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A reconstruction method is presented for the generation of three-dimensional maps of the grain boundaries within powders or polycrystals. The grains are assumed to have a mosaic spread below 1°. They are mapped layer by layer in a non-destructive way by diffraction with hard X-rays. First the diffraction spots are sorted with respect to grain of origin by the indexing program GRAINDEX. Next for each grain the reconstruction is performed by ART – an iterative algebraic algorithm. The method is optimized by simulations. It is verified by a 50 keV study on one embedded layer in an aluminium specimen. The layer comprises ∼50 grain sections of an average size of 100 µm. Based on the use of five reflections per grain, a resolution of ∼5 µm is inferred.

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