The thermal decomposition of nanosized aluminum hydroxides, which are precipitated from solution in direct and inverse mixing of the chemical agents, is studied. The thermal treatment of hydroxides between 370 and 870 K results in their two-stage thermal decomposition. Intermediate decomposition products are amorphous aluminum oxyhydroxide AlO(OH) 1+x and boehmite. Nanosized γ-Al 2 O 3 begins forming even at 570 K. The thermal decomposition of amorphous oxyhydroxide AlO(OH) 1+x ceases when amorphous alumina forms at 770-870 K. This results in powders representing a mixture of amorphous and γ-alumina.