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Transmission electron microscopy (TEM) imaging and electron diffraction (ED) techniques are widely used in the studies of thin films and nanoparticles. Although various advanced techniques have been well established, such as high-resolution electron microscopy (HREM) and convergent beam electron diffraction (CBED), the conventional TEM imaging and selected-area electron diffraction (SAED) techniques remain the essential methods for microstructure and crystal structure characterization. Digital TEM image processing and quantitative ED analysis (QED) has become one trend for improvements. Recently computer programs [1,2] have been developed for analysis of SAED patterns of polycrystalline phases. In this paper, we report the preliminary results on a TEM/QED study of FePt ultrathin films and Co/CoO core shell particles.