Abstract
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.
Highlights
X-ray reflectometry (XRR) is a well-known and established technique for the characterization of single- and multi-layered thin-film structures with layer thicknesses in the nanometer range
The NiKα XRF from the layer is not accessible with the copper tube and the available optics as the Ni-K edge (8.3 keV) is above the energy of the CuKα radiation (8.04 keV), but it is important to note that the SiKα Grazing incidence X-ray fluorescence (GIXRF) from the substrate is modulated because of the interference effects caused by the layer
The evaluation was done with the software JGIXA (Ingerle et al, 2016)
Summary
X-ray reflectometry (XRR) is a well-known and established technique for the characterization of single- and multi-layered thin-film structures with layer thicknesses in the nanometer range. The combined measurement and evaluation of GIXRF and XRR data can improve the obtained information, as it reduces uncertainties and ambiguities of the individual techniques, especially for the analysis of samples, for which the exact stoichiometry might not be known (Ingerle et al, 2014a). In a previously published approach, we modified an existing GIXRF setup by adding a detector for the simultaneous acquisition of XRR intensities (Ingerle et al, 2014b). This setup has several advantages (e.g. vacuum chamber and exchangeable tube anode material), it suffers from a somewhat limited measurement resolution because of minimum motor step size as well as beam divergence. A custom control software was developed in order to synchronize the acquisition of XRF spectra with the angular movement during an XRR scan
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