Lead dioxide is the active constituent of the positive electrode in the lead‐acid battery. Both the α‐ and the β‐modifications are present in battery electrodes and X‐ray diffraction techniques must be used to differentiate the role of each in the reactions occurring in the lead‐acid battery system. Standard samples of the two forms of lead dioxide are necessary for this purpose, and samples prepared by various methods have been studied. Powder patterns of electrodeposited samples of both α‐ and β‐lead dioxide showed preferred orientation effects which could not be removed by grinding. Chemically prepared samples of the two forms were well crystallised and did not produce preferred orientation effects. α‐Lead dioxide prepared by the oxidation of yellow lead monoxide (using a fused mixture of sodium chlorate and sodium nitrate) and β‐lead dioxide prepared by hydrolysis of lead tetra‐acetate were chosen as standard samples for X‐ray studies and their diffraction patterns have been recorded. A mechanism of nucleation has been proposed for the formation of α‐lead dioxide in alkaline and neutral media, and the β‐form in acid media.
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