Aluminum hydroxide is an essential material for the industrial production of ceramics (especially insulators and refractories), desiccants, absorbents, flame retardants, filers for plastics and rubbers, catalysts, and various construction materials. The calcination process of Al(OH)3 first induces dehydration and, finally, results in α-Al2O3 formation. Nevertheless, this process contains various intermediary steps and has been proven to be complicated due to the development of numerous transitional alumina. Each step of the investigation is vital for the entire process because the final properties of materials based on aluminum trihydroxide are determined by their phase composition, morphology, porosity, etc. In this paper, five dried, milled, and size-classified aluminum hydroxide specimens were thermally treated at 260, 300, and 400 °C; then, they were studied in order to identify the effects of temperature on their properties, such as particle morphology, specific surface area, pore size, and pore distribution. The major oxide compounds identified in all samples were characteristic of bauxite—namely, Al2O3 * 3H2O, SiO2, Fe2O3, Na2O, and CaO. Particles with smaller sizes (<10 µm = 76.28%) presented the highest humidity content (~5 wt.%), while all samples registered a mass loss of ~25 wt.% on ignition at 400 °C. The identified particles had the shapes of hexagonal or quasi-hexagonal platelets and resulted in large spherulitic concretions. The obtained results suggest that ceramic powders calcined at 400 °C should be used for applications as adsorbents or catalysts due to their high specific area of about 200–240 m2/g and their small pore width (3–3.5 nm).