硅化镁制备单硅烷的工艺研究

Research on Preparation Method of Monosiliane by Mg_2Si Method

单硅烷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、氧化硅和金属硅化物。介绍了一种以硅化镁、氯化铵为原料,液氨为溶剂,经高压釜加压间歇反应制备单硅烷的方法。实验通过对原料配比、溶剂含水、氯化铵溶液浓度、反应时间和反应温度等制备工艺的研究,得到的优化工艺条件为:氯化铵和硅化镁的物质的量比为8∶1,液氨含水<10-5,氯化铵液氨溶液浓度为20%,反应时间为3 h,反应温度为-20℃,单硅烷的收率>95%。

Monosilane can be used to manufacture various high purity crystalline silicon,non-crystalline silicon,silicon nitride,silicon oxides and metal silicides as a Si source gas.A method of producing monosiliane was provided with magnesium silicide and ammonium chloride as raw materials,anhydrous ammonia as solvent,autoclave as pressure batch reactor.By the research of reaction ratio,water in liquid ammonia,concentration of ammonium chloride solution,reaction time and reaction temperature,the obtained optimal conditions were that ratio of ammonium chloride to magnesium silicide was 8∶1,water in liquid ammonia was below 10-5,the solution of liquid ammonium including ammonium chloride was 20%,reaction time was 3 h,reaction temperature was-20 ℃.The yield of monosiliane was more than 95%.