Al and AlN sublayers with thickness of 100 and 500 nm, respectively, deposited on sapphire using pulsed laser ablation are characterized by elevated-temperature X-ray diffraction. Pole figure measurements performed at room temperature indicate heteroepitaxial growth of Al on AlN and AIN on sapphire with Al(111)[110]parallel toAlN(0001)[1120] and AlN(0001)[1010]parallel toAl(2)O(3)(0001)[1120], respectively. The diffraction measurements in the temperature range of 25-550degreesC allow to resolve in-plane residual stresses for both sublayers simultaneously. The heating up of the structure is accompanied by a decrease of room temperature tensile stress and a subsequent plastic deformation in Al sublayer in the temperature range of 350-550degreesC while, in the AlN sublayer, a decrease of room temperature compressive stress as well as a post-annealing stress relaxation are observed. The temperature behavior of the stresses in the structure can be interpreted by the mismatch of thermal expansion coefficients between sublayers and substrate. (C) 2003 Elsevier B.V. All rights reserved.