表面氧含量对高纯硅粉高温氮化行为的影响  

Effects of Surface Oxygen Content on the High-temperature Nitridation of High-purity Silicon Powders

作　　者：兰宇 李兵[1] 周子皓 张以纯 尹传强[1] 魏秀琴[1] 周浪[1] LAN Yu;LI Bing;ZHOU Zihao;ZHANG Yichun;YIN Chuanqiang;WEI Xiuqin;ZHOU Lang(Institute of Photovoltaics/School of Materials Science and Engineering,Nanchang University,Nanchang 330031)

机构地区：[1]南昌大学光伏研究院/材料科学与工程学院,南昌330031

出　　处：《材料导报》2018年第16期2719-2722,共4页Materials Reports

基　　金：江西省优势科技创新团队计划专项(20113BCB24007);有色金属及特色材料加工重点实验室开放基金(12KF-20);南昌大学研究生创新专项资金立项项目(CX2016017)

摘　　要：研究了表面氧含量对高纯硅原料在氮氢气氛下直接氮化行为的影响,并合成高α相氮化硅。研究结果表明,硅粉在氮氢气氛下1 350℃保温3h,氮化产物中α-Si_3N_4含量随原料氧含量的增加呈先增加后减少的趋势,当硅原料表面氧含量为3.91%时,氮化产物中α-Si_3N_4含量可达97%以上,残留硅含量低于1%,产物中部氧含量为1.71%,在此环境下硅粉氮化主要以化学气相沉积的方式进行,产物形貌以杆状α-Si_3N_4晶须为主。硅原料表面氧含量低于4.38%时,氮化产物α-Si_3N_4含量均在95%以上,另有少量的β-Si_3N_4和残留硅,XRD测试精度范围内无氮氧化硅相存在。当硅原料氧含量高于5.61%时,产物中则出现氮氧化硅,随着原料氧含量增加,氮氧化硅含量明显上升。当硅原料氧含量低于5.61%时,残留硅含量随氧含量增加明显减少,说明原料中氧的增加可以显著加快氮化速率,降低氮化产物中残留硅的含量。The effects of surface oxygen content on the nitridation of high-purity silicon powders were studied,high-αphase silicon nitride was prepared via direct nitridation process of silicon powders in the N 2/H 2 atmosphere.The results show that the content ofα-Si 3N 4 in nitridation products tended to increase first and then decrease with the increase of the oxygen content on the silicon surface.When the surface oxygen content of silicon powders was 3.91%,theα-Si 3N 4 content of nitridation products could reach 97%,the residual silicon content was lower than 1%and the oxygen content in central region was 1.71%,the micrograph morphology of nitridation products mainly composed of rod shapedα-Si 3N 4 whisker which was formed by chemical vapor deposition at 1 350℃for 3 hours in the N 2/H 2 atmosphere.When the surface oxygen content of silicon powders was lower than 4.38%,all the content of theα-Si 3N 4 in nitridation products was over 95%,a small amount ofβ-Si 3N 4 and residual silicon phase,which was examined by XRD,can be observed,but no silicon oxynitride.While the oxygen content of silicon powders was higher than 5.61%,the content of silicon oxynitride increased obviously with the increase of oxygen content.While the oxygen content of silicon powders was lower than 5.61%,the residual silicon of nitridation products decreased significantly with the increase of oxygen content,which showed that the increase of oxygen in silicon powders could accelerate the nitridation rate significantly and then reduce the content of residual silicon in nitridation products.

关 键 词：α-氮化硅 氧含量 直接氮化法 高纯硅粉 氮氧化硅 

分 类 号：TQ174[化学工程—陶瓷工业]