In this study, the hydrogen generation from the hydrolysis of NaBH4 with Ni (o) catalyst prepared in the presence of plasma is investigated. The catalytic properties of nickel catalyst prepared in the presence of plasma are investigated based on NaBH4 concentration, NaOH concentration, temperature, plasma applying time and plasma applying voltage. The results indicated that nickel catalyst reduced with plasma was completed in only 35 min, while the nickel catalyst produced in known method is completed in 80 min. Characteristics of this nickel-based catalyst are carried out by using XRD, BET, SEM and XPS. The activation energy for zero-order is found to be 51.35 kJ mol(-1). (C) 2013 Elsevier B.V. All rights reserved.