季铵碱树脂催化三甲氧基硅烷制备甲硅烷

为制备高纯度甲硅烷气体,用强碱性季铵碱阴离子交换树脂催化三甲氧基硅烷溶液进行歧化反应.采用脉冲放电氦离子化检测器测试粗甲硅烷气体,用气相色谱-质谱联用仪、感应耦合等离子体质谱仪测试精馏提纯的副产物四甲氧基硅烷.实验结果表明:在30～50℃和0.2～0.3 MPa条件下反应制备的粗甲硅烷气体中,H2、O2、Ar、N2、CH4的质量浓度分别为221.12、1.76、1.61、17.97、0.15μg/L,纯度达到99.9%;副产物四甲氧基硅烷中,金属杂质总质量浓度低于0.15μg/L,可用来制备高纯度硅溶胶;季铵碱催化三甲氧基硅烷歧化反应,反应条件温和,三甲氧基硅烷转化率96%,硅烷产率95%.催化剂易于购买,采用固定床反应器易于控制反应,易于连续加料,此工艺具有工业化生产价值.     

歧化法制备单硅烷的工艺进展

单硅烷(SiH4)作为一种提供硅组分的气体源,可用于制造多种高纯度晶体硅、非晶硅、氮化硅、氧化硅及金属硅化物,因其高纯度和能够实现精细控制而成为至今为止世界唯一大规模生产粒状高纯硅的中间产物。SiH4的工业合成方法包括硅化镁法、氯硅烷或烷氧基硅烷歧化法、氯硅烷还原法等,重点介绍了用歧化法制备SiH4的工艺,原料可用芳基硅烷、烷氧基硅烷以及氯硅烷等。     

硅烷的精制及罐装

介绍了硅烷(SiH4)的物化性质和应用.电子和半导体行业用SiH4要求有高的纯度,重点介绍了SiH4的精制工艺.SiH4的精制方法主要有吸附法、冷冻法和精馏法3类,它们均能满足各自的工艺需要.此外,详细介绍了国外高纯SiH4的灌装工艺.     

电化学法制备单硅烷工艺概述

单硅烷（SiH4）作为一种提供硅组分的气体源,可用于制造多种高纯度晶体硅、非晶硅、氮化硅、氧化硅及金属硅化物,因其高纯度和能够实现精细控制而成为至今为止世界唯一大规模生产粒状高纯硅的中间产物。介绍了SiH4的物化性质及毒性。SiH4的工业合成方法包括硅化镁法、氯硅烷或烷氧基硅烷歧化法、氯硅烷还原法等,但它们存在工艺流程复杂、设备成本高、需要对产物进行复杂的精制等问题。详细介绍了几种国外公司开发的电化学合成SiH4的装置及工艺,该类方法具有操作安全和经济、可实现高度一体化、可现场发生、以及产物精制工艺简单等优点。     

三氯氢硅歧化反应精馏生产硅烷的模拟简

The reactive distillation process for producing high purity monosilane via trichlorosilane redistribution reaction was simulated. Rigorous RadFrac block was employed in Aspen Plus simulation package. Accurate results could be given when the chemical kinetics was taken into account in the equilibrium stage model. A single column process was used for the verification of previous studies. The results showed that 99.9% purity monosilane could be achieved in the reactive distillation. A pumparound block was employed to reduce the condenser duty with inexpen- sive coolant. The effects of operating pressure, feed stage location, liquid holdup per stage and pumparound loca- tion were also investigated. The energy consumption was limited, but the refrigerant temperature was too low, which is the fatal disadvantage. Therefore, a double columns process was developed to increase the condenser tem- perature. The simulation results demonstrated that a reasonable temperature could be achieved by varying the recy- cle stream location.     

两种工业合成单硅烷的工艺介绍

单硅烷(SiH4)作为一种提供硅组分的气体源,可用于制造多种高纯度晶体硅、非晶硅、氮化硅、氧化硅及金属硅化物,详细介绍了硅化镁法和还原法制备SiH4的工艺。硅化镁法的优点是工艺简单、成熟,原料易得;其缺点是分离和回收液氨时能耗大,SiH4收率相对较低。还原法的优点是可实现连续化生产、反应易于控制。     

From monosilane to crystalline silicon, Part I: Decomposition of monosilane at 690–830 K and initial pressures 0.1–6.6 MPa in a free-space reactor

Thermal decomposition of undiluted monosilane at high pressures produces amorphous spherical silicon particles, with a mean diameter of 3 μm, clustered together. The size of the particles remains unchanged regardless of monosilane initial pressures between 0.13 and 6.61 MPa. This may reflect that the particle nucleation process is completed at an early stage of the decomposition reaction and/or demonstrate growth inhibition caused by the high hydrogen pressure resulting from the decomposition. The hydrogen content of the particles goes through a maximum of 5 at% at 2 MPa initial pressure and seems to flatten at some 3.5 at% hydrogen at the highest monosilane initial pressures studied. After dehydrogenation by heat treatment, the present raw-silicon powder is easily melted and crystalline silicon obtained on cooling.