The processes of electrochemical deposition of zirconia from nonaqueous electrolytes on different substrates have been investigated. Cyclic voltammetry and linear sweep voltammetry have been used to investigate the oxygen and hydrogen reduction processes preceding/accompanying the discharge of the zirconium complex being identified. On the basis of simultaneous XPS and SEM analyses, the potential region of zirconia layer formation has been defined. The kinetic parameters of successive and parallel reduction processes have been determined. The factors hindering the formation of thick zirconia layers have been discussed.