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原位一步还原碳化法合成碳包覆 MoC 的热学和结构研究。

Thermal and structural studies of carbon coated MoC synthesized via in-situ single step reduction-carburization.

机构信息

School of Physics and Materials Science, Thapar University, Patiala, 147 004, India.

出版信息

Sci Rep. 2017 Jun 14;7(1):3518. doi: 10.1038/s41598-017-03197-8.

Abstract

Carbon coated nano molybdenum carbide (MoC) has been synthesized at 800 °C through single step reduction route using molybdenum trioxide (MoO) as a precursor, polypropylene (P.P) as a carbon source and magnesium (Mg) as a catalyst in an autoclave. The synthesized samples were characterized by X-ray diffraction (XRD), thermal analysis techniques (TG/DTA/DTG), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Williamson- Hall (W-H) analysis has been done to estimate various parameters like strain, stress and strain energy density. Multi-stage kinetic analysis of the product phase has been studied to establish the nature of the thermal decomposition. Coats-Redfern method applied to determine the mechanism involved in the decomposition of the product phase shows that initial and final stage follow F1 mechanism whereas middle stage follow F3 mechanism. The activation energy (E ) and pre-exponential factor (A) has also been determined. The morphological studies shows that the particles have partially spherical/faceted shape, with carbon coated having wide particle size distribution. The surface chemistry and surface area analysis were studied by X-ray photoelectron spectroscopy (XPS) and Brunauer-Emmet-Teller (BET), respectively. The formation mechanism of carbon coated MoC nano particles has been predicted based on the XRD, TG/DTA & DTG and microstructural results.

摘要

在高压釜中,通过一步还原法,以三氧化钼 (MoO) 为前驱体、聚丙烯 (P.P) 为碳源、镁 (Mg) 为催化剂,在 800°C 下合成了碳包覆纳米碳化钼 (MoC)。通过 X 射线衍射 (XRD)、热分析技术 (TG/DTA/DTG)、场发射扫描电子显微镜 (FESEM) 和透射电子显微镜 (TEM) 对合成的样品进行了表征。采用 Williamson-Hall (W-H) 分析估算了应变、应力和应变能密度等各种参数。对产物相的多阶段动力学分析进行了研究,以确定其热分解的性质。应用 Coats-Redfern 方法确定分解产物相涉及的机制表明,初始和最终阶段遵循 F1 机制,而中间阶段遵循 F3 机制。还确定了活化能 (E) 和频率因子 (A)。形貌研究表明,颗粒具有部分球形/有面形状,碳包覆颗粒具有较宽的粒径分布。通过 X 射线光电子能谱 (XPS) 和 Brunauer-Emmet-Teller (BET) 分别研究了表面化学和比表面积分析。根据 XRD、TG/DTA 和 DTG 以及微观结构结果,预测了碳包覆 MoC 纳米颗粒的形成机制。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/1e06/5471264/65327af66003/41598_2017_3197_Fig1_HTML.jpg

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