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High-resolution FIB-TEM-STEM structural characterization of grain boundaries in the high dielectric constant perovskite CaCu3Ti4O12
Affiliation:1. College of Ocean Science and Engineering, Shanghai Maritime University, Shanghai 201306, China;2. Department of Optical Science and Engineering, Fudan University, Shanghai 200433, China;3. College of Mechanical and Electronic Engineering, Shanghai Jian Qiao University, Shanghai, 201306, China;1. Department of Optical Science and Engineering, Fudan University, Shanghai, 200433, China;2. Editorial Department of Journal, Cangzhou Normal University, Cangzhou, Hebei, 061001, China;3. College of Ocean Science and Engineering, Shanghai Maritime University, Shanghai, 201306, China
Abstract:In this work, the grain boundaries composition of the polycrystalline CaCu3Ti4O12 (CCTO) was investigated. A Focused Ion Beam (FIB)/lift-out technique was used to prepare site-specific thin samples of the grain boundaries interface of CCTO ceramics. Scanning transmission electron microscopy (STEM) coupled with energy dispersive X-ray spectrometry (EDXS) and Electron Energy Loss Spectroscopy (EELS) systems were used to characterize the composition and nanostructure of the grain and grain boundaries region. It is known that during conventional sintering, discontinuous grain growth occurs and a Cu-rich phase appears at grain boundaries. This Cu-rich phase may affect the final dielectric properties of CCTO but its structure and chemical composition remained unknown. For the first time, this high-resolution FIB-TEM-STEM study of CCTO interfacial region highlights the composition of the phases segregated at grain boundaries namely CuO, Cu2O and the metastable phase Cu3TiO4.
Keywords:Grain boundaries  Scanning-transmission electronic microscopy  High angle aperture dark field imaging  Electron energy loss spectroscopy  Focused ion beam  Nanostructure
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