The invention provides a preparation method of Ce-Co-S-P nanocrystals. The method comprises the following steps: mixing ceric ammonium nitrate, cobalt acetylacetonate, oleic acid, n-dodecanethiol and tri-n-octylphosphine, heating to 320 DEG C, carrying out heat preservation reaction, and carrying out dispersion sedimentation and centrifugal separation on the obtained product to obtain the Ce-Co-S-P nanocrystals. The Ce-Co-S-P nanocrystals prepared in the invention have excellent OER performance, and can efficiently catalyze OER in a fuel cell. A one-pot method is adopted, Ce is used for effectively adjusting the phase change of Co-S-P nanosheets, meanwhile, the catalytic performance is adjusted, the process is simple, the reaction temperature is low, the reaction time is short, the method is suitable for batch production, and the method has important guiding significance on renewable energy technology development.