It was found that exchanging Ca/D152 with Ni(NH3)Þx (x = 1–6) solution is advantageous to make bead-shaped Ni–Ca/C with low nickel loadings, and exchanging with Ni2+(C2H5OH, H2O) solution is preferable for making bead-shaped Ni–Ca/C having high nickel loadings. The detected intensive interaction between nickel and its sup- port carbon greatly contributes to the very high catalytic activity of the bead-shaped Ni–Ca/C.