Zirconia alumina (ZrO2/Al2O3)-pillared saponite was prepared by the impregnation method using zirconium oxide chloride solution as a precursor. The effect of zirconia concentration on the physicochemical properties was studied with X-ray diffraction (XRD), surface area analysis and scanning electron microscopy (SEM). Its surface activity with respect to the change in physical properties was quantified by spectroscopic investigation of the adsorption of nitrogen oxide (NOx). Significant differences were found in the material textural parameters with increasing zirconium (Zr) content, decreasing specific surface area and the formation of the monoclinic zirconia phase. It was found that zirconia dispersion contributed to the enhanced NOx adsorption.