Kaolinic and bentonitic-clays are selected to prepare transition metals, iron, cobalt and nickel catalysts. The metals are incorporated into two supports through new impregnation technique. The original clays and the prepared catalysts were subjected to different techniques. The crystallite size (X-ray diffraction analysis) increases from iron to cobalt then to nickel upon heating and the increase for bentonitic-catalysts is higher than that for kaolinic-ones. Infrared spectra show the appearance of bands signifying the presence of iron, cobalt and nickel bonded to OH group constituting the silica-silica tetrahedral sheets inside the clay structure. The enthalpy (ΔH) andentropy (ΔS) values (differential scanning calorimetric) are lower for bentonitic-catalysts than for kaolinic-catalysts. Thus, the incorporation of the metal hydroxide in the interlamella of the silicate-silicate bentonite clay structure facilitates the interaction between the unpaired electrons on the adjacent atoms and the support which enables the prepared catalysts to be more active for catalytic conversion.