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高氯酸2-甲基苯并咪唑鎓新型半有机晶体的晶体结构、拉曼光谱、傅里叶变换红外光谱、紫外-可见吸收光谱、光致发光光谱、热重-差示扫描量热法及介电性能

Crystal Structure, Raman, FTIR, UV-Vis Absorption, Photoluminescence Spectroscopy, TG-DSC and Dielectric Properties of New Semiorganic Crystals of 2-Methylbenzimidazolium Perchlorate.

作者信息

Balashova Elena, Zolotarev Andrey, Levin Aleksandr A, Davydov Valery, Pavlov Sergey, Smirnov Alexander, Starukhin Anatoly, Krichevtsov Boris, Zhang Hongjun, Li Fangzhe, Luo Huijiadai, Ke Hua

机构信息

Ioffe Institute, Politechnicheskaya 26, 194021 Saint Petersburg, Russia.

Institute of Earth Sciences, Saint Petersburg State University, Universitetskaya Nab. 7/9, 199034 Saint Petersburg, Russia.

出版信息

Materials (Basel). 2023 Feb 28;16(5):1994. doi: 10.3390/ma16051994.

DOI:10.3390/ma16051994
PMID:36903111
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC10004103/
Abstract

Single crystals of 2-methylbenzimidazolium perchlorate were prepared for the first time with a slow evaporation method from an aqueous solution of a mixture of 2-methylbenzimidazole (MBI) crystals and perchloric acid HClO. The crystal structure was determined by single crystal X-ray diffraction (XRD) and confirmed by XRD of powder. Angle-resolved polarized Raman and Fourier-transform infrared (FTIR) absorption spectra of crystals consist of lines caused by molecular vibrations in MBI molecule and ClO tetrahedron in the region = 200-3500 cm and lattice vibrations in the region of 0-200 cm. Both XRD and Raman spectroscopy show a protonation of MBI molecule in the crystal. An analysis of ultraviolet-visible (UV-Vis) absorption spectra gives an estimation of an optical gap ~3.9 eV in the crystals studied. Photoluminescence spectra of MBI-perchlorate crystals consist of a number of overlapping bands with the main maximum at ≅ 2.0 eV. Thermogravimetry-differential scanning calorimetry (TG-DSC) revealed the presence of two first-order phase transitions with different temperature hysteresis at temperatures above room temperature. The higher temperature transition corresponds to the melting temperature. Both phase transitions are accompanied by a strong increase in the permittivity and conductivity, especially during melting, which is similar to the effect of an ionic liquid.

摘要

首次采用缓慢蒸发法，从2-甲基苯并咪唑（MBI）晶体与高氯酸HClO的混合水溶液中制备出高氯酸2-甲基苯并咪唑单晶。通过单晶X射线衍射（XRD）确定晶体结构，并通过粉末XRD进行确认。晶体的角分辨偏振拉曼光谱和傅里叶变换红外（FTIR）吸收光谱由200 - 3500 cm区域内MBI分子和ClO四面体中的分子振动产生的谱线以及0 - 200 cm区域内的晶格振动组成。XRD和拉曼光谱均表明晶体中MBI分子发生了质子化。对紫外可见（UV - Vis）吸收光谱的分析给出了所研究晶体中约3.9 eV的光学带隙估计值。MBI - 高氯酸盐晶体的光致发光光谱由多个重叠带组成，主峰最大值在≅2.0 eV处。热重 - 差示扫描量热法（TG - DSC）表明在室温以上温度存在两个具有不同温度滞后的一级相变。较高温度的转变对应于熔化温度。两个相变都伴随着介电常数和电导率的强烈增加，尤其是在熔化过程中，这类似于离子液体的效应。

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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/456b444f7a7a/materials-16-01994-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/d8145f778291/materials-16-01994-g011.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/e80786e9c35c/materials-16-01994-g012.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/47b8de5ca9a4/materials-16-01994-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/4f6a41ddbafb/materials-16-01994-g002.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/18f2390743ab/materials-16-01994-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/057f3a8face7/materials-16-01994-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/7f8c4e4c836e/materials-16-01994-g006a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/102799ed583e/materials-16-01994-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/3531723bebe6/materials-16-01994-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/ddda92a1db5b/materials-16-01994-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/456b444f7a7a/materials-16-01994-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/d8145f778291/materials-16-01994-g011.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/77ca/10004103/e80786e9c35c/materials-16-01994-g012.jpg

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