Application of an Electrochemical Quartz Crystal Microbalance to the study of electrocatalytic films

The EQCM was used to study the deposition and composition of electrodeposited pure PbO{sub 2} and Bi-doped PbO{sub 2} active toward anodic oxygen-transfer reactions. Within the doped films, Bi is incorporated as Bi{sup +5} in the form of BiO{sub 2}A, where A is ClO{sub 4}{sup {minus}} or NO{sub 3}{sup {minus}}. For deposition of these 2 materials, changes in hydration between the Au oxide and the depositing film resulted in higher mass-to-charge ratios. XRD and XPS were used to study the films; the rutile structure of PbO{sub 2} is retained even with the Bi doping. The EQCM was also used to study the formation and dissolution of Au oxide and preoxide structures formed on the Au substrate electrodes in acidic media. The preoxide structures were AuOH and increased the surface mass. For the formation of stable Au films on quartz wafers, Ti interlayers between Au and quartz was found to be very effective.