基于流态化技术硅粉直接氮化制备氮化硅粉

尹少武; 王立*; 童莉葛; 孙淑凤

北京化工大学学报(自然科学版) ›› 2008, Vol. 35 ›› Issue (1) : 70-74.

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北京化工大学学报(自然科学版) ›› 2008, Vol. 35 ›› Issue (1) : 70-74.
材料科学与工程

基于流态化技术硅粉直接氮化制备氮化硅粉

  • 尹少武; 王立*; 童莉葛; 孙淑凤
作者信息 +

Preparation of silicon nitride powder by a direct nitridation process based on fluidization technology

  • YIN ShaoWu; WANG Li; TONG LiGe; SUN ShuFeng
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文章历史 +

摘要

提出了一种基于流态化技术,利用硅粉直接氮化制备氮化硅粉的新工艺。在常温下,以氮气为载气,将硅粉快速流化并夹带离开供料装置,硅粉和氮气组成的气-固两相流进入到预热器中,预热后的混合物从底部进入到高温悬浮床的高温区,以稀相气力输送的方式连续穿过高温悬浮床,在高温常压下发生燃烧合成反应,最后在出口经冷却装置冷却后,由收集装置收集,得到氮化产物。借助SEM、XRD、元素分析和FTIR等方法分析了氮化产物的形貌、物相组成、化学成分以及价键结构。实验结果表明:对于平均粒径为2.7μm的硅粉,在反应温度为1653K, 反应时间为2.7min时,硅的转化率为53.4%,氮化产物为非晶氮化硅粉。通过理论预测,如果将反应温度升高至1723K,硅粉氮化7.1min后,其转化率可达99%。本文提出的方法可连续制备优质氮化硅粉,而且比现有的其他制备方法具有更高的生产效率。

Abstract

A method for the preparation of silicon nitride powder by a direct nitridation process based on fluidization technology is described. At room temperature, using nitrogen as carrier gas, silicon powder was rapidly fluidized and the gas-solid two-phase mixture was carried from the feeding device into a preheater. The preheated mixture was then passcd through a high-temperature suspended bed by a dilute phase pneumatic conveying process. Combustion synthesis at atmospheric pressure and high temperature afforded the nitridation products which were passed through a cooling device and collected. The morphology, phase composition, chemical composition and structure of the nitridation products were studied by SEM, XRD, elemental analysis and FTIR spectroscopy. In the case of silicon powder with particle size of 2.7μm, with a reaction temperature of 1653 K and reaction time of 2.7 minutes, the conversion of silicon was 53.4 %, and the products comprised amorphous silicon nitride powders. Theoretical predictions suggest that if the reaction temperature is increased to 1723 K, and the reaction time extended to 7.1 minutes, and the conversion of silicon should reach 99 %. The method present- ed here can be used for the continuous production of high-quality silicon nitride powders and has higher production efficiency than existing methods.

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尹少武; 王立*; 童莉葛; 孙淑凤. 基于流态化技术硅粉直接氮化制备氮化硅粉[J]. 北京化工大学学报(自然科学版), 2008, 35(1): 70-74
YIN ShaoWu; WANG Li; TONG LiGe; SUN ShuFeng
.
Preparation of silicon nitride powder by a direct nitridation process based on fluidization technology[J]. Journal of Beijing University of Chemical Technology, 2008, 35(1): 70-74

参考文献

[1] 陈宏,穆柏春,郑黎明.氮化硅微粉制备技术[J].辽宁工学院学报,2006,26(3):195-195.
[2] 王声宏,张英才,韩文成,等.自蔓延高温合成氮化硅的研究[J].粉末冶金工业,2004,14(5):1-5.
[3] 李亚伟,张忻,田海兵,等.硅粉直接氮化反应合成氮化硅研究[J].硅酸盐通报,2003(1):30-34.
[4] 王锐,李道火,黄永攀,等.激光诱导化学气相沉积法制备纳米氮化硅及粉体光谱特性研究[J].中国粉体技术,2003,9(4):35-38.
[5] 陕绍云,杨建锋,高积强,等.用碳热还原法制备多孔氮化硅陶瓷[犑].无机材料学报,2006,21(4):913-918.
[6] Fukuoka H, Shimizu M, Ochiai H, et al. Preparation of silicon nitride powder by partially nitriding in a fluidized bed and then completing nitridation in a moving bed:US:5232677[P]. 1993-08-03.
[7] Liu Yaodian, Kimura S. Fluidized-bed nitridation of fine silicon powder [J]. Powder Technology, 1996, 106:160 167. [
8] Jovanovic Z R. Kinetics of direct nitridation of pelletized silicon grains in a fluidized bed: experiment, mechanism and modeling [J]. Journal of Materials Sciences, 1998(33): 2339 2355.
[9] Koike J, Kimura S. Mechanism of nitridation of silicon powder in a fluidized-bed reactor [J ]. Journal of the American Ceramic Society, 1996,79(2): 365 370.
[10]吕秀玮.流态化合成氮化硅的鼓泡床热模实验与CFD模拟研究[D]:硕士学位论文.南京:南京工业大学,2004.
[11]王立,尹少武,董继昌,等.基于流态化技术常压连续合成氮化硅粉末的方法:中国,CN1792774[P].2006-06-28.
[12]尹少武,王立,甘恢琪,等.用于制备氮化硅粉的高温电阻炉的设计与应用[J].冶金能源,2007,26(1):34-38 [13] Jovanovic Z, Kimura 5, Levnspiel 0. Effects of hydrogen and temperature on the kinetics of the fluidized-bed nitridation of silicon[J]. Journal of American Ceramic Society, 1994, 77(1): 186 192.
[14] Campos-Loriz D, Riley F L. The effects of hydrogen on the nitridation of silicon[J 1. Journal of Materials Science Letters, 1979,14(4): 1007 1008.
[15]罗康碧,罗明河,李沪萍.反应工程原理[J].北京:科学出版社,2005.

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