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Technologically important coatings of transition-metal aluminides can be produced by thermal or ion beam mixing of multilayer structures sputter deposited on substrates. The quantitative detection of constituents by depth profiling is sufficient to establish the efficiency of mixing methods. However, to decide whether a mixture of nanoparticles or a stoichiometric alloy is formed, EXAFS analysis of the local atomic neighborhood in the film is required. Ni K edge EXAFS spectra are measured on a series of samples of Ni/Al multilayer on Si(111) surface, after ion mixing at different substrate temperatures. The spectra show that with increasing temperature the nickel aluminide phase gradually substitutes the Ni fcc metal phase.

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