A thin alumina-hydrotalcite (Al-HT) film was fabricated from the synthesized boehmite and HT sol samples. The sols were a Newtonian fluid within 12 h of the sol synthesis and pseudo-plastic flow thereon. Co-precipitated HT demonstrated poorly crystallized periclase and spinel structures and apparent doublet peak of hydrotalcite at 2θ = 39-44• , indicative of a disordered structure. The heated Al-HT sample demonstrated highly amorphous structure with single hydrotalcite peak but barely observed γ -alumina and γ -boehmite phases. The exfoliation of the spinel, gibbsite and periclase in the Al-HT was caused by the intercalation of boehmite into the HT layers that impeded the formation of the oxides phases.