α-Alumina (α-Al2O3), widely used as a raw material or production in advanced manufacturing industry, has attracted much attention in terms of its preparation temperature. A simple dissolution-evaporation-precipitation process was employed to obtain the amorphous Al-oxalate (AAO) precursor, serving as the starting material for the low temperature preparation of nano α-Al2O3. The crystalline structure and thermal behavior of the AAO were compared with commercially available aluminum hydroxide (Al(OH)3) powder using the X-ray powder diffraction (XRD) instrument, the thermal gravity analysis and differential scanning calorimetry (TG-DSC). The phase transition mechanism of AAO was investigated by the fourier transform infrared spectroscopy (FTIR), transmission electron microscope (TEM), scanning electron microscope (SEM), and 27Al magic angle spinning nuclear magnetic resonance (27Al-MAS-NMR). The DSC results indicated that AAO underwent a phase transformation at 982 °C. The α-alumina diffraction peaks appeared in AAO at 1000 °C, while α-Al2O3 phase was observed for Al(OH)3 at 1200 °C. Furthermore, an absorption peak at 452 cm−1, corresponding to Al–O bond in α-alumina was detected at 1000 °C. The proposed low-temperature preparation mechanism of α-alumina from AAO is as follows: four coordination Al-oxalate species entities coexist within the AAO sample; with increasing temperature, organic acid functional groups oxidize and volatilize, resulting in the formation of tetra-coordinate [AlO4], penta-coordinate [AlO5], and hexa-coordinate [AlO6] atomic groups; these atomic clusters further polymerize to form a structurally dense α-alumina crystal at the nano-scale (∼50 nm) at around 1000 °C. The experimental findings present a novel approach and method for the low-temperature preparation of nano-sized alumina powder. Additionally, a feasible theoretical reference for the low-temperature phase transition mechanism of amorphous Al-oxalate was provided.
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