A Processable Mullite Precursor Prepared by Reacting Silica and Aluminum Hydroxide with Triethanolamine in Ethylene Glycol: Structural Evolution on Pyrolysis

A simple, processable precursor to mullite can be synthesized in quantities of 100 g in a few hours by direct reaction of silica, aluminum hydroxide, and triethanolamine in ethylene glycol. To delineate a processing window whereby precursor shapes can be transformed into mullite, the chemical and phase microstructural evolution of this precursor on pyrolysis to selected temperatures in air is followed by thermal gravimetric analysis, differential thermal analysis, diffuse reflectance infrared Fourier transform spectroscopy, solid‐state 27 Al and 29 Si nuclear magnetic resonance, X‐ray diffractometry, and Brunauer‐Emmett‐Teller analytical methods. The precursor behaves as a single‐phase, atomically mixed material that initially transforms to a porous, amorphous aluminosilicate when heated to temperatures as high as 950°C. Above 950°C, the precursor first transforms to tetragonal mullite, based on comparison with the literature, and, on continued heating above 1200°C, to orthorhombic mullite with coincident loss of porosity.