Abstract We introduce a new method for the synthesis of Al-Ni nanosized particles. After partial oxidation, this technique is able to produce ultrafine sub-nanometric nickel clusters dispersed with an amorphous aluminium oxide. Such clusters consist of about 15 nickel atoms which exhibit discrete electronic energy levels and superparamagnetism. A very significant enhancement of the catalytic properties is observed. We expect that division of metals down to such a reduced scale will lead us to new properties and to a technological breakthrough since upscaling this method to industrial production rate is straightforward.