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Both GaAs and InP heterojunction bipolar transistors (HBT’s) were analyzed by x-ray diffraction measurements with (002) reflection. For GaAs HBT’s, the InGaP emitter thickness and alloy composition were accurately determined. For InP HBT’s, both the base and emitter layer thicknesses could be extracted. Thickness determined from x-ray diffraction measurements agreed well with that measured by transmission electron microscopy. © 2002 American Vacuum Society.