The performance of InGaAs/GaAs pseudomorphic high electron mobility transistors is anticipated to improve with increased channel thickness due to reduced effects of quantum confinement. However, greater channel thicknesses increase the probability of forming misfit dislocations which have been reported to impair device properties. We characterized the composition and thickness of the active layer in Al0.25Ga0.75As / In0.21Ga0.79As structures with different channel thicknesses (75 Å - 300 Å) to within ± 0.005 and ± 8 Å using high resolution x-ray techniques. We determined, using Hall and rf measurements, that the device properties of these structures improved with increasing thickness up to about 185-205 Å; degraded properties were observed for thicker channel layers. Cathodoluminescence results indicate that the mosaic spread observed in x-ray triple axis rocking curves of these device structures is due to the presence of misfit dislocations. Thus, even though misfit dislocations are present, the device structure performs best with a channel thickness of ∼185 Å. These results demonstrate that one can fabricate functional devices in excess of critical thickness considerations, and that these x-ray techniques provide an effective means to evaluate structural properties prior to device processing.