We demonstrate, for the first time, the use of electrochemical imaging to identify defect and defect free areas in single crystal boron doped diamond (BDD) electrodes. Specifically, we show that defects contain different boron dopant concentrations than the surrounding single crystal matrix and that these variations can be visualized using intermittent contact−scanning electrochemical microscopy (IC‐SECM). The measured IC‐SECM tip currents provide quantitative information on the rates of electron transfer across the single crystal BDD electrodes, which correlate with variations in boron doping levels. In some instances, IC‐SECM outperforms alternative methods such as Raman microscopy and cathodoluminescence imaging, due to its intrinsic surface‐sensitivity, expanding the application and impact of electrochemical microscopy for materials characterization. The results obtained, and procedure outlined, are particularly valuable for the assessment and screening of single crystal BDD electrodes.
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