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Keywords:

  • three-dimensional chemical imaging;
  • scanning transmission X-ray microscopy;
  • NEXAFS spectroscopy;
  • polystyrene microspheres;
  • polyacrylates;
  • tomography.

Three-dimensional (3-d) chemical mapping using angle-scan tomography in a scanning transmission X-ray microscope is demonstrated. Apparatus, experimental procedures and data processing are presented and the 3-d spatial resolution is evaluated. The technique is illustrated using mapping of a low-density acrylate polyelectrolyte in and outside of polystyrene microspheres dispersed in water in a 4 µm-diameter microcapillary. The 3-d chemical visualization provides information about the microstructure that had not previously been observed.