Monolithic diphasic gels of mullite by sol–gel process under ultrasound stimulation

Abstract

Diphasic gel in the mullite composition was prepared from a colloidal sol of boehmite mixed with a hydrolyzed tetraethoxisilane (TEOS) solution. The boehmite sol was obtained by peptization of a poorly crystallized or very small mean crystallite size (∼34 Å) precipitate, resulting from the reaction between solutions of aluminum sulfate and sodium hydroxide. Ultrasound was utilized in the processes of the TEOS hydrolysis and the boehmite peptization, and also for complete homogenization of the mixture to gel. The wet gel is almost clear and monolithic. The gel transparency is lost on drying, when syneresis has ended, so that the interlinked pore structure starts to empty and is recovered upon water re-absorption. Cracking closely accompanies this critical drying process. Differential thermal analysis (DTA) and X-ray diffraction (XRD) show that the solid structure of the gel is composed of an amorphous silica phase, as a matrix, and a colloidal sized crystalline phase of boehmite. Upon heat treatment, the boehmite phase within the gel closely follows the same transition sequence as in pure alumina shifted towards higher temperatures. Orthorhombic mullite formation was detected at 1300°C.