Laboratory of Advanced Materials and Catalytic Engineering, State Key Laboratory of Fine Chemicals, Dalian University of Technology, China.
Phys Chem Chem Phys. 2011 May 28;13(20):9432-8. doi: 10.1039/c1cp20197b. Epub 2011 Apr 11.
Silica supported CoSi particles were synthesized by metal organic chemical vapor deposition of the Co(SiCl(3))(CO)(4) precursor carried in hydrogen at atmospheric pressure and moderate temperature in a fluidized bed reactor. In contrast, CoCl(2) supported on silica was formed by using argon as the carrier gas. The samples were characterized by X-ray diffraction, transmission electron microscopy, ultraviolet-visible spectroscopy, and thermogravimetric/differential thermogravimetric analysis. The precursor Co(SiCl(3))(CO)(4) reacted with the hydroxyl groups of amorphous silica via loss of HCl and introduced cobalt species onto the surface. The decomposition mechanism of the supported precursor on silica was investigated by in situ Fourier transform infrared spectroscopy from room temperature to 300 °C in a hydrogen or argon atmosphere. The results showed that CO and HCl elimination occurred in a hydrogen atmosphere, while only CO elimination occurred in Ar. All of the results showed that it was possible to prepare supported CoSi at lower temperatures via changing the carrier gas.
通过在常压和中等温度下，在流化床反应器中用氢气携带 Co(SiCl(3))(CO)(4)前体进行金属有机化学气相沉积，合成了硅负载的 CoSi 颗粒。相比之下，通过使用氩气作为载气形成了负载在硅上的 CoCl(2)。通过 X 射线衍射、透射电子显微镜、紫外-可见光谱和热重/差示热重分析对样品进行了表征。前体 Co(SiCl(3))(CO)(4)通过失去 HCl 与无定形硅的羟基反应，并将钴物种引入到表面上。通过在氢气或氩气气氛中从室温到 300°C 的原位傅里叶变换红外光谱研究了负载在硅上的前体的分解机制。结果表明，在氢气气氛中发生 CO 和 HCl 的消除，而在 Ar 中仅发生 CO 的消除。所有结果表明，通过改变载气可以在较低温度下制备负载型 CoSi。
