Using a high-pressure (HP) technique, samples of γ-Al2O3 were obtained by compaction at 4.5 GPa, in a
toroidal-type apparatus, at room temperature (RT) and at higher temperatures. Compaction at RT produced
crack-free, translucent, and dense samples. An improvement of these properties was observed for samples
compacted at higher temperatures up to 565 °C. The nanocrystalline structure of γ-Al2O3 is retained, and the
samples became transparent, showing high hardness (HV = 17 ± 1 GPa) and high density (95% of theoretical
density). To understand the mechanisms of consolidation, a comparative analytical study by Fourier transform
infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and X-ray diffraction (XRD) was conducted
on the compacted γ-Al2O3 samples and the original powder. An FTIR study was done using the KBr technique
and a high-vacuum cell, where the samples were submitted to thermal treatments up to 450 °C. For samples
compacted at RT, a reduction in the content of adsorbed water was observed, compared to the original powder.
Also, the surface hydroxyl groups became bridged, promoting dehydroxylation reactions, which were confirmed
by TGA technique. In the dehydroxylation region, a weight loss was observed, and the water was released
only at temperatures above 300 °C. For samples compacted simultaneously with temperature, the FTIR and
TGA results did not show water release up to 500 °C. The compaction at temperatures higher than 565 °C
yielded the formation of an aluminum hydroxide (diaspore) and the phase transformation from γ- to α-Al2O3.
All these results support strongly the idea that the compaction at HP has caused the formation of a strong
structure, with closed pores containing trapped water and hydroxylated internal surfaces, which confirms a
proposed model for “cold-sintering”. At temperatures higher than 565 °C, this kind of structure is responsible
for the formation of diaspore plus α-Al2O3.