To ensure all samples originated from the exact same batch, a large batch of γ-Al
2O
3 was prepared, similar to the previously reported method [13 (
link)]. To this end, 156 g of AlCl
3·6H
2O (
Fluka) were dissolved in 137 mL of distilled water and 200 mL ethanol (
Bioenergie Icking GmbH). After complete dissolution, 10.2 g of
oxalic acid (dihydrate,
Merck) were added and dissolved. Without delay, the reaction mixture was placed in a flask surrounded by an ice bath and cooled down to 4 °C, then 140 mL of
propylene oxide (
Acros Organics) were added, all at once, under vigorous stirring. The ice bath was removed after 6.5 min, and the reaction mixture was stirred at room temperature for another 6.5 min. The obtained sol was poured into a beaker, sealed and placed in an oven at 40 °C for gelation. To ensure a uniform heat transfer, the beaker resided in a water bath. After 24 h, solvent exchange to pure ethanol was carried out under static conditions for 3 days. The opaque white gel was then transferred to a drying cabinet pre-heated at 70 °C, with the lid removed. Drying was terminated after 7 days. Ultimately, the obtained xerogel was pre-calcined at 650 °C for 6 h, with a heating rate of 3 K min
−1. Characterization of the starting material was carried out as described in
Section 3.1.
Jähnichen T., Carstens S., Franz M., Laufer O., Wenzel M., Matysik J, & Enke D. (2023). Towards High Surface Area α-Al2O3–Mn-Assisted Low Temperature Transformation. Materials, 16(8), 3047.