Cobalt hexacyanoferrate (CoHCF) nanoparticles have been synthesized by mixing aqueous solutions of K3Fe(CN)6 and CoCl2 under vigorous stirring at different temperatures and following two different procedures, drop-by-drop or immediate mixing. The resulting CoHCF nanoparticles, with dimensions of several tens of nanometers, were characterized using TEM, SEM-EDX, IR, and XRD. Their electrochemical behavior was investigated in comparison with the CoHCF powder bulk compound. The CoHCF nanoparticles exhibit an electrochemically driven conversion to the bulk one that has been investigated by a chemometric approach in order to establish the best synthetic parameters. The rate and the degree of conversion depend on the synthesis temperature.
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