金项目(51971217);国家磁约束核聚变能发展研究专项项目(2019YFE03130000);中国科学院战略先导科技专项项目(XDA0410000)

通讯作者: 李艳芬，yfli@imr.ac.cn，主要从事先进能源用高性能钢铁材料研究;
张家榕，jrzhang14s@imr.ac.cn，主要从事先进核用钢铁材料研究

Corresponding author: LI Yanfen, professor, Tel: (024)23978990, E-mail: yfli@imr.ac.cn;
ZHANG Jiarong, Tel: (024)83973136, E-mail: jrzhang14s@imr.ac.cn

作者简介: 付海阳，1998年生，男，博士生

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表1 9Cr氧化物弥散强化(9Cr-ODS)和中国低活化马氏体(CLAM)钢的化学成分 (mass fraction / %)

表2 9Cr-ODS和CLAM钢的热处理工艺

图1 腐蚀实验回路装置示意图

图2 9Cr-ODS钢及CLAM钢基体晶粒尺寸的EBSD像

图3 9Cr-ODS和CLAM钢在静态和动态高温高压水中的氧化增重曲线

图4 9Cr-ODS钢和CLAM钢在静态和动态高温高压水中腐蚀后的XRD谱

图5 静态条件下腐蚀不同时间后9Cr-ODS和CLAM钢表面腐蚀产物的SEM像

表3 图5中标记点的EDS结果 (mass fraction / %)

图6 动态条件下腐蚀不同时间后9Cr-ODS钢和CLAM钢的表面腐蚀产物形貌

表4 图6中标记点的EDS结果 (mass fraction / %)

图7 9Cr-ODS和CLAM钢在静态和动态高温高压水中腐蚀1000 h后外表面Fe的详细XPS

图8 9Cr-ODS钢在动态高温高压水中腐蚀1000 h后Fe2p3/2的非线性最小二乘(NLS)拟合结果

图9 9Cr-ODS和CLAM钢在静态和动态高温高压水中腐蚀1000 h后外表面中Cr的详细XPS

图10 9Cr-ODS和CLAM钢在静态高温高压水下腐蚀不同时间后横截面的SEM像

图11 动态条件下9Cr-ODS钢和CLAM钢中表面腐蚀产物横截面的SEM像

图12 9Cr-ODS钢在静态、动态高温高压水中腐蚀1000 h后横截面的SEM像及EPMA元素分布图

图13 9Cr-ODS钢在动态高温高压水中腐蚀1000 h后氧化膜截面的TEM像和SAED花样

No.	Formation	$Δ G 0 = R T l n p O 2$ / (kJ·mol^-1·O₂^-1)
1	$4 F e 3 O 4 + O 2 = 6 F e 2 O 3$	-327.801
2	$43 F e + O 2 = 23 F e 2 O 3$	-446.466
3	$32 F e + O 2 = 12 F e 3 O 4$	-461.299
4	$2 F e + 2 C r 2 O 3 + O 2 = 2 F e C r 2 O 4$	-600.519
5	$12 F e + C r + O 2 = 12 F e C r 2 O 4$	-654.714
6	$43 C r + O 2 = 23 C r 2 O 3$	-672.778

表5 在325 ℃、25 MPa条件下钢表面氧化物的标准生成Gibbs自由能

图14 9Cr-ODS钢在静态、动态高温高压水中腐蚀过程的示意图

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