Although the AlxGa(1-x)As alloy system has been extensively investigat
ed, there are still considerable uncertainties in measuring the value
of x. Here a new AlxGa(1-x)As calibration structure, grown by molecula
r beam epitaxy, has been used to establish unambiguous alloy compositi
ons. Such 'standard' AlxGa(1-x)As layers were measured by high-resolut
ion X-ray diffraction, photoluminescence, and Raman spectroscopy to de
termine the compositional variations of the measured physical paramete
rs. The formulae provided give a reliable calibration base for other c
haracterization tools. A detailed analysis of the X-ray results shows
that Vegard's law does not hold fur the variation of the AlxGa(1-x)As
lattice constant with x.