Small-angle scattering is widely used for measuring materials microstructure in the 1–100 nm size range. Ultrasmall-angle x-ray scattering (USAXS), typically achieved through crystal collimation, extends this size range to include features over 1 μm in size. This article reports on USAXS on the UNICAT beam line 33-ID at the Advanced Photon Source. The instrument makes use of a six-reflection crystal pair as a collimator and another six-reflection crystal pair as an analyzer. First principle absolute calibration and a broad scattering vector range make this a very effective instrument, limited only by the fact that the measurement of anisotropic microstructures is excluded due to slit smearing from the crystal collimation. This limitation has recently been removed by adding a horizontally reflecting crystal before and another after the sample. This creates a USAXS instrument with collimation in two orthogonal directions. We call this configuration effective pinhole USAXS. Now, anisotropic materials are probed using 9–17 keV photons in the same physically-relevant (from 50 nm to over 1 μm) microstructural size range as that available for materials which scatter isotropically.

Ilavsky, J., Allen, A. J., Long, G. G., & Jemian, P. R. (2002). Effective pinhole-collimated ultrasmall-angle x-ray scattering instrument for measuring anisotropic microstructures. Review of Scientific Instruments, 73(3), 1660–1662.