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A type of activated carbon that is further chemically activated to obtain a high surface area (~3322m[sup 2]g[sup -1]) (hsAC), is loaded with nickel nanoparticles by a direct hydrothermal method, and tested for hydrogen storage. The chemical composition, crystal structure, and micro structure of hsAC with or without Ni loading are characterised in addition to the nitrogen absorbance isotherms. Hydrogen storage studies showed that metal doping has no effect on the cryogenic storage, and the maximum room temperature (RT) storage capacity through spillover on the Ni-doped hsAC materials achieved 0.79 wt-% at 30 Pa with enhancement factors of 2.93. The smaller catalyst size was a critical factor that determined the enhancement of RT storage capacity of the materials. The Ni catalyst size was controlled by the doped Ni content. Tuning the Ni catalyst size together with an optimum carbon spillover receptor should play an effective role in further enhancement by the spillover effect. [ABSTRACT FROM AUTHOR]