A commercial Empyrean X-ray diffractometer was adapted for combined grazing incidence X-ray fluorescence analysis (GIXRF) measurements with X-ray reflectivity (XRR) measurements. An energy-dispersive silicon drift detector was mounted and integrated in the angle-dependent data acquisition of the Empyrean. Different monochromator/X-ray optics units have been compared with the values obtained by the Atominstitut GIXRF + XRR spectrometer. Data evaluation was performed by JGIXA, a special software for combined GIXRF + XRR data fitting, developed at Atominstitut. A sample consisting of a ~50 nm nickel layer on a silicon substrate was used to compare the performance criteria (i.e. divergence and intensity) of the incident beam optics. An Empyrean X-ray diffractometer was successfully refitted to measure both GIXRF and XRR data.

It is demonstrated that a complex X-ray characterization of semiconductor films epitaxially grown on metal oxide buffer layers and Si(111) substrates is possible using laboratory-based equipment. This is demonstrated with epi-germanium on Pr2O3 as buffer material. Pole figure measurements prove that epi-Ge layers are nearly single crystalline with exactly the same in-plane orientation (type A) as the Si(111) substrate, while the lattice of the oxide layer is 180° rotated around the [111] surface normal (type B). Only a small fraction (less than 0.6 vol %) of the epi-Ge exhibits type B rotation twins. The main structural defects are microtwin lamellas lying in {111} planes 70.5° inclined to the wafer surface. The different in-plane orientation of the Si substrate and epi-Ge on one side and the Pr2O3 buffer layer on the other side allows a very sensitive analysis of strain and defects even for a 10-nm oxide layer buried under a 100-nm Ge. The epi-Ge layers are nearly fully relaxed and the Pr2O3 buffer layer is compressively strained. Due to the existing defects the Ge (111) planes are tilted in a characteristic pattern relative to the Si substrate.