Sol-Gel Synthesis of Transparent Alumina Gel and Pure Gamma Alumina by Urea Hydrolysis of Aluminum Nitrate

Abstract

γ-Alumina was synthesized by a sol-gel method with the aluminum ion hydrolysis control performed by urea. The initial saturated Al³⁺/urea solution presented urea coordinated with the aluminum ion, as shown in the ¹³C NMR and ²⁷Al NMR spectra and longitudinal relaxation times, T ₁, from the latter. The substitution of water molecules in the Al³⁺ coordination shell by urea controlled the hydrolysis process and provided an extensive nucleation during the initial steps of the aluminum hydroxide formation due to urea thermolysis at 90°C. The resulting sol, composed of Al(OH)₃ nanoparticles, coalesced and became a transparent gel permeated by a solution of urea and the polycation ion [Al₁₃O₄(OH)₂₄(H₂O)₁₂]⁷⁺. The freshly prepared gel was transformed, under heating at 300°C, directly to γ-alumina, characterized by FTIR, ²⁷Al-MAS-NMR and S_BET techniques, without δ- or θ-phases, as a consequence of the high degree of homogeneity of the γ-alumina precursor.