Metastable long-period superstructures in an L10-TiAl single crystal with a composition gradient were observed successfully by transmission electron microscopy with a focused ion beam (FIB) microsampling technique. The composition gradient from 54.7 to 75 at.% Al with approximately 6 microm width was detected by electron probe microanalysis and foil specimens containing the composition-gradient area were fabricated by the FIB microsampling method. The foil specimens clearly exhibit sequential changes in long-period superstructure depending on the Al concentration.
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