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通过在向列相和近晶 C 相中的 13C NMR 对三环介晶的相特征和分子有序性进行研究。

Phase characterization and study of molecular order of a three-ring mesogen by 13C NMR in smectic C and nematic phases.

机构信息

Polymer Laboratory, Central Leather Research Institute (Council of Scientific & Industrial Research, CSIR), Adyar, Chennai 600 020, India.

出版信息

J Phys Chem B. 2011 Oct 13;115(40):11554-65. doi: 10.1021/jp203388v. Epub 2011 Sep 15.

Abstract

Molecules exhibiting a thermotropic liquid-crystalline property have acquired significant importance due to their sensitivity to external stimuli such as temperature, mechanical forces, and electric and magnetic fields. As a result, several novel mesogens have been synthesized by the introduction of various functional groups in the vicinity of the aromatic core as well as in the side chains and their properties have been studied. In the present study, we report three-ring mesogens with hydroxyl groups at one terminal. These mesogens were synthesized by a multistep route, and structural characterization was accomplished by spectral techniques. The mesophase properties were studied by hot-stage optical polarizing microscopy, differential scanning calorimetry, and small-angle X-ray scattering. An enantiotropic nematic phase was noticed for lower homologues, while an additional smectic C phase was found for higher homologues. Solid-state high-resolution natural abundance (13)C NMR studies of a typical mesogen in the solid phase and in the mesophases have been carried out. The (13)C NMR spectrum of the mesogen in the smectic C and nematic phases indicated spontaneous alignment of the molecule in the magnetic field. By utilizing the two-dimensional separated local field (SLF) NMR experiment known as SAMPI4, (13)C-(1)H dipolar couplings have been obtained, which were utilized to determine the orientational order parameters of the mesogen.

摘要

由于其对温度、机械力以及电场和磁场等外部刺激的敏感性,表现出热致液晶性质的分子因其重要性而受到关注。因此,通过在芳核附近以及侧链中引入各种官能团,已经合成了几种新型介晶,并对其性能进行了研究。在本研究中,我们报告了具有一个末端羟基的三环介晶。这些介晶通过多步合成路线合成,并通过光谱技术完成了结构表征。通过热台偏光显微镜、差示扫描量热法和小角 X 射线散射研究了介相性质。对于较低同系物,观察到各向同性向列相,而对于较高同系物,还发现了额外的近晶 C 相。对典型介晶在固态和介相中的固态高分辨率天然丰度(13)C NMR 研究进行了研究。在近晶 C 和向列相中的介晶的(13)C NMR 谱表明分子在磁场中自发排列。通过利用称为 SAMPI4 的二维分离局部场(SLF)NMR 实验,获得了(13)C-(1)H 偶极耦合,利用该偶极耦合可以确定介晶的取向有序参数。

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