Here we demonstrate for the first time a novel approach based on electrochemical for production of Ni-Al alloy mesoporous powder. It can be elucidated that at first step, Al will be dissolved and is oxidized in a solution. Thus, electrons will be liberated and Ni ions with attraction these liberated electrons will be reduced. In consequence, they will deposit on the Al surface. Morphology and chemical composition of the produced powder was characterized by SEM, EDS and XRD. The processing parameters including time and the solution pH were evaluated using the nitrogen adsorption and desorption isotherms analysis. The obtained results verified that the produced powder contains mesoscale porosities with size about 16–20 nm. The results show that the processing time has no effect on the porosities size. However, changing time from 15 to 45 min increases specific surface area of the powder from 311.3 to 386.8m2/gr respectively. In contrast, increasing time beyond 45min decreases this factor. It was found that the solution pH affects both porosities size and specific surface area of the powder. Highest specific surface area and lowest porosity size is related to pH 4. Decreasing pH below 4 is caused that porosities size increases and consequently specific surface area decreases because of the high hydrogen reduction and therefore the low Ni deposition efficiency.
