Osip Honorata, Czosnek Cezary, Janik Jerzy F, Marchewka Jakub, Sitarz Maciej
Faculty of Energy and Fuels, AGH University of Science and Technology, Mickiewicza 30, 30-059 Krakow, Poland.
Faculty of Materials Science and Ceramics, AGH University of Science and Technology, Mickiewicza 30, 30-059 Krakow, Poland.
Materials (Basel). 2021 Jan 14;14(2):386. doi: 10.3390/ma14020386.
Silicon oxynitrides (SiON) have many advantageous properties for modern ceramic applications that justify a development of their new and efficient preparation methods. In the paper, we show the possibility of preparing amorphous SiON-based materials from selected liquid organosilicon compounds, methyltrimethoxysilane CHSi(OCH) and methyltriethoxysilane CHSi(OCH), by a convenient spray pyrolysis method. The precursor mist is transported with an inert gas or a mixture of reactive gases through a preheated tube reactor to undergo complex decomposition changes, and the resulting powders are collected in the exhaust filter. The powders are produced at the tube at temperatures of 1200, 1400, and 1600 °C under various gas atmosphere conditions. In the first option, argon Ar gas is used for mist transportation and ammonia NH gas serves as a reactive medium, while in the second option nitrogen N is exclusively applied. Powder X-Ray Diffraction (XRD) results confirm the highly amorphous nature of all products except those made at 1600 °C in nitrogen. SEM examination shows the spheroidal particle morphology of powders, which is typical for this method. Fourier Transform Infrared (FT-IR) spectroscopy reveals the presence of Si-N and Si-O bonds in the powders prepared under Ar/NH, whereas those produced under N additionally contain Si-C bonds. Raman spectroscopy measurements also support some turbostratic free carbon C in the products prepared under nitrogen. The directly determined O- and N-contents provide additional data linking the process conditions with specific powder composition, especially from the point of view of oxygen replacement in the Si-O moieties formed upon initial precursor decomposition reactions by nitrogen (from NH or N) or carbon (from the carbonization of the organic groups).
氮氧化硅(SiON)在现代陶瓷应用中具有许多有利特性,这使得开发其新型高效制备方法成为必要。在本文中,我们展示了通过便捷的喷雾热解方法,从选定的液态有机硅化合物,即甲基三甲氧基硅烷CHSi(OCH)和甲基三乙氧基硅烷CHSi(OCH)制备非晶态SiON基材料的可能性。前驱体雾滴通过惰性气体或反应性气体混合物输送通过预热的管式反应器,以经历复杂的分解变化,然后将所得粉末收集在排气过滤器中。在各种气体气氛条件下,于1200、1400和1600℃的温度下在管式反应器中制备粉末。在第一种方案中,使用氩气Ar输送雾滴,氨气NH用作反应介质,而在第二种方案中仅使用氮气N。粉末X射线衍射(XRD)结果证实,除了在氮气气氛中于1600℃制备的产物外,所有产物均具有高度非晶态性质。扫描电子显微镜(SEM)检查显示了粉末的球形颗粒形态,这是该方法的典型特征。傅里叶变换红外(FT-IR)光谱揭示了在Ar/NH气氛下制备的粉末中存在Si-N和Si-O键,而在N气氛下制备的粉末中还含有Si-C键。拉曼光谱测量也支持在氮气气氛下制备的产物中存在一些乱层游离碳C。直接测定的O和N含量提供了将工艺条件与特定粉末组成联系起来的额外数据,特别是从初始前驱体分解反应形成的Si-O部分中的氧被氮(来自NH或N)或碳(来自有机基团的碳化)取代的角度来看。