containing Ni metal from 0% to 12% with nearly monodisperse Ni particles distributed from 9 A˚ to 20 A˚ and having microporous structure with specific surface area from 510 m2/g to 650 m2/g and very high catalytic activity for hydrogenation, were prepared by carbonizing nickel and calcium-doped D152 resins (Ni–Ca/D152) having different nickel loadings by exchang- ing calcium-doped Dl52 resins (Ca/D152) with Ni2+ of different contents in NH3–NHþ solution as well as C2H5OH solution.