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The intimate blending of two incompatible polymeric materials constitutes one of the most important fields of study in polymer science. A vast arsenal of techniques, ranging from copolymerization to melt-blending, has been assembled to mix intrinsically immiscible polymers and optimize the physical properties of the resultant system. For some systems, however, even established techniques cannot produce useable blends. To overcome this limitation, non-equilibrium mechanical alloying (high-energy ball milling of two or more dissimilar powders) has been employed to produce blends of poly(ethylene terephthalate) (PET) and Vectra (73/27 oxybenzoate/oxynaphthoate). Characterization of these blends by TEM is confounded by the absence of a preferential staining agent, in which case Scanning Transmission X-ray Microscopy (STXM) provides a valuable alternative in examining the morphology and chemistry of these blends.The x-ray microscope utilizes a diffraction element called a zone plate to focus soft x-rays into a microprobe. A thin section of sample is placed in this microprobe, and the transmitted photon intensity measured.