Multidimensional shearforce-based constant-distance mode scanning electrochemical microscopy (4D SF/CD-SECM) was utilized for the investigation of the activity distribution of oxygen reduction catalysts. Carbon-supported Pt model catalyst powders have been immobilized in recessed microelectrodes and compared to a spot preparation technique. Microcavities serve as platform for the binder-free catalyst sample preparation exhibiting beneficial properties for constant-distance mode SECM imaging concerning modified surface area and catalyst loading. The integration of the redox competition mode of SECM into the detection scheme of the 4D SF/CD mode is demonstrated for specifically adapting high-resolution SECM experiments to powder-based catalyst preparations.
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Nebel et al. (2014) studied this question.
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