A series of solids was synthesized by the incorporation of Ni and Mo active species on delaminated clay with novel acidic properties, by impregnation and auto-combustion. The resulting solids were characterized by X-ray fluorescence, X-ray diffraction (XRD), textural analysis by N-2 physisorption, temperature-programmed reduction (TPR), transmission electron microscopy (TEM) and, in situ diffuse reflectance infrared Fourier-transform spectroscopy (DRIFTS). Decane hydroconversion was used to evaluate the potential of the materials as hydro-cracking catalysts for vacuum bottoms. XRD was used to confirm modification of the material and good active phase dispersion. TPR revealed an important decrease in the reduction temperatures with auto-combustion method. Low-temperature reducible species play a key role in the catalytic performance for decane hydroconversion.