The availability of intense, focused synchrotron X-ray microbeams has enabled new techniques for materials investigations with sub-micron spatial resolution. The scanning microbeam setup we have developed at the XOR-UNI beamline at the Advanced Photon Source (APS) is versatile in that it provides 1D, 2D or 3D scans (including depth resolution), and call alternate between polychromatic- and monochromatic-beam modes. Focusing in both modes uses elliptical Kirkpatrick-Baez (K-B) reflecting mirrors. Beam diameters of similar to 500 nm FWHM are now routine, and 90 nm focus has been demonstrated. In white-beam mode, a CCD detector records a complete Laue diffraction pattern, which is analyzed with all automated indexing program. These X-ray diffraction patterns provide real-space maps of the local lattice structure, crystal orientation, grain morphology, and strain tensor. Spatially-resolved X-ray microdiffraction studies are now providing previously unavailable measurements of local microstructures. These measurements, in turn, yield new insights in several classic fields of materials science. This paper will illustrate the application of polychromatic scanning X-ray microscopy with examples from I D 2D and 3D materials systems. In I D systems, we have mapped the Structure and orientation of an individual ZnO nanorod along with the associated Ge catalyst particle used to control the nanocrystal growth. In 2D systems, X-ray microdiffraction studies have revealed the mechanisms for local crystallographic tilting in epitaxial oxide films grown on textured Ni substrates for superconducting applications. In 3D systems, X-ray microscopy investigations have included in-situ Studies of microstructural evolution during thermal grain growth in polycrystalline aluminum. In general, these spatially-resolved measurements provide important new insights and are valuable as input for theoretical and Computer modeling studies of a wide range of material processes. (C) 2008 Elsevier B.V. All rights reserved.