Molybdenum splats usually exhibit splitting morphology onto aluminum and stainless steel substrates due to substrate melting and their own high surface tension using plasma spraying. In this study, Mo particles were sprayed onto different substrates, which were treated by dry-ice blasting combined with substrate preheating. The splats were studied using detailed microstructural characterization with an emphasis on the splat shape. Moreover, the corresponding Mo coatings deposited onto different substrates were obtained. The results showed that the splitting splat formed on stainless steel was different from that on the aluminum surface. Dry-ice blasting combined with substrate preheating slightly modify the morphology of Mo splat sprayed on aluminum and stainless steel surfaces.