In this paper, the molybdenum phosphide (MoP) catalysts (TPR-MoP and TPR-MoP-Pla) were prepared by the traditional method and the RF (radio frequency) thermal plasma technique respectively and characterized by x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS), transmission electron microscope (TEM), hydrogen temperature-programmed desorption (H 2 -TPD) and carbon monoxide temperature-programmed desorption (CO-TPD) measurements, and their catalytic performance for HAS was evaluated. The results showed that the total and C 2+ alcohols selectivity of the catalyst after plasma treatment (TPR-MoP-Pla) were enhanced. The enhanced catalytic performance could be related to more dislocation defects and the synergistic effect between Mo 0-2+ and Mo 4+ valence species in the TPR-MoP-Pla catalyst. In addition, this work suggests that thermal plasma treatment can be used as a new preparation technique for the synthesis of materials with rich species.