The aim of this work is to prepare and characterize Al2O3-ZrO2 powders by Pechine method and to evaluate them as supports for palladium catalysts in the selective reduction of NO with CH4. The effect of aluminum ion on the final characteristics of the zirconia powder is also investigated. The catalytic supports were characterized by X-ray diffraction (XDR), scanning electron microscopy (SEM) and catalytic activity. The XRD data showed the formation of tetragonal zirconia phase, with crystallite size of 6.3 and 6.1 nm for the supports prepared with 0.1 and 0.5 moles of Al3+, respectively. Both supports showed porous and homogeneous agglomerates. Pd/Al2O3-ZrO2 catalysts were active NO reduction by CH4.