原位拉曼光谱技术研究600合金和690合金在模拟压水堆工况下的腐蚀行为
InSitu Raman Spectroscopy Study on Corrosion Behavior of Alloy 600 and Alloy 690 in Simulated PWR Primary Water
摘 要
介绍了一种可用于核电材料在模拟压水堆工况下腐蚀行为研究的原位表征技术。设计并制作了原位拉曼观察用高压釜，通过在样品表面电化学沉积金颗粒的方法实现拉曼信号的增强。采用拉曼光谱技术研究了600合金以及690合金在高温高压水环境中的氧化膜特征。结果表明：当极化电位从-0.85 V(SHE,下同)增加到-0.5 V，600合金腐蚀氧化膜中的尖晶石含量显著增加，而690合金的氧化膜成分及含量均无明显变化。原位拉曼光谱技术可用于研究氧化膜随腐蚀时间的演变情况以及环境参数改变对氧化膜的影响等，具有可对比性强的特点，可以用来研究材料在模拟压水堆环境中的腐蚀行为。
高温高压水
腐蚀行为
insitu Raman spectroscopy
hightemperature and highpressure water
corrosion behavior
Abstract
An insitu characterization technique is introduced, which could be used in the study on corrosion behavior of nuclear materials in simulated PWR primarywater. A hightemperature autoclave with an Raman observation window was designed and fabricated. Raman signal was significantly amplified due to a thin layer of Au nanoparticles electrochemically deposited on sample′s surface, insitu Raman spectroscopy was used to investigate the surface films formed on alloy 600 and alloy 690 in hightemperature and highpressure water. As the polarization potential increased from -0.85 V to -0.5 V (vs. SHE), the amount of spinel in the surface film of alloy 600 increased, while the composition and the amount of surface film of alloy 690 were unchanged. Insitu Raman spectroscopy can be used in the investigation of surface films changing with time or environmental parameters, and has wide applications in the study on the corrosion behavior in simulated PWR primary water.
中图分类号 TG172.82 DOI 10.11973/fsyfh201607005
所属栏目 核电设备材料防护
基金项目 国家核电技术有限公司资助项目（2015SN010006）
收稿日期 2016/3/23
修改稿日期
网络出版日期
作者单位点击查看
备注汪 峰，高级工程师，博士，从事核电材料腐蚀研究
引用该论文: WANG Feng,Thomas M. Devine. InSitu Raman Spectroscopy Study on Corrosion Behavior of Alloy 600 and Alloy 690 in Simulated PWR Primary Water[J]. Corrosion & Protection, 2016, 37(7): 549
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【3】马林生，王快社，岳强,等. 核反应堆用锆合金性能分析\[J\]. 金属世界,2014(5):3842.
【4】周邦新,李强,黄强,等. 水化学对锆合金耐腐蚀性能影响的研究\[J\]. 核动力工程,2000,21(5):439447.
【5】李成涛,宋利君,任爱,等. 690合金在核电一回路水环境的应力腐蚀行为\[J\]. 哈尔滨工程大学学报,2013,34(11):14651470.
【6】张志明，王俭秋，韩恩厚,等. 表面状态对690TT合金腐蚀及应力腐蚀行为的影响\[J\]. 中国腐蚀与防护学报,2011,31(6):441445.
【7】但体纯,吕战鹏,王俭秋,等. 690合金在高温水中的应力腐蚀裂纹扩展行为\[J\]. 金属学报,2010,46(10):12671274.
【8】周邦新,李强,刘文庆,等. 水化学及合金成分对锆合金腐蚀时氧化膜显微组织演化的影响\[J\]. 稀有金属材料与工程,2006,35(7):10091016.
【9】李强，杨艳平，黄昌军,等. Zr4合金氧化膜显微组织与疖状腐蚀机制研究\[J\]. 稀有金属材料与工程,2013,42(9):18141819.
【10】章海霞,李中奎. 新锆合金氧化膜的晶体结构分析\[J\]. 稀有金属材料与工程,2006,35(12):19081911.
【11】L Z P,CHEN J J,SHOJI T,et al. Characterization of microstructure,local deformation and microchemistry in alloy 690 heataffected zone and stress corrosion cracking in high temperature water\[J\]. Nucl Mater,2015,465(5):471481.
【12】ZHU L K,YAN Y,LI J X,et al. Stress corrosion cracking at low loads:surface slip and crystallographic analysis\[J\]. Corros Sci,2015(97):619626.
【13】KUANG W J,WAS G S. The effects of grain boundary carbide density and strain rate on the stress corrosion cracking behavior of cold rolled alloy 690\[J\]. Corros Sci,2015(97):107114.
【14】SENNOUR M,MARCHETTI L,MARTIN F,et al. A detailed TEM and SEM study of Nibase alloys oxide scales formed in primary conditions of pressurized water reactor\[J\]. J Nucl Mater,2010,402(2/3):147156.
【15】李中奎,刘建章,周廉,等. 新锆合金氧化膜微观组织结构的研究\[J\]. 稀有金属材料与工程,2002,31(4):261265.
【16】鲁艳萍,姚美意,周邦新,等. 热处理对N36锆合金腐蚀与吸氢性能的影响\[J\]. 上海大学学报,2008,14(2):194199.
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【19】NOVOTNY L,HECHT B. Principles of NanoOptics\[M\]. Cambridge:Cambridge Univeristy,2006:407422.
【20】KNEIPP K,MOSKOYITS M,KNEIPP H. Surfaceenhanced raman scatteringphysics and applications\[M\]. New York:Springer,2010:6785.
【21】汪峰，DEVINE T M. 高温高压水中镍和铬表面氧化膜的原位表面增强型拉曼光谱研究\[J\]. 原子能科学技术，2013,47(增):387393.
【22】WANG F,HARRINGTON S,DEVINE T M. In situ investigation of the passive films formed on chromium in aqueous (pH=8.4) borate buffer and aqueous chloride solutions\[J\]. Electrochem Soc Trans,2007,31(3):3947.
【23】OBLONSKY L J,DEVINE T M. A surface enhanced raman spectroscopic study of the passive films formed in borate buffer on iron,nickel,chromium and stainless steel\[J\]. Corros Sci,1995,37(1):1741.
【24】汪峰，Devine T M. 核电站蒸汽发生器传热管用Inconel合金在高温高压水中的腐蚀行为研究\[J\]. 腐蚀科学与防护技术，2015,27(1):1924.
【25】FARROW R L,BENNER R E,NAGELBERG A S,et al. Characterization of surface oxides by Raman spectroscopy\[J\]. Thin Solid Films,1980,73(2):353358.
【26】CHEN M,SHU J F,XIE X D,et al. Natural CaTi2O4structured FeCr2O4 polymorph in the Suizhou meteorite and its significance in mantle mineralogy\[J\]. Geochim Cosmochim Acta,2003,67(20):39373942.
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