Void formation at the interface between thick AlN layers and (0 0 0 1) sapphire substrates was investigated to form a predefined separation point of the thick AlN layers for the preparation of freestanding AlN substrates by hydride vapor phase epitaxy (HVPE). By heating 50-200 nm thick intermediate AlN layers above 1400 degrees C in a gas flow containing H-2 and NH3, voids were formed beneath the AlN layers by the decomposition reaction of sapphire with hydrogen diffusing to the interface. The volume of the sapphire decomposed at the interface increased as the temperature and time of the heat treatment was increased and as the thickness of the AlN layer decreased. Thick AlN layers subsequently grown at 1450 degrees C after the formation of voids beneath the intermediate AlN layer with a thickness of 100 mm or above self-separated from the sapphire substrates during post-growth cooling with the aid of voids. The 79 mu m thick freestanding AlN substrate obtained using a 200 nm thick intermediate AlN layer had a flat surface with no pits, high optical transparency at wavelengths above 208.1 nm, and a dislocation density of 1.5 x 10(8) cm(-2). (C) 2010 Elsevier B.V. All rights reserved.