The invention provides a preparation method of molybdenum boride powder. In the preparation steps, the molybdenum boride powder which completely accords with material design phase compositions can be controlled to be prepared by means of a high-temperature and high-pressure synthesis mode according to setting of the B/Mo mole ratio n (n=0.5, 1, 2, 2.5, 4) before synthesis, controllable synthesis of target molybdenum boride material phase compositions is achieved, and the synthesized molybdenum boride powder is uniform in particle size, complete in grain crystallization and excellent in property. The method is controllable in technological process, short in technological route, high in targeted property, convenient to operate, efficient, economical in energy, safe and good in reliability. The finished molybdenum boride powder is uniform in particle size distribution and complete in grain crystallization, the chemical purity is higher than or equal to 99.8%, and the product quality stability is good, the properties are obviously improved compared with a molybdenum boride material synthesized through a conventional method, and therefore the produced molybdenum boride material shows excellent physical and chemical properties in industrial application.