A series of highly dispersed bimetallic and bifunctional catalysts Pt@M-MCM-41 (M = Ni, Co) were prepared successfully by in situ synthesis combined with a coprecipitation method. In the catalysts, the transition metal ions were incorporated into the MCM-41 framework and highly dispersed in tetrahedral coordination by in situ thermal crystallization using ammonia as the ligand. The platinum components were highly dispersed in the inner of the M-MCM-41 (M = Ni, Co) matrix via coprecipitation in alkaline condition. These catalysts possess good performance for hydrocracking of residual oil.