Titanium oxide nano tubes (TiOx) were prepared by the electrochemical anodizing method from at different process time and different potential in 0.1 M HF solution. Their morphologies were determined with surface photographs and scanning electron microscopy (SEM) images. Ni nano particles were deposited in conductive TiOx nano tubes arrays via pulsed electrodeposition method. Their catalytic activity towards the hydrogen evolution reaction (HER) was assessed by recording cyclic voltammetry technique, cathodic current potential curves, hydrogen gas volumes and electrochemical impedance spectroscopy techniques. The highest HER activity thought the studied is observed on the TiOx((30))-Ni. Copyright (C) 2012, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.