SiCl_4中SiHCl_3的去除及检测方法研究进展  

Progress in Removal and Determination of Trichlorosilane in Silicon Tetrachloride

作　　者：毛威[1] 苏小平[1] 王铁艳[1] 袁琴[1] 

机构地区：[1]北京有色金属研究总院国晶辉红外光学科技有限公司,北京100088

出　　处：《稀有金属》2011年第1期143-149,共7页Chinese Journal of Rare Metals

基　　金：国家科技支撑计划课题(2007BAE39B06)资助项目

摘　　要：SiCl4是光纤制造的关键原材料,其质量的高低决定着光纤的传输性能。SiHCl3是SiCl4中常见的一种含氢杂质,其含量的多少对SiCl4质量产生严重影响。综述了国内外对于SiCl4中SiHCl3去除方法的研究进展,主要有精馏法、等离子体法、光化法,以及吸附法、部分水解法等其他一些方法。国内常用精馏法提纯SiCl4,但由于SiHCl3和SiCl4的沸点较为接近,精馏法对于SiCl4中SiHCl3的去除仍然存在着一定的限度;等离子体法去除SiHCl3效果好,但对于设备、技术要求相对较高;光化法对于SiHCl3的去除十分有效,可将SiHCl3的含量降到1×10-6以下。同时介绍了SiCl4中SiHCl3含量的检测方法,包括气相色谱法、傅里叶变换红外光谱法(FT-IR法)、红外空气参考法。气相色谱法具有取几毫克SiCl4即可检出其中微克级SiHCl3的特点,其检测下限为0.1×10-6;FT-IR法不仅可用于实验室分析,而且可应用于生产现场分析,对SiHCl3的测量下限为0.6×10-6;红外空气参考法对SiHCl3的测量下限为2×10-6。进行SiCl4中SiHCl3的去除工艺、检测技术研究,对于光纤用高纯SiCl4的提纯,进而对于光纤用关键原料国产化,具有重要的意义。SiCl4 was one of the main materials for making optical fiber,and its quality would decide the transmission performance of optical fiber.As one kind of hydrogen impurities which was often found in SiCl4,concentration of SiHCl3 would influence on the quality of SiCl4.The progress on removal of SiHCl3 in SiCl4 was summarized.The removing methods mainly included rectification method,plasma method,photochemistry method and other methods such as adsorption method,partial hydrolysis method,etc.Rectification was a popular method to purify SiCl4 in China.However,there existed a certain limit in rectification for removal of SiHCl3 in SiCl4 because the boiling point of SiHCl3 and SiCl4 was closer.The effect of plasma method on removing SiHCl3 was good but relatively high equipment and technique was needed.Photochemistry method was effective for removal of SiHCl3,and content of SiHCl3 could drop below 1×10-6.Determination of SiHCl3 in SiCl4 was also discussed,including gas chromatogram determination,Fourier transform infrared spectroscopy（FT-IR）,and infrared spectroscopy.Gas chromatogram had the characteristic that μg level of SiHCl3 could be detected in a few milligrams of SiCl4,and detection limit was 0.1×10-6.FT-IR method could be used in experimental analysis and production site analysis,and detection limit was 0.6×10-6.The detection limit of infrared spectroscopy for SiHCl3 was 2×10-6.Researches for removal and determination of SiHCl3 in SiCl4 were important to purification of high-purity SiCl4 for optical fiber,so as to the localization of critical material for optical fiber.

关 键 词：SiCl4 光纤 SiHCl3 去除 检测 

分 类 号：TQ127.21[化学工程—无机化工]