Localized Electrosynthesis and Subsequent Electrochemical Mapping of Catalytically Active Metal–Organic Frameworks

In recent years, metal–organic frameworks (MOFs) have shown great potential to be used as porous, high surface area catalytic materials capable of driving electrochemical energy conversion reactions. However, further improvement in their electrocatalytic performance necessitates methods to couple high-throughput MOF synthesis and their subsequent electrochemical activity characterization. In this work, scanning electrochemical microscopy (SECM) is employed to perform a localized, micron-scale electrosynthesis of two types of MOFs, Al₂(OH)₂-TCPP, and HKUST-1. SECM is also utilized to analyze the electrocatalytic hydrogen evolution reaction activity of the as-prepared MOF micropatterns, via i) substrate-generation tip-collection mode to map the MOF's electrochemical reactivity, and ii) redox competition mode, to accurately extract the MOF's catalytic onset potential. Thus, the presented method provides a means to shed light on the operation principles of electroactive MOFs, toward their future incorporation in alternative fuel-production schemes.