Structures of Al0.047Ga0.953Sb layers on GaSb (100) substrates were studied by high resolution X-ray diffraction (HRXRD) using reciprocal space maps (RSM) and rocking curves around the (004) and (115) reflections. The layers were grown at 450°C with a supersaturation of 10°C in a conventional Liquid Phase Epitaxy (LPE) system varying the growth time from 1 to 4min resulting in an increment of thickness. It was found that tilt, relaxation and dislocation density of the layers can be calculated using its rocking curves and reciprocal space mapping and it is found that these characteristics are influenced by the thickness of layer.