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Updated: Jun 16, 2025
Exfoliation and Analysis of Large-area, Air-Sensitive Two-Dimensional Materials
Published on: January 5, 2019
Optically Transparent Carbon-Silicon Nitride Windows for Correlative Structural and Electrochemical Analysis of
Sasha E Alden1, Oluwasegun J Wahab1, Lingjie Zhang1
1Department of Chemistry, Texas A&M University, College Station, Texas 77843, United States.
Abstract:
We report an optically transparent carbon electrode-silicon nitride (OTCE-SiNx) window platform fabricated through clean-room microfabrication techniques. A wafer-scale fabrication process was implemented, which enabled a batch preparation of 2925 windows (100 × 100 μm) in user-friendly configurations. Application of OTCE-SiNx windows is demonstrated in the high-resolution structural and nanoscale electrochemical characterization of nanocrystals by transmission electron microscopy (TEM) and electrochemical scanning probe microscopy. High-resolution TEM (HR-TEM) and aberration-corrected high-angle annular dark-field TEM (HAADF-TEM) were achieved for nanocrystals supported on the OTCE-SiNx, with minimal background electron scattering or interference from the OTCE-SiNx. Additionally, the stability of OTCE-SiNx under prolonged voltammetric cycling was investigated. Scanning electrochemical cell microscopy (SECCM) revealed uniform nanoscale electrochemistry. Correlative electrochemical and electron microscopy on OTCE-SiNx was demonstrated for the hydrogen evolution reaction (HER) at clusters of sub-10 nm Au nanospheres.
