Diamond-WC-Co composites is prepared by using the high pressure cubic cell at 5.50 GPa and 1 100~1 500 °C for 2 min, with mass fraction of 5% diamond powder (average grain size 7 μm), 90% WC powder (average grain size 150 nm), 5% Co powder (average grain size 0.9 μm) as the starting materials. The sample characterization is performed through the X-ray diffraction, Raman spectrum, scanning electron microscope and Vickers hardness tester. The synthesized diamond-WC-Co composites has a uniform phase distribution, and the diamond particles are well bonded with the cemented carbide matrix. The sample has the best performance under the thermodynamic conditions of 5.50 GPa and 1 250 ℃ for 2 min, with a relative density of 96% and a Vickers hardness of 23.60 GPa.