Holzinger Angelika, Neusser Gregor, Austen Benjamin J J, Gamero-Quijano Alonso, Herzog Grégoire, Arrigan Damien W M, Ziegler Andreas, Walther Paul, Kranz Christine
Institute of Analytical and Bioanalytical Chemistry, Ulm University, Albert-Einstein-Allee 11, 89081 Ulm, Germany.
Faraday Discuss. 2018 Oct 1;210(0):113-130. doi: 10.1039/c8fd00019k.
The investigation of electrochemical processes at the interface of two immiscible electrolyte solutions (ITIES) is of great interest for sensing applications, and serves as a surrogate to the study of biological transport phenomena, e.g. ion channels. Alongside e-beam lithography, focused ion beam (FIB) milling is an attractive method to prototype and fabricate nanopore arrays that support nanoITIES. Within this contribution, we explore the capability of FIB/scanning electron microscopy (SEM) tomography to visualize the actual pore structure and interfaces at silica-modified nanoporous membranes. The nanopores were also characterized by atomic force microscopy (AFM) using ultra-sharp AFM probes to determine the pore diameter, and using scanning transmission electron microscopy (STEM) and energy dispersive X-ray (EDX) spectroscopy, providing additional information on the elemental composition of deposits within the pores. Si-rich particles could be identified within the pores as well as at the orifice that had faced the organic electrolyte solution during electrochemical deposition. The prospects of the used techniques for investigating the interface at or within FIB-milled nanopores will be discussed.
对两种不混溶电解质溶液（ITIES）界面处的电化学过程进行研究，在传感应用方面具有重大意义，并且可作为研究生物传输现象（如离子通道）的替代方法。除了电子束光刻技术，聚焦离子束（FIB）铣削是一种用于制作和制造支持纳米ITIES的纳米孔阵列的有吸引力的方法。在本论文中，我们探索了FIB/扫描电子显微镜（SEM）断层扫描技术可视化二氧化硅改性纳米多孔膜实际孔结构和界面的能力。还使用超尖锐原子力显微镜（AFM）探针通过原子力显微镜（AFM）对纳米孔进行表征以确定孔径，并使用扫描透射电子显微镜（STEM）和能量色散X射线（EDX）光谱，提供有关孔内沉积物元素组成的更多信息。在孔内以及在电化学沉积过程中面对有机电解质溶液的孔口处都可以识别出富含硅的颗粒。将讨论所使用的技术在研究FIB铣削纳米孔处或内部界面方面的前景。
