Koul R K, Suri Shivani, Singh Vishal, Bamzai K K
Crystal Growth & Materials Research Laboratory, Department of Physics and Electronics, University of Jammu, Jammu 180006, India.
Int Sch Res Notices. 2014 Oct 20;2014:141463. doi: 10.1155/2014/141463. eCollection 2014.
Synthesis of mixed gadolinium calcium heptamolybdate (GdCaHM) system in silica gel medium using single gel single tube technique has been successfully achieved. The grown crystal exhibits various morphologies, which includes spherulites, multifaceted, and square platelets. The nature of the grown material was established by X-ray diffraction (XRD) studies. Fourier transform infrared spectroscopy (FTIR) study signifies the presence of heptamolybdate (Mo7O24) and water symmetry structure, whereas energy dispersive X-ray analysis (EDAX) establishes the stoichiometric of the grown crystal as GdCaMo7O24·8H2O. The thermal behaviour was studied using the thermoanalytical techniques, which include thermogravimetry (TG), differential thermal analysis (DTA), and differential scanning calorimetry (DSC). Results obtained on the application of TG based models, namely, Horowitz-Metzger, Coats-Redfern, and Piloyan-Novikova, suggest the contracting cylindrical model as the relevant model for the thermal decomposition of the material. The kinetic parameters, namely, the order of reaction (n), activation energy (E a ), frequency factor (Z), and entropy (ΔS∗), were also calculated using these three models.
采用单凝胶单管技术在硅胶介质中成功合成了混合钆钙七钼酸盐(GdCaHM)体系。生长出的晶体呈现出多种形态,包括球晶、多面体和方形片状。通过X射线衍射(XRD)研究确定了生长材料的性质。傅里叶变换红外光谱(FTIR)研究表明存在七钼酸盐(Mo7O24)和水对称结构,而能量色散X射线分析(EDAX)确定生长晶体的化学计量式为GdCaMo7O24·8H2O。使用热分析技术研究了热行为,这些技术包括热重分析(TG)、差示热分析(DTA)和差示扫描量热法(DSC)。基于TG的模型(即Horowitz-Metzger、Coats-Redfern和Piloyan-Novikova)应用所获得的结果表明,收缩圆柱模型是该材料热分解的相关模型。还使用这三种模型计算了动力学参数,即反应级数(n)、活化能(E a )、频率因子(Z)和熵(ΔS∗)。