Electrospun Ni and Cu metal oxide catalysts are successfully synthesized through electrospinning and conventional sol-gel methods to show advantages of electrospinning on catalytic performance in ammonia borane (NH3BH3) methanolysis for hydrogen production. An experimental assessment is presented by the characterization of interior and exterior properties of all catalysts and their catalytic activity towards NH3BH3 methanolysis. The systematic studies are performed in order to figure out of kinetic interpretation. Catalytic NH3BH3 methanolysis reactions are carried out at different catalyst amounts (5-15 mg), initial NH3BH3 concentrations (0.36-6.0 M) and temperatures (20-50 degrees C). Thanks to the higher pore volume/S BET ratio, fiber type nanostructured Cu oxide catalyst exhibits the highest catalytic activity compared with sol-gel prepared ones. The results of kinetic studies show that the fiber type Cu oxide catalyst catalyzed methanolysis of NH3BH3 and follows the first order reaction kinetic model with 35 kJ mol(-1) activation energy value. (C) 2019 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.