Abstract
Cathodic electrodeposition of oxides on platinum from MoO3–K2MoO4 (3.85–75 mol% MoO3) under DC and pulsed galvanostatic modes is discussed in combination with voltammetry data. Characteristic potential values (as related to oxygen evolution onset) are reported for Mo(VI/IV) redox processes, as well as for electrochemical equilibria with participation of molybdenum metal and Pt–Mo alloys. On the basis of scan rate effects and results for various potential limits, and also of voltammetry with preliminary potentiostatic accumulation of products, molybdate reduction mechanism complicated by a chemical step of Mo metal oxidation is proposed. This qualitative assumption is verified in preparative electrolysis experiments with products identification by means of X-ray diffractometry, scanning electron microscopy, and EDX local analysis. Deposition under pulsed mode is found to be useful tool to adjust the duration of chemical step and by these means to alter the composition of final products. The conditions supporting the formation of MoO2 and more reduced oxides are formulated.
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