In this study, the parameters on the catalytic hydrolysis of the sodium borohydride (NaBH4, SBH) and ammonia boranes (NH3BH3, AB) mixtures were investigated such as the effect of Zr additive in the catalyst, using in-situ or powder catalysts, the molar ratio of the SBH/AB mixture (2,4, 8, neat SBH ,neat AB) and temperature. As the catalyst, in-situ synthesized Ni-B and Zr-Ni-B for the first time were used to produce H2 from hydrolysis of the SBH and AB mixtures. The SBH and AB mixtures were used to determine provided or not an effect on reaction. Catalyst preparation and hydrolysis reactions took place in the same reactor spontaneously for in-situ works. The Zr-Ni-B catalyst gives better results than Ni-B and increases efficiency at 25 degrees C and 35 degrees C temperature. When Zr-Ni-B catalyst compared experimentally among themselves, the best yield result at 45 degrees C temperature, for neat SBH, mole ratio in 4 and mole ratio in 8, as 87%, 86% and 83% respectively. For hydrolysis reactions with Zr-Ni-B catalyst, activation energies of SBH and AB were calculated as 45.23 kJ/mol and 79.76 kJ/mol, respectively. SEM, BET, XPS analyzes have been used to characterize these catalysts. The addition of Zr provided increase effect on the surface area. The surface area increases from 44.33 m(2)/g to 175.50 m(2)/g. (C) 2021 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.