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The nano-sized ZrO2 reinforced Mo alloys were prepared by hydrothermal synthesis and subsequent sintering. During preparation, the nano-sized ZrO2 particles were added into the Mo powder via hydrothermal synthesis. This work investigated the differences in mechanical properties and microstructures of the Mo-ZrO2 alloys prepared by hydrothermal synthesis and the other traditional method. As the amount of ZrO2 particles increased, the grain size of the Mo powders reduced obviously. The grains were refined obviously after sintering. The ZrO2 particles added by hydrothermal synthesis can effectively restrain the growth of grains and improve mechanical properties such as strength and hardness.