A Zn_xCu_1−xAl₂O₄ catalyst was prepared via the microwave-assisted solution combustion method (MSC). This method presents a fast procedure for industrial scale catalyst preparation. The physicochemical properties of the fabricated catalyst were characterized using XRD, FTIR, BET, SEM and TEM analyses. The catalytic performance through the esterification reaction was examined under the following conditions: reaction temperature = 180 °C, catalyst concentration = 3% (w/w), molar ratio of oleic acid to methanol = 9 and reaction time = 6 h. XRD results showed that loading both zinc and copper oxides on alumina at a ratio of amounts that were nearly the same resulted in decreased crystalline size and well-dispersed copper-alumina and zinc-alumina crystals. Moreover, the mean pore diameter of the sample was increased by simultaneous loading of zinc and copper oxides on alumina that enhanced permeation of the reactants within pores and increased the interaction of the reactant with the catalyst active sites. The catalyst showed minimum tendency towards adsorbing moisture from air, which was attributed to it having less atoms on the surface through which binding with H₂O molecules takes place. The highest level of activity in the esterification reaction (96.9%) was obtained at the optimum ratio of the Zn:Cu molar ratio, identified to be 2:3. The sample particles ranged from 10 to 30 nm in size, without agglomeration.