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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 is the key raw material for optical fiber manufacturing, the quality of which determines the optical fiber transmission performance. SiHCl3 is a common hydrogen-containing impurity in SiCl4. The content of SiHCl3 has a serious impact on the quality of SiCl4. The research progress of SiHCl3 removal methods in SiCl4 is reviewed at home and abroad, mainly including distillation, plasma, photochemical, adsorption and partial hydrolysis. However, as the boiling points of SiHCl3 and SiCl4 are close to each other, the rectification method still has some limitations on the removal of SiHCl3 in SiCl4. The removal of SiHCl3 by the plasma method is effective, but the relative technical requirements for the equipment are relatively lower High; photochemical method for the removal of SiHCl3 is very effective, SiHCl3 content can be reduced to below 1 × 10-6. At the same time, SiCl4 SiHCl3 content detection methods, including gas chromatography, Fourier transform infrared spectroscopy (FT-IR method), infrared air reference method. Gas chromatography with a few milligrams of SiCl4 can be detected in which micrograms of SiHCl3 characteristics, the detection limit of 0.1 × 10-6; FT-IR method not only for laboratory analysis, and can be applied to the production site analysis of SiHCl3 The lower limit of measurement is 0.6 × 10-6; the lower limit of measurement of SiHCl3 by infrared air reference method is 2 × 10-6. SiCl4 in SiHCl3 removal process, testing technology research, for the purification of high purity SiCl4 fiber, and then for the localization of key raw materials for optical fiber, is of great significance.