Ce 2 (MoO 4 ) 3 was prepared using dielectric barrier discharge (DBD) plasma method, co-precipitation method and hydrothermal method, respectively, with water/ethanol (W/O) as solvent, oleylamine (OAm) and oleic acid (OAc) as additives. Preparation method showed significant influence on the morphological and structural properties, as well as photocatalytic performance. Ce 2 (MoO 4 ) 3 synthesized with DBD plasma (MO-P) was mainly flowerlike nanosheets, which were beneficial to promoting electron transfer and providing more space for catalytic activity. Also, MO-P samples exhibited more oxygen vacancies, which were conducive to the photocatalytic performance. What's more, MO-P showed lower PL intensity and narrow energygap, which implied a slow photoelectron-hole pair recombination rate and an increased electron transfer rate. The degradation rate of methyl orange (50 mg/L) could achieve 98% within 12 min with 0.5 g/L MO-P. Hydroxyl radicals (•OH) and superoxide radicals (•O 2 − ) played a major effect. Plasma synthesis method exhibited potential application prospect in photocatalysts preparation.