Characterization of nanoparticle and thin-film texture: pole-figure measurements in grazing-incidence configuration

X-ray diffraction pole-figure measurements are essential to analyze crystallographic texture in thin films and nanoparticles. Conventionally, large and equal incident and exit angles beyond the critical angle of the studied material are used, limiting surface sensitivity. This study demonstrates the use of grazing-incidence wide-angle X-ray scattering (GIWAXS) while rotating the sample azimuthally in its own plane to acquire pole figures that are more sensitive to the near-surface region compared with pole figures measured in standard Schulz geometry. Comparative measurements on supported Pt nanoparticles in GIWAXS and Schulz geometry at two different synchrotron beamlines confirm the improved sensitivity of the GIWAXS pole figures. By tuning the incident angle, the substrate diffraction background can be reduced and the information depth inside a Pt thin film can be selected. In addition, the near-horizontal sample orientation during GIWAXS – only tilted by the small incident angle – reduces constraints on sample environments compared with conventional Schulz geometry. The increased sensitivity to the near-surface region of a grazing-incidence X-ray beam, combined with the simpler measurement geometry, prove grazing-incidence pole figures to be powerful for future in situ and ex situ texture analysis on thin films and supported nanoparticles.