Research has been carried out on variations in calcination temperature on ZnO and ZnO/Mopl-CTAB characters in degrading methyl orange (MO). This study aimed to determine the effect of calcination temperature on the character of ZnO and ZnO/Mopl-CTAB and to determine the effect in degrading methyl orange. This research was carried out by synthesizing ZnO and ZnO/Mopl-CTAB materials by varying the calcination temperature in the final process, namely at temperatures of 150, 250, 350 and 450 °C. The solid material powder obtained was characterized using SEM EDX, BET, FTIR, XRD, and DR-UV. Based on the characterization results, the greater the calcination temperature can affect the characteristics of the photocatalyst material including morphology, functional groups, crystal structure, crystal lattice, crystallinity, surface area, pore size, pore volume and bandgap energy. The results of the photodegradation activity test in degrading MO proved that the best or optimum material for use in MO degradation in bright conditions was ZnO/Mopl-CTAB with a calcination temperature of 450 that resulted in the most optimum % removal at 50 minutes of 78% while ZnO was only 53 % in the 40th minute. In the dark conditions the best material was ZnO/Mopl-CTAB with a calcination temperature of 150 that was 52% in the 50th minute while the optimum condition for ZnO occurred at the 450 °C calcination temperature treatment that was 31% in the 50th minute 40. The kinetics of reactions that occur in both dark and light conditions followed the pseudo-second order reaction kinetics model.