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A novel mesoporous intermetallic NiAl nanocompound was successfully prepared at 600 °C in a molten LiCl with an assistance of CaH2. The obtained powder had a fine crystal structure assigned to a single phase intermetallic NiAl. The measured BET surface area was as high as 113.9m2/g, originating from the mesopores (3.1 nm on average) and the unique crumpled morphology. Calcium species, such as CaH2, Ca(OH)2, CaO and CaCl2, could work as templates in alloying process and they were readily removable by NH4Cl solution rinsing afterwards. As far as we know, this paper is the first report of mesoporous metal aluminide with a defined crystal structure and a high surface area of >100m2/g. [ABSTRACT FROM AUTHOR]