Total reflection X-ray fluorescence (TXRF) analysis is a well-established method to monitor lowest level contamination on semiconductor surfaces. Even light elements on a wafer surface can be excited effectively when using high-flux synchrotron radiation in the soft X-ray range. To meet current industrial requirements in nondestructive semiconductor analysis, the Physikalisch-Technische Bundesanstalt (PTB) operates dedicated instrumentation for analyzing light element contamination on wafer pieces as well as on 200- and 300-mm silicon wafer surfaces. This instrumentation is also suited for grazing incidence X-ray fluorescence analysis and conventional energy-dispersive X-ray fluorescence analysis of buried and surface nanolayered structures, respectively. The most prominent features are a high-vacuum load-lock combined with an equipment front end module and a UHV irradiation chamber with an electrostatic chuck mounted on an eight-axis manipulator. Here, the entire surface of a 200- or a 300-mm wafer can be scanned by monochromatized radiation provided by the plane grating monochromator beamline for undulator radiation in the PTB laboratory at the electron storage ring BESSY II. This beamline provides high spectral purity and high photon flux in the range of 0.078-1.86 keV. In addition, absolutely calibrated photodiodes and Si(Li) detectors are used to monitor the exciting radiant power respectively the fluorescence radiation. Furthermore, the footprint of the excitation radiation at the wafer surface is well-known due to beam profile recordings by a CCD during special operation conditions at BESSY II that allow for drastically reduced electron beam currents. Thus, all the requirements of completely reference-free quantitation of TXRF analysis are fulfilled and are to be presented in the present work. The perspectives to arrange for reference-free quantitation using X-ray tube-based, table-top TXRF analysis are also addressed.

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.

The Metrology Light Source (MLS), the new electron storage ring of the Physikalisch-Technische Bundesanstalt (PTB) located in Berlin, is dedicated to metrology and technological developments in the UV and extreme UV spectral range as well as in the IR and THz region. The MLS can be operated at any electron beam energy between 105 and 630 MeV and at electron beam currents varying from 1 pA (one stored electron) up to 200 mA. Moreover, it is optimized for the generation of coherent synchrotron radiation in the far IR/THz range. Of special interest for PTB is the operation of the MLS as a primary radiation source standard from the near IR up to the soft x-ray region. Therefore, the MLS is equipped with all the instrumentation necessary to measure the storage ring parameters and geometrical parameters needed for the calculation of the spectral photon flux according to the Schwinger theory with low uncertainty.

For the quantitative surface characterization of a monocrystalline silicon sphere, PTB has constructed and put into operation an analytical instrument, which combines x-ray fluorescence and x-ray photoelectron spectroscopy techniques. The main objective of this novel instrument is the characterization of the oxide layer and unintentional contaminations, e.g. from hydrocarbons. It is equipped with a ball manipulator allowing measurements at each point on the surface of ball-shaped samples with a diameter of about 93.7 mm. Monocrystalline silicon spheres with this diameter allow a realization of the SI base unit of mass.

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