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New kinetics data have been obtained for a Ni + Al self-propagating high-temperature synthesis (SHS). In order to achieve a time resolution of 0.005 s it was necessary to increase the intensity of the incident beam and the aperture of the X-ray detector. A graphite monochromator with a wavelength bandwidth of Δλ/λ ≃ 10−2, instead of the traditional 10−3–10−4, and a two-dimensional detector (DED-5) were used for these purposes. Analysis of the kinetics data indicated that the main chemical transformations occurred during 60–70 ms. The DED-5 detector also helped to establish that the recrystallization process of intermetallide NiAl took place some time after the SHS, and the formation of crystallites could be seen as separate Bragg spots on the detector image.

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