ISSN 1008-5548

CN 37-1316/TU

2006年12卷  第6期
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自蔓燃高温合成氮化硅粉体的研究

Research of Silicon Nitride Powder Prepared by Self-propagating High-temperature Synthesis

Doi:10.13732/j.issn.1008-5548.2006.06.004
作者:李金富,常永威,李康,王正军,段关文,王拥军

摘 要: 研究了自蔓燃高温合成方法制备氮化硅粉体, 借助于 XRD、 SEM 等检测方法, 分析了自蔓燃高温合成氮化硅过程中硅粉粒度、 氮气、温度、稀释剂与孔隙率等方面对反应产物的影响, 并对反应机 理进行了分析。由于有添加剂氯化铵的存在, 反应中不是单纯的硅粉 氮化反应。只要控制反应中的工艺参数, 就可以采用自蔓燃得到不同 相含量的 Si3N4 粉体; 考虑到燃烧温度, 在氮化硅粉体的合成过程中, 涉及到 3 个反应机制: 低温机制、中温机制、高温机制; 氮气压力下硅 粉的自蔓燃合成反应, 必须要引入 Si3N4 稀释剂, 来控制反应温度和 反应速度, 获得不同相含量的粉体。压坯气孔率控制在 30%~70%, 否则反应不能进行金属硅粉的粒度细, 合成的 Si3N4 中 α相含量高。 

关键词: 自蔓燃高温合成; 氮化硅粉体; 反应机理

Abstract: Si3N4 powder was prepared by the self-propagating high-tem perature synthesis (SHS) and examined by X-ray diffraction and SEM. It was studied how the following parameters influenced the final product: nitrogen purity and pressure, combustion temperature, diluents content, the porosity, and so on. The experimental shows that the different type of Si3N4 powder can be prepared by SHS as long as the parameters be con trolled during the reaction. Because of the existence of the NH4Cl, the re action involves not only the silicon nitriding mechanism, but also other mechanisms. Considering the combustion temperature, the SHS Si3N4process involves three mechanisms: low-temperature mechanism, mod erate-temperature mechanism, high-temperature mechanism. During the process Si3N4 powder must be introduced as starting raw materia1 in or der to control reaction temperature and obtain the desired αcontent of Si3N4 powder, the porosity of body should be controlled at 30%~70%,otherwise, SHS reaction will not carry on the Si3N4 powder with high α phase content can be prepared when fine silicon metal powder used. 

Keywords: self-propagating high-temperature synthesis; silicon mitride powder; reaction mechanism