超导材料用铌表面清洗工艺  

Cleaning Technology of Niobium for Superconducting Materials

作　　者：周安林[1] 李建峰[1] 刘建伟[1] 

机构地区：[1]西部超导材料科技股份有限公司超导材料制备国家工程实验室,西安710018

出　　处：《中国表面工程》2013年第4期83-87,共5页China Surface Engineering

基　　金：国家高技术研究发展计划(863计划)(2007AA03Z205);国家重点基础研究发展计划(973计划)(2008CB717903);国家科技部ITER专项(2008GB101001);国际科技合作项目(2007DFD50700)

摘　　要：采用乳化剂溶液在超声波作用下对金属铌表面进行去油去灰清洗,并用硝酸和氢氟酸混合酸液进行酸洗,通过扫描电镜(SEM)、光电子能谱(XPS)及腐蚀深度对清洗表面进行分析。结果表明:采用乳化剂溶液在超声波作用下清洗对去油去灰有很好效果,可以获得均一的酸洗初始腐蚀界面,其中乳化剂温度为40～50℃,超声波频率为20～25kHz,采用混合酸液浓度为35%分析纯硝酸和10%分析纯氢氟酸的清洗工艺能达到较好的清洗效果和均一的表面状态。合理控制硝酸和氢氟酸浓度对于保证清洗质量和防止材料吸氢脆化很关键,通过腐蚀可以实现表面以Nb2O5状态存在转变为以单质铌存在,实现氧化物的溶解,改善表面结构;铌清洗后在环境放置稳定性强,不容易吸水、氧化和变质;清洗液特征可以通过游离氟离子、铌离子、酸度进行表征。Cleaning process was studied by removing the oil with emulsifier solution under the effect of ultrasound and pickling surface with the mixed acid of nitric acid and hydrofluoric acid. Cleaning surface was analyzed by SEM, XPS and corrosion depth. The results show that using emulsifier solution under the effect of ultrasound has a good effect on the ash and oil cleaning, which can create a uniform interface for pickling. The temperature of emulsifier is 40-50 ℃ and frequency of ultrasonic is 20-25 kHz. Cleaing with the mixed acid of nitric acid of 35% and hydrofluoric acid of 10% can achieve good cleaning effect and surface state requirements. The surface chemical structure changes and Nb2O5 dissolves into Nb. Reasonable control of nitric acid and hydrofluoric acid concentration can ensure the cleaning quality and prevent material from absorbing hydrogen. Good washing and drying processes are necessary to ensure the quality. Niobium has strong stability after cleaning. Cleaning fluid characteristics can be characterized by the free fluoride ion, niobium ion and acidity.

关 键 词：铌 清洗 吸氢 表面状态 

分 类 号：TG178[金属学及工艺—金属表面处理] TM26[金属学及工艺—金属学]