A novel ultra-high vacuum instrument for X-ray reflectometry and spectrometry-related techniques for nanoanalytics by means of synchrotron radiation has been constructed and commissioned. This versatile instrument was developed by the Physikalisch-Technische Bundesanstalt, Germany's national metrology institute, and includes a 9-axis manipulator that allows for an independent alignment of the samples with respect to all degrees of freedom. In addition, a rotational and translational movement of several photodiodes as well as a translational movement of an aperture system in and out of the beam is provided. Thus, the new instrument enables various analytical techniques based on energy dispersive X-ray detectors such as reference-free X-ray fluorescence analysis (XRF), total-reflection XRF, grazing-incidence XRF in addition to optional X-ray reflectometry measurements or polarization-dependent X-ray absorption fine structure analyses. With this instrument samples having a size of up to 100 mm × 100 mm can be analyzed with respect to their mass deposition, elemental or spatial composition, or the species in order to probe surface contamination, layer composition and thickness, the depth profile of matrix elements or implants, the species of nanolayers, nanoparticles or buried interfaces as well as the molecular orientation of bonds. Selected applications of this advanced ultra-high vacuum instrument demonstrate both its flexibility and capability.

Photon-in/photon-out experiments at thin specimens have been carried out to determine $L$-subshell fluorescence yields as well as Coster-Kronig transition probabilities of Au, Pb, Mo, and Pd using radiometrically calibrated instrumentation in the Physikalisch-Technische Bundesanstalt (PTB) laboratory at the electron storage ring BESSY II in Berlin. An advanced approach was developed in order to derive the fluorescence line intensities by means of line sets of each subshell that were corrected for self-absorption and broadened with experimentally determined detector response functions. The respective photoelectric cross sections for each subshell were determined by means of transmission measurements of the same samples without any change in the experimental operating condition. All values derived were compared to those of earlier works. A completely traceable uncertainty budget is provided for the determined values.

The accurate characterization of nanolayered systems is an essential topic for today’s developments in many fields of material research. Thin high-k layers and gate stacks are technologically required for the design of current and future electronic devices and can be deposited, e.g., by Atomic Layer Deposition (ALD). However, the metrological challenges to characterize such systems demand further development of analytical techniques. Reference-free Grazing Incidence X-ray Fluorescence (GIXRF) based on synchrotron radiation can significantly contribute to the characterization of such nanolayered systems. GIXRF takes advantage of the incident angle dependence of XRF, in particular below the substrate’s critical angle where changes in the X-ray Standing Wave field (XSW) intensity influence the angular intensity profile. The reliable modeling of the XSW in conjunction with the radiometrically calibrated instrumentation at the PTB allows for reference-free, fundamental parameter-based quantitative analysis. This approach is very well suited for the characterization of nanoscaled materials, especially when no reference samples with sufficient quality are available. The capabilities of this method are demonstrated by means of two systems for transistor gate stacks, i.e., Al₂O₃ high-k layers grown on Si or Si/SiO₂ and Sc₂O₃ layers on InGaAs/InP substrates.

We studied the resonant Raman scattering of x rays in the vicinity of the $K$ absorption edge of silicon. The investigation was carried out at the plane grating monochromator beamline for undulator radiation of the PTB laboratory at BESSY II in Berlin. Cross sections were determined absolutely for a wide energy range of incident photons with small relative uncertainties employing calibrated instrumentation avoiding any reference samples. The experimentally determined values differ clearly from the theoretical ones found in the literature.