In this paper, mesoporous alumina with different pore sizes and wall crystalline. structures was synthesized at calcination temperatures over 550 degrees C. The characterization of the samples calcined at 550, 800, 1100, and 1300 degrees C, respectively, was performed using TEM, XRD, FTIR, TG/DTA, and N-2 adsorption/desorption techniques. The correlation between pore size and wall crystalline structure on calcination temperature was systematically investigated. (C) 2007 Elsevier Inc. All rights reserved.