Heterostructural properties of pseudomorphic (AlGaAs/GaAs), partially strained (GaInAs/GaAs), and highly strained (GaAs/Si) semiconductor systems have been studied using High Resolution Double-Crystal X-ray Diffraction (DXRD), Transmission Electron Microscopy (TEM), and Scanning Electron Microscopy (SEM). Using the high resolution DXRD with CuKα1 and two-reflection Si (220) monochromator, we obtained (004) symmetric and (115) or (224) asymmetric reflection rocking curves for samples grown by molecular beam epitaxy. With 0.5 μm thick samples, perpendicular and in-plane lattice mismatches were calculated using elastic theory and compared with each other. The different degree of relaxation for these samples was observed and correlated with the lattice mismatch, X-ray layer peak broadening (i.e., full width at half maximum), and SEM surface morphology. For a GaInAs/GaAs sample, the strain relaxation along one of the <110> directions was more than the other direction, that is, the strain relaxation is not isotrophic. Also we observed that the lines were mainly parallel in one direction, i.e., they did not form a cross-hatch pattern. TEM images from both cross-sectional and planar views of the samples will be presented.