Water-vapor adsorption and surface area measurement of poorly crystalline boehmite

Shan-Li Wang, Birck Nanotechnology Center, Purdue University
Cliff T. Johnston, Birck Nanotechnology Center, Purdue University
David L. Bish, Hydrology, Geochemistry, and Geology, Los Alamos National Laboratory
Joe L. White, Agronomy, Purdue University
Stanley L. Hem, Industrial and Physical Pharmacy, Purdue University

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Water-vapor adsorption on poorly crystalline boehmite (PCB) was studied using a gravimetric FTIR apparatus that measured FTIR spectra and water adsorption isotherms simultaneously. The intensity of the δ(HOH) band of adsorbed water changed linearly with water content and this linear relationship was used to determine the dry mass of the sample. Adsorption and desorption isotherms of PCB showed a Type IV isotherm. The BETH2O surface area of PCB was 514 ± 36 m2/g. The mean crystallite dimensions of PCB were estimated to be 4.5× 2.2× 10.0 nm (dimensions along the a, b, and c axes, respectively) based on application of the Scherrer equation to powder diffraction data of PCB. A surface area value of 504 ± 45 m2/g calculated using the mean crystallite dimensions was in good agreement with the BETH2O surface area. This work also demonstrated a method to determine surface areas for materials with minimal perturbation of their surface structure. In addition, the FTIR spectra of PCB were influenced by changes in water content. The δ(AlOH) band at 835 cm−1 observed under dry conditions was assigned to the non-H-bonded surface OH groups. As the amount of adsorbed water increased, the intensity at 835 cm−1 decreased and that at 890 and 965 cm−1 increased. The 890- and 965-cm−1 bands are assigned to surface OH groups H-bonded with adsorbed water.