Department of Chemistry, School of Science, The University of Tokyo , 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033, Japan.
Graduate School of Engineering Science, Osaka University , 1-3 Machikaneyama, Toyonaka, Osaka, 560-8531, Japan.
Langmuir. 2016 Jul 12;32(27):6825-9. doi: 10.1021/acs.langmuir.6b01370. Epub 2016 Jul 1.
Microstructured electrodes are significant to modern electrochemistry. A representative aromatic group, 4-ferrocenylphenyl one, was covalently bound to a micropatterned silicon electrode via the arylation of a hydrogen-terminated silicon(111) surface formed selectively on a Si wafer. Starting from a silicon(100)-on-insulator (SOI) wafer, the aromatic monolayer was attached sequentially by spin-coating a resist, electron beam lithography, Cr/Au deposition, lift-off, anisotropic etching with aqueous KOH solution, and Pd-catalyzed arylation. Cyclic voltammetry (CV) and X-ray photoelectron spectroscopy (XPS) are used to characterize the coupling reaction between 4-ferrocenyl group and silicon substrate, and to confirm performance of the final modified microsized electrode. These data show that this synthetic protocol gives chemically well-defined and robust functionalized monolayers on a silicon semiconducting surface with a small electrode.
微结构化电极对现代电化学具有重要意义。通过对在硅片上选择性形成的氢终止硅(111)表面的芳基化反应,将代表性的芳基基团之一,4-二茂铁基苯基,共价键合到微图案化的硅电极上。从硅(100)-在绝缘体(SOI)晶片开始,通过旋涂抗蚀剂、电子束光刻、Cr/Au 沉积、剥离、用氢氧化钾溶液各向异性蚀刻以及钯催化芳基化反应,依次附着芳族单层。循环伏安法(CV)和 X 射线光电子能谱(XPS)用于表征 4-二茂铁基与硅基底之间的偶联反应,并确认最终修饰的微尺寸电极的性能。这些数据表明,该合成方案在具有小电极的硅半导体表面上提供了化学定义明确且稳定的功能化单层。