化工学报2024,Vol.75Issue(1) :377-390.DOI:10.11949/0438-1157.20230685

6N电子级氘气的制备与纯化技术研究

Preparation and purification of 6N electronic-grade deuterium gas

孟祥军 花莹曦 张长金 张弛 杨林睿 杨若昔 刘鉴漪 许春建
化工学报2024,Vol.75Issue(1) :377-390.DOI:10.11949/0438-1157.20230685

6N电子级氘气的制备与纯化技术研究

Preparation and purification of 6N electronic-grade deuterium gas

孟祥军 1花莹曦 2张长金 2张弛 3杨林睿 3杨若昔 3刘鉴漪 3许春建3
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作者信息

  • 1. 天津大学化工学院,化学工程联合国家重点实验室,天津 300072;中船(邯郸)派瑞特种气体股份有限公司,河北 邯郸 056002
  • 2. 中船(邯郸)派瑞特种气体股份有限公司,河北 邯郸 056002
  • 3. 天津大学化工学院,化学工程联合国家重点实验室,天津 300072
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摘要

电子级氘气在集成电路制造的高温退火工艺中起到关键作用,高端制程工艺要求其纯度高达6N.提出了完整的6N氘气电解制备与纯化技术路线,包括:(1)设计出高效FeNi@ClBC OER催化剂,性能显著优于商用催化剂,提高了催化效率并降低整体能耗;(2)提出了电解阳极端氧气气提脱除重水中氮气等杂质的工艺流程,重水杂质的减少降低了氘气纯化的难度;(3)提出了深度脱氧、脱水工艺流程,筛选出最佳脱氧催化剂和脱水吸附分子筛并对工艺参数进行了优化,实现产品中杂质氧和水含量(体积分数)分别低于1×10-8和1.65×10-7的目标.实验得到的超高纯氘气产品指标达到了6N,满足先进制程集成电路制造需求,为低成本生产超高纯氘气提供了参考.

Abstract

Electronic-grade deuterium gas is of paramount importance in the integrated circuit industry during the high-temperature annealing process,the purity standard for deuterium gas reaches as high as 6N in the 7 nm and even more advanced processes.In this study,a comprehensive technological process for the electrolytic preparation and purification of 6N deuterium gas was proposed,including:(1)designing FeNi@ClBC as a highly efficient OER catalysts,surpassing the performance of the commercial catalyst(RuO2),enhancing the catalytic efficiency while reducing the overall energy consumption;(2)introducing a gas stripping method using electrolytic anode oxygen to remove impurities such as nitrogen from heavy water,and by reducing impurities in heavy water,the purification difficulty of deuterium is significantly diminished;(3)proposing in-depth oxygen and moisture removal processes,screening the optimal catalyst and molecular sieve for the adsorption of oxygen and moisture,and the process parameters are optimized to achieve target oxygen and moisture contents(volume fraction)below 1×10-8 and 1.65×10-7,respectively.The ultra-high-purity deuterium gas product index obtained in the experiment reached 6N,which meets the manufacturing needs of advanced process integrated circuits and provides a reference for the low-cost production of ultra-high-purity deuterium gas.

关键词

电解/制备/催化/吸附/纯化/分离

Key words

electrolysis/preparation/catalysis/adsorption/purification/separation

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基金项目

化学工程联合国家重点实验室自主研究课题(SKL-ChE-22T06)

河北省科技研发平台与新型研发机构建设专项(205676103H)

出版年

2024
化工学报
中国化工学会 化学工业出版社

化工学报

CSTPCDCSCD北大核心
影响因子:1.26
ISSN:0438-1157
参考文献量32
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