声化学获得的SnS2纳米颗粒的热探测:TG残留SnS2的元素、结构和形态研究

Ankurkumar J. Khimani , Sunil H. Chaki , Ranjan Kr. Giri , Reena R. Meena , Rohitkumar M. Kannaujiya , Milind P. Deshpande
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引用次数: 8

摘要

采用声化学方法合成了二硫化锡(SnS2)纳米粒子。通过X射线能量色散分析(EDAX)和X射线光电子能谱(XPS)对Nps进行表征,得到其化学组成。X射线衍射(XRD)用于相和晶体结构的测定。合成的Nps是多晶的,并且具有六边形结构。通过扫描电子显微镜(SEM)和高分辨率透射模式对合成的Nps的表面形态进行了检查。通过EDAX、XPS、XRD、SEM和傅立叶变换红外光谱对热分析后的残余样品进行了表征。比较了热后分析和合成的SnS2-Nps样品的所得结果。Nps的热分析是通过记录热重和差热重曲线来进行的。在惰性氮气氛中,在环境温度至850 K的温度范围内,以5、10、15和20 K·min−1的三种加热速率记录这些同时的热曲线。采用等转化Kissinger Akahira Sunose、Flynn Wall Ozawa和Friedman方法分析了热曲线数据和热力学参数;测定了活化能(Ea)、活化熵变化(ΔS*)、活化焓变化(ΔH*)和活化Gibb自由能变化(ΔG*)。详细讨论了所有获得的结果。
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Thermal exploration of sonochemically achieved SnS2 nanoparticles: Elemental, structural, and morphological investigations of TG residual SnS2

The nanoparticles (Nps) of tin disulfide (SnS2) are synthesized by sonochemical route. The Nps are characterized by dispersive analysis of X-ray energy (EDAX) and X-ray photoelectron spectroscopy (XPS) to get the chemical composition. The diffraction of X-ray (XRD) is used for determination of phase and crystal structure. The as-synthesized Nps are polycrystalline and possess hexagonal structure. The surface morphology of the as-synthesized Nps is examined by electron microscopy in scanning (SEM) and high-resolution transmission modes. The residual sample after the thermal analysis is characterized by EDAX, XPS, XRD, SEM and Fourier transformed infra-red spectroscopy. The obtained results of the post-thermal analyzed and as-synthesized SnS2 Nps samples are compared. The thermal analysis of the Nps is carried out by recording the thermogravimetric and differential thermogravimetric curves. These simultaneous thermo-curves are recorded in the temperature range of ambient to 850 K in inert nitrogen atmosphere for three heating rates of 5, 10, 15 and 20 K·min−1. The thermal curves data are analyzed by the isoconversional Kissinger-Akahira-Sunose, Flynn-Wall-Ozawa, and Friedman methods, and the thermodynamic parameters; activation energy (Ea), change in activation entropy (ΔS*), change in activation enthalpy (ΔH*) and change in activation Gibb's free energy (ΔG*) are determined. All the obtained outcomes are discussed in detail.

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