The influence of the calcination procedure on electrocatalytic properties for oxygen evolution at Ti/IrO2 electrodes was investigated by using cyclic voltammetry （CV） and anodic polarization tests. Thermal decomposition at single temperature of 500 ~C for each layer （conventional method） was adopted as the standard procedure. Scanning electron microscopy （SEM）, X-ray diffraction （XRD） and electrochemical impedance spectroscopy （EIS） show the standard procedure leads to compact oxide coatings, with large grain distributing on coatings and high resistance of obtained electrodes. Both applying the lower temperatures in first three under-layers （step-method） and the programming heating in each layer can, to some extent, overcome the disadvantages of the conventional procedure, and thereby improve the electrochemical activities of electrodes. By using the modified procedures, the electrode resistance is found to decrease due to the inhibition of substrate oxidation. When using the controlled programming calcination （heating rate）, the coating becomes more porous and rugged.