Operando analysis of the electrosynthesis of Ag2O nanocubes by scanning electrochemical microscopy

The strategy proposed herein employs the scanning electrochemical microscope in a generation collection like mode to depict mechanism implied electrosynthesis of metal oxides nanoparticles, NPs. It offers simultaneous NPs precursors and single NP-level electroanalysis by nanoimpact coulometry. former process is operated under controlled fluxes within wide field precursor diffusion inter-MEs gap thus forming tunable reaction layer allowing growth size gradient this gap. latter exploits much slower NPs, spatially frozen, near collecting microelectrode. then allows dynamically situ monitor modes without perturbing their synthesis. As proof concept, synthesis Ag 2 O nanocubes, NCs, described, using an microelectrode generate + ions while facing Au both electrogenerates HOand collect as-synthetized NCs. dynamic analysis NCs reductive impacts, getting insights stability. Particularly it suggests two steps starting from quasi-instantaneous nucleation >260 nm nucleus followed mass-transfer driven crystallization over nuclei.