An investigation has been made of the properties of lead dioxide electro‐deposited from dilute solutions made alkaline with , i.e., under conditions which were expected to produce . The apparent coulombic efficiency, measured gravimetrically, is strongly dependent on both the pH and the lead (biplumbite) ion concentration. Efficiency values encountered in this study ranged as high as 115%. A detailed composition analysis has been made on a material deposited from solution at an apparent coulombic efficiency of 112%. Analyses for water, lead, and active oxygen lead to the empirical composition Si is the major trace contaminant, as measured by emission spectrography, but it is not present to the extent that silicate need be considered as an integral part of the electrodeposited compound. Quantitative analysis shows that nitrate is not an inclusion. Electron photomicrographs reveal a uniform finegrained structure in which the crystal faces and boundaries are slightly curved. X‐ray diffraction analysis gives an pattern. This is the same pattern reported in the literature for , prepared by chemical methods. The real coulombic efficiency of plating, recalculated on the basis of the analysis for composition, is 98%. The rapid drop in the apparent coulombic efficiency as the pH is increased is suggested to be the result of an approach in the net lead oxidation state to 4.00.
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