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Spherulitic Crystallization in Langmuir-Blodgett Films of the Ditetradecyldimethylammonium-Au(dmit)2 Salt.
Langmuir ( IF 3.7 ) Pub Date : 2020-01-07 , DOI: 10.1021/acs.langmuir.9b03677 Yasuhiro F Miura 1, 2 , Hironari Akiyama 2 , Naoki Sugimoto 2 , Yoshiya Akagi 1 , Tetsuya Aoyama 3 , Hidenobu Shiroishi 4 , Mitsuo Takahashi 4
Langmuir ( IF 3.7 ) Pub Date : 2020-01-07 , DOI: 10.1021/acs.langmuir.9b03677 Yasuhiro F Miura 1, 2 , Hironari Akiyama 2 , Naoki Sugimoto 2 , Yoshiya Akagi 1 , Tetsuya Aoyama 3 , Hidenobu Shiroishi 4 , Mitsuo Takahashi 4
Affiliation
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Spherulitic crystallization in Langmuir-Blodgett (LB) films of the ditetradecyldimethylammonium-Au(dmit)2 [2C14N+Me2-Au(dmit)2] salt has been characterized by polarized light microscopy, Fourier-transform infrared (FT-IR) spectroscopy, and X-ray diffraction (XRD) analyses. Analyses by differential scanning calorimetry (DSC) for the bulk crystals indicate that annealing in the temperature range of 58-100 °C may be appropriate to improve the order in the LB film. The polarized light microscopy measurement further revealed that a spherulite structure was formed after the film was annealed at 80 °C for 60 min. FT-IR spectroscopy measurements demonstrated that the order of the principal hydrocarbon chains was improved and that the rotation of CH3 groups was hindered by the annealing. Out-of-plane XRD analyses revealed that the d-spacing of the 2C14N+Me2-Au(dmit)2 LB film changed from 3.1 to 2.5 nm upon annealing. We hypothesize that a layered structure with interdigitated hydrocarbon chains, which is equivalent to or close to that of the corresponding bulk crystal, has been realized in the LB film by annealing. We consider that two different kinds of one-dimensional (1D) interactions along the a-axis are the driving forces to realize the spherulite structure in the LB system; one is an extended 1D contact due to the pronounced interdigitation of the alkyl chains of the ammonium ion, which plays a role similar to that of the folding of chains in the lamellar structures of polymers, and the other is a 1D extended sulfur-sulfur contact between Au(dmit)2 dimer pairs. So far, spherulite formation in LB films has been reported almost exclusively for polymerized materials. Here, we demonstrate that a spherulite texture can also be formed in LB films based on nonpolymerized materials via the interdigitation of hydrocarbon chains, leading to a new well-ordered state.
中文翻译：
二十四烷基二甲基铵-Au（dmit）2盐在Langmuir-Blodgett膜中的球晶结晶。
二十四烷基二甲基铵-Au（dmit）2 [2C14N + Me2-Au（dmit）2]盐在Langmuir-Blodgett（LB）膜中的球晶结晶已通过偏振光显微镜，傅立叶变换红外（FT-IR）光谱，和X射线衍射（XRD）分析。通过差示扫描量热法（DSC）对块状晶体的分析表明，在58-100°C的温度范围内进行退火对于改善LB膜的有序性可能是合适的。偏光显微镜的测量还表明，在80℃下将膜退火60分钟后，形成了球晶结构。FT-IR光谱测量表明，主要烃链的顺序得到了改善，并且退火阻碍了CH3基团的旋转。平面外XRD分析显示，退火后2C14N + Me2-Au（dmit）2 LB膜的d间隔从3.1 nm改变为2.5 nm。我们假设通过退火在LB膜中已经实现了具有相互交叉的烃链的层状结构，该层状结构等于或接近相应的块状晶体的层状结构。我们认为，沿a轴的两种不同类型的一维（1D）相互作用是在LB系统中实现球晶结构的驱动力。一个是由于铵离子烷基链的明显相互交叉而产生的一维扩展接触，其作用类似于聚合物的层状结构中链折叠的作用，另一种是一维扩展的硫-硫接触Au（dmit）2二聚体对之间。迄今为止，据报道，LB膜中球晶的形成几乎完全是针对聚合材料。在这里，我们证明了基于非聚合材料的LB膜中也可以通过烃链的相互指状形成球晶织构，从而导致新的有序状态。
更新日期：2020-01-07
中文翻译：
二十四烷基二甲基铵-Au（dmit）2盐在Langmuir-Blodgett膜中的球晶结晶。
二十四烷基二甲基铵-Au（dmit）2 [2C14N + Me2-Au（dmit）2]盐在Langmuir-Blodgett（LB）膜中的球晶结晶已通过偏振光显微镜，傅立叶变换红外（FT-IR）光谱，和X射线衍射（XRD）分析。通过差示扫描量热法（DSC）对块状晶体的分析表明，在58-100°C的温度范围内进行退火对于改善LB膜的有序性可能是合适的。偏光显微镜的测量还表明，在80℃下将膜退火60分钟后，形成了球晶结构。FT-IR光谱测量表明，主要烃链的顺序得到了改善，并且退火阻碍了CH3基团的旋转。平面外XRD分析显示，退火后2C14N + Me2-Au（dmit）2 LB膜的d间隔从3.1 nm改变为2.5 nm。我们假设通过退火在LB膜中已经实现了具有相互交叉的烃链的层状结构，该层状结构等于或接近相应的块状晶体的层状结构。我们认为，沿a轴的两种不同类型的一维（1D）相互作用是在LB系统中实现球晶结构的驱动力。一个是由于铵离子烷基链的明显相互交叉而产生的一维扩展接触，其作用类似于聚合物的层状结构中链折叠的作用，另一种是一维扩展的硫-硫接触Au（dmit）2二聚体对之间。迄今为止，据报道，LB膜中球晶的形成几乎完全是针对聚合材料。在这里，我们证明了基于非聚合材料的LB膜中也可以通过烃链的相互指状形成球晶织构，从而导致新的有序状态。
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