Hydrogen is an alternative and clean energy carrier, but there are still some production related problems. In this aspect, it is crucial to efficiently generate hydrogen from hydrogen rich materials such as sodium borohydride. In this study, Co3O4 supported Ni and Co catalysts are synthesized via microwave irradiation technique for hydrogen generation from sodium borohydride. In this context, firstly, Co3O4 support material is synthesized by chemical method. Then, Ni and Co catalysts are decorated onto Co3O4 support material by microwave irradiation-polyol method. Prepared catalysts and support material are characterized by using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma-mass spectrometer (ICP/MS). A new system is designed by our group in order to determine the activity of the prepared catalysts for hydrogen generation. The effects of different initial NaOH concentrations on hydrogen generation rate are investigated. It is observed that the rate of hydrogen generation increased with an increase in initial NaOH concentration. Co-Co3O4 catalyst at 10% NaOH initial concentration shows the highest hydrogen generation rate as 2823 ml/g(cat).min. In summary, Co-based catalysts are exhibited more activity than Ni-based catalysts in terms of hydrogen generation. (C) 2018 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.