Bismuth basic nitrates (BBNs) were synthesized via an electrochemical method, i.e., by electrodeposition from an acidic solution of bismuth nitrate, followed by thermal treatment in an air environment. For the first time, the influence of various electrochemical parameters on the morphology, crystal structure, and chemical structure of BBNs was examined. The following synthesis parameters were investigated: electrodeposition current density, thermal treatment temperature of the obtained deposit, and working electrode material (cathode). The obtained materials were characterized by SEM-EDX, XRD, FTIR, TG, and N