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通过同步热分析和拉曼光谱研究监测有机-无机化合物[(C3H7)4N][SnCl5(H2O)]·2H2O的脱水过程。

Monitoring dehydration of the organic-inorganic [(C3H7)4N][SnCl5(H2O)]·2H2O compound using simultaneous thermal and Raman studies.

作者信息

Hajlaoui S, Chaabane I, Guidara K, Bulou A

机构信息

Unité de recherche de la matière condensée, Faculté des Sciences de Sfax, Université de Sfax, BP 1171, 3000 Sfax, Tunisia.

Unité de recherche de la matière condensée, Faculté des Sciences de Sfax, Université de Sfax, BP 1171, 3000 Sfax, Tunisia.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2016 Jul 5;164:43-51. doi: 10.1016/j.saa.2016.03.027. Epub 2016 Mar 31.

Abstract

In this work we report the experimental studies of the structural phase transition in the [(C3H7)4N]SnCl5(H2O)]·2H2O compound by differential scanning calorimetric (DSC) and Raman spectroscopic. The X-ray powder diffraction study of the [(C3H7)4N][SnCl5(H2O)]·2H2O sample at room temperature showed that this compound is monoclinic and has P121/c1 space group. Differential scanning calorimetric disclosed two types of phase transitions in the temperature range 356-376 (T1) K and at 393K (T2) characterized, by a loss of water molecules and probably a reconstruction of new anionic parts after T2 transition. The Raman scattering spectra recorded at various temperatures in the wavenumber range from 100 to 3800cm(-1) covering the domains of existence of changes in the vicinity of the two phase transitions detected by DSC measurement. A detailed study of the spectral parameters (wave number, reduced intensity and the full width at half maximum) as a function of temperature of a chosen band, associated with (νs(SnO)+νs(SnCl)), based on an order-disorder model allowed us to obtain information relative to the activation energy and correlation length.

摘要

在本工作中,我们报道了通过差示扫描量热法(DSC)和拉曼光谱对[(C3H7)4N]SnCl5(H2O)]·2H2O化合物结构相变的实验研究。[(C3H7)4N][SnCl5(H2O)]·2H2O样品在室温下的X射线粉末衍射研究表明,该化合物为单斜晶系,具有P121/c1空间群。差示扫描量热法揭示了在356 - 376(T1)K温度范围内和393K(T2)时的两种相变类型,其特征是水分子的损失,并且在T2转变后可能会重建新的阴离子部分。在100至3800cm(-1)波数范围内于不同温度下记录的拉曼散射光谱覆盖了通过DSC测量检测到的两个相变附近存在变化的区域。基于有序 - 无序模型,对与(νs(SnO)+νs(SnCl))相关的选定谱带的光谱参数(波数、归一化强度和半高宽)作为温度的函数进行详细研究,使我们能够获得有关活化能和相关长度的信息。

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