Jan Wernecke

The feature sizes of only a few nanometres in modern nanotechnology and next-generation microelectronics continually increase the demand for suitable nanometrology tools. Grazing-incidence small-angle X-ray scattering (GISAXS) is a versatile technique to measure lateral and vertical sizes in the nanometre range, but the traceability of the obtained parameters, which is a prerequisite for any metrological measurement, has not been demonstrated so far. In this work, the first traceable GISAXS measurements, demonstrated with a self-assembled block copolymer grating structure with a nominal pitch of 25 nm, are reported. The different uncertainty contributions to the obtained pitch value of 24.83 (9) nm are discussed individually. The main uncertainty contribution results from the sample–detector distance and the pixel size measurement, whereas the intrinsic asymmetry of the scattering features is of minor relevance for the investigated grating structure. The uncertainty analysis provides a basis for the evaluation of the uncertainty of GISAXS data in a more general context, for example in numerical data modeling.

The feature sizes of only a few nanometers in modern nanotechnology and next-generation microelectronics continually increase the demand for suitable nanometrology tools. Grazing incidence small-angle X-ray scattering (GISAXS) is a versatile technique to measure lateral and vertical sizes in the nm-range, but the traceability of the obtained parameters, which is a prerequisite for any metrological measurement, has not been demonstrated so far. In this work, the first traceable GISAXS measurements, demonstrated with a self-assembled block copolymer grating structure with a nominal pitch of 25 nm, are reported. The different uncertainty contributions to the obtained pitch value of 24.83(9) nm are discussed individually. The main uncertainty contribution results from the sample-detector distance and the pixel size measurement, whereas the intrinsic asymmetry of the scattering features is of minor relevance for the investigated grating structure. The uncertainty analysis provides a basis for the evaluation of the uncertainty of GISAXS data in a more general context, for example in numerical data modeling.

A dedicated in-vacuum X-ray detector based on the hybrid pixel PILATUS 1M detector has been installed at the four-crystal monochromator beamline of the PTB at the electron storage ring BESSY II in Berlin, Germany. Owing to its windowless operation, the detector can be used in the entire photon energy range of the beamline from 10 keV down to 1.75 keV for small-angle X-ray scattering (SAXS) experiments and anomalous SAXS at absorption edges of light elements. The radiometric and geometric properties of the detector such as quantum efficiency, pixel pitch and module alignment have been determined with low uncertainties. The first grazing-incidence SAXS results demonstrate the superior resolution in momentum transfer achievable at low photon energies.

A dedicated in-vacuum X-ray detector based on the hybrid pixel PILATUS 1M detector has been installed at the four-crystal monochromator beamline of PTB at the electron storage ring BESSY II in Berlin. Due to its windowless operation, the detector can be used in the entire photon energy range of the beamline from 10 keV down to 1.75 keV for small-angle X-ray scattering (SAXS) experiments and anomalous SAXS (ASAXS) at absorption edges of light elements. The radiometric and geometric properties of the detector like quantum efficiency, pixel pitch and module alignment have been determined with low uncertainties. The first grazing incidence SAXS (GISAXS) results demonstrate the superior resolution in momentum transfer achievable at low photon energies.

Grazing incidence small-angle x-ray scattering (GISAXS) and x-ray reflectometry (XRR) have been used to investigate structural parameters, especially period length, line width, groove width, and line height, of grating test structures in the sub-micron range. The gratings are e-beam written structures on a quartz substrate with a fixed period length, but different line and groove widths, covered by a layer of ruthenium. A Ru layer thickness of 9.4 nm has been determined with XRR. GISAXS was performed in two orientations, with an incident beam alignment perpendicular and parallel to the grating lines. The scattering patterns in parallel orientation have been analysed without numerical simulation by Fourier transformation. The obtained results for line and groove width are in good agreement with nominal values. The analysis method has been validated by analysing simulated scattering data. A superposition of scattering intensities measured for different azimuthal rotation angles close to parallel alignment was used to determine the line height of a grating of 27.3 nm, which is also close to the nominal value. The Fourier analysis procedure opens up the possibility of traceable structure determination with GISAXS in the nanometre range.