Nanocrystalline nickel aluminides (nano-NiAl and nano-Ni3Al) are synthesize
d by reactions of NiCl2 and LiAlH4 in Et2O or 1,3,5-trimethylbenzene, follo
wed by annealing of the reaction products at 550-750 degrees C. The reactio
n pathways followed in the two solvents differ, leading to nanocrystalline
materials of different composition and microstructure. The nanocrystalline
nickel aluminide powders are highly susceptible to adventitious oxidation,
which produces Al2O3 Consolidates obtained by hot pressing the powders at 7
00-1200 degrees C and 350-650 MPa in an Ar atmosphere contain 8-23 wt % Al2
O3. They possess densities of 80-98% of theory, and Vickers microhardnesses
of 4.0-6.3 +/- 0.3 GPa. Hot-pressing temperatures of greater than or equal
to 1200 degrees C are required to produce consolidates having good environ
mental stability. Consolidates are also produced by hot pressing admixtures
of nano-Ni and nano-Al, with and without added nano-AIN as a second, reinf
orcement phase. The resulting nanocrystalline and nanocomposite nickel alum
inides exhibit the highest purities, densities, and hardnesses (up to 7.4 /- 0.9 GPa) among the samples studied.