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Preparation of Silicon Nitride and Oxonitride by Gas-Phase Pyrolysis of Hexamethyldisilazane
Inorganic Materials: Applied Research ( IF 0.5 ) Pub Date : 2020-04-13 , DOI: 10.1134/s2075113320020288
N. A. Ovsyannikov , Yu. F. Kargin , A. S. Lysenkov , N. A. Alad’ev , S. N. Ivicheva , K. A. Solntsev

Abstract

The technique was developed, the installation was done, and the conditions for the production of Si3N4 and Si2N2O by the method of gas-phase pyrolysis of hexamethyldisilazane (CH3)3-Si-NH-Si-(CH3)3 (HMDS) were experimentally studied. In the experiments, two different methods of inputting the raw material were used—the input of a vapor–gas mixture (bubbling feeder with heating to supply the HMDS vapor in a stream of carrier gases) and input as a gas-droplet stream (pneumatic nozzle). The effect of gas-dynamic synthesis conditions at temperatures up to 1100°C on the properties of silicon oxonitride and silicon nitride nanopowders was studied. The influence of the conditions of mixing the reactants, the volume ratio of nitrogen/ammonia, and the content of HMDS in the vapor–gas mixture on the yield of products was shown. The dependences of the degree of conversion of the feedstock on the gas flow rate and the concentration of ammonia in the gas phase were obtained. The optimal conditions for the pyrolysis process were found: temperature, the ratio of the components of the gas mixture, the conditions of mixing, and the contact times of the phases. X-ray amorphous Si3N4 and Si2N2O powders with particle sizes of 50–200 nm and a specific surface area of up to 15 m2/g and powders of alpha modification of silicon nitride Si3N4 in the form of threadlike crystals with a particle diameter of 50–200 nm were obtained.


中文翻译:

六甲基二硅氮烷气相热解法制备氮化硅和氮氧化物

摘要

开发了该技术,进行了安装,并确定了通过六甲基二硅氮烷(CH 33 -Si-NH-Si-()气相热解法生产Si 3 N 4和Si 2 N 2 O的条件。CH 33(HMDS)进行了实验研究。在实验中,使用了两种不同的输入原料的方法-蒸气-气体混合物(鼓泡供料器,加热加热以在载气流中供应HMDS蒸气)和作为液滴流(气动)输入喷嘴)。研究了高达1100°C的气体动力学合成条件对氧氮化硅和氮化硅纳米粉体性能的影响。显示了反应物混合条件,氮气/氨气的体积比以及汽-气混合物中HMDS的含量对产物收率的影响。获得了原料转化率对气体流速和气相中氨浓度的依赖性。发现了热解过程的最佳条件:温度,气体混合物中各组分的比例,混合条件和各相的接触时间。X射线非晶硅粒径为50-200 nm,比表面积最大为15 m 2 / g的3 N 4和Si 2 N 2 O粉末以及呈线状晶体形式的氮化硅Si 3 N 4的α改性粉末,获得的粒径为50-200 nm。
更新日期:2020-04-13
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