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In this paper, we describe the modification of Nanoscale Impedance Microscopy(NIM), namely, a combination of contact-mode atomic force microscopy with localimpedance measurements. The postulated approach is based on the application ofmultifrequency voltage perturbation instead of standard frequency-by-frequencyanalysis, which among others offers more time-efficient and accuratedetermination of the resultant impedance spectra with high spatial resolution.Based on the impedance spectra analysis with an appropriate electric equivalentcircuit, it was possible to map surface resistance and contact capacitance.Polycrystalline heavy boron-doped diamond (BDD) electrodes were the researchobject. Recent studies have shown that the exposure of such electrodes tooxidizing environment may result in the modification of termination type, andthus it is a key factor in describing the electric and electrochemicalproperties of BDD. We have successfully applied multifrequency NIM, whichallowed us to prove that the modification of termination type is selective andoccurs with different propensity on the grains having specific crystallographicorientation. Furthermore, our approach enabled the detection of even subtlesubmicroscopic surface heterogeneities, created as a result of variousoxidation treatments and to distinguish them from the surface heterogeneityrelated to the local distribution of boron at the grain boundaries.

Multifrequency Nanoscale Impedance Microscopy (m-NIM): A novel approach  towards detection of selective and subtle modifications on the surface of  polycrystalline boron-doped diamond electrodes