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Ni, W, Mo and C catalysts were mixed and mechanically processed at room temperature for different grinding times: 0, 40, 80, 120, 160, 200 and 240h. The phases at every stage of milling were studied by X-ray diffraction (XRD). The powders were used in the catalytic aquathermolysis reaction of heavy oil. X-RD showed by increasing the milling time from 0 to 240h, nanostructured carbide phases were synthesized...