Three dimensional reciprocal space measurement by x-ray diffraction using linear and area detectors: Applications to texture and defects determination in oriented thin films and nanoprecipitates

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The authors present a method for the fast and efficient measurement of volumes of reciprocal space by x-ray diffraction using linear and area detectors. The goal of this technique is to obtain a complete overview of the reciprocal space to detect and characterize the nature and orientation of all the phases present. They first explain the detailed procedures and scan strategies required for transforming raw scattering data into three-dimensional maps of reciprocal space and present a complete open-source software package for advanced data processing, analysis, and visualization. Several case studies, chosen to highlight the overall capabilities of the technique, are then introduced. First, thermal diffuse scattering from a monocrystalline Si substrate is characterized by the presence of lines linking diffraction peaks in reciprocal space. Second, a detailed investigation of texture in multiphase thin layers permits us to reveal the unambiguous presence of fiber, axiotaxial, and epitaxial components in oriented films. The visualization of a significant fraction of reciprocal space has allowed us to identify an unexpected metastable phase, which could not be deduced from measurements carried out in the Bragg-Brentano geometry. The technique is then used to study planar defects in nickel silicides formed by solid-state reactions and micro twins in a GaP matrix containing coherent MnP precipitates. Overall, the authors show that the systematic acquisition of significant volumes of reciprocal space permits us to observe behaviors that might otherwise remain undetected when analyses are restricted to typical measurement scans. © 2013 American Vacuum Society.