The optimum calcination and sintering conditions for the preparation of the desired phases with the proper stoichiometry of the bulk high-temperature superconductors YBa2Cu3O7−x (YBCO) and Bi2Sr2CaCu2Oy (BSCCO) were investigated by differential scanning calorimetry. DSC analysis on the corresponding superconducting coatings, electrophoretically deposited, indicated that the sintering and annealing procedure was suitable for the production of stable, strong and adherent coatings. X-ray diffraction analysis, Raman spectroscopy and magnetic measurements confirmed the improved properties of the superconducting powders and coatings obtained.