Development of in-situ analysis system for molecular layrs on solid surface solution.

由于对溶液中固体表面分子层的观察和分析是通过各种技术分开进行的，因此很难准确地捕捉到分子层的结构/取向的真实图像。在这项研究中，结合多种技术开发了新的分析系统。细节是一样的。现场FT-IR-石英晶体微天平组合系统。购买了一台新的FT-IR仪器，设计并制作了一种以QCM为电极的新型电化学红外电池。在FT-IR测量过程中，即使当电极被压在电池CaF_2窗口上时，该电池也可以进行QCM测量。使用该系统，可以同时监测在不同条件下制备的自组装单分子膜在电极电位作用下的界面质量和结构的变化。原位UV/Vis-Quartz晶体微天平组合系统采用QCM上沉积的10-50 nm真空薄金属层作为电极，置于UV/Vis光谱仪的光路中，可以同时测量电化学反应过程中的UV/Vis光谱和质量变化。将该体系应用于紫精和普鲁士蓝的氧化还原实验，验证了该体系的有效性。STM/AFM-石英晶体微天平组合系统对STM和AFM系统进行了改进，使其可以在STM/AFM成像过程中同时记录QCM的频率。STM/AFM图像与频率图像的比较表明，针尖-衬底的相互作用引起了应力，导致了频率的变化。

Since observation and analysis of molecular layrs on solid surface in solution have been carried out separately by various techniques, it is rather difficult to capture real pictures of structure/orientation of molecular layrs accurately. In this study, new analysis systems which combine many techniques are developed. The detail is as fellows.1. In-situ FT-IR-Quartz Crystal Microbalance Combined System.A new FT-IR machine was purchased and a novel electrochemical IR cell which employs QCM as an electrode was designed and constructed. This cell permits QCM measurement possible even when the electrode was pressed against cell CaF_2 window during FT-IR measurement.Using this system, simultaneous monitoring of changes of interfacial mass and structure of self-assembled monolayr prepared under various conditions during application of electrodes potential was carried out.2. In-situ UV/VIS-Quartz Crystal Microbalance Combined System.Very thin metal layr (10-50nm) vacuum deposited on QCM was employed as an electrode.This electrode was placed in light path of UV/VIS spectrometer so that UV/VIS spectra and mass change can be measured simultaneously during electrochemical reactions. The effectiveness of this system was demonstrated for redox of viologen and Prussian blue.3. STM/AFM-Quartz Crystal Microbalance Combined System.STM and AFM systems were modified so that frequency of the QCM can be recorded simultaneously during STM/AFM imaging. The comparison between STM/AFM image and frequency image shows that the tip-substrate interaction causes the stress, resulting frequency change.