Hydrogen is a promising fuel for it is clean, highly abundant and non-toxic, but on-board storage of hydrogen is still a challenge. So it is imperative to have an efficient method of hydrogen storage. The mesoporous MCM-48 especially the nickel-containing MCM-48 has great potential in hydrogen storage. MCM- 48 was prepared by hydrothermal synthesis. Then electroless plating technology was used to deposit Ni on the surface of MCM-48 under ultrasonic environment. Powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and N2 adsorption-desorption were employed to investigate the pore structure properties. The results showed that all the samples had Ia3d cubic structure and pore channels were highly ordered. Hydrogen adsorption studies showed that the MCM-48 after nickel plating adsorbed nearly twice the amount of hydrogen than pure MCM-48 at 2.0 MPa, 263 K. So we believe that a small amount of Ni can improve the capacity of hydrogen adsorption of MCM-48 efficiently.