A plasma treatment of Co-W-B catalyst increases the rate of hydrogen generation from the hydrolysis of NaBH4. The catalytic properties of Co-W-B prepared in the presence of plasma have been investigated as a function of NaBH4 concentration, NaOH concentration, temperature, plasma applying time, catalyst amount and plasma gases. The Co-W-B catalyst prepared with cold plasma effect hydrolysis in only 12 min, where as the Co-W-B catalyst prepared in known method with no plasma treatment in 23 min. The activation energy for first-order reaction is found to be 29.12 kJ mol(-1). Copyright (C) 2013, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.