Ja. Haber et We. Buhro, KINETIC INSTABILITY OF NANOCRYSTALLINE ALUMINUM PREPARED BY CHEMICAL SYNTHESIS - FACILE ROOM-TEMPERATURE GRAIN-GROWTH, Journal of the American Chemical Society, 120(42), 1998, pp. 10847-10855
Nanocrystalline aluminum (nano-Al) is synthesized by two chemical meth
ods. Method A consists of the following: reaction of LiAlH4 and AlCl3
at 164 degrees C in 1,3,5-trimethylbenzene produces nano-Al with an av
erage mean coherence length (crystallite size) of 160 +/- 50 nm. The b
yproduct LiCl is removed by washing with MeOH at -25 or 0 degrees C. M
ethod B consists of the following: nano-Al is produced by decompositio
n of H3Al(NMe2Et) under reflux in 1,3,5-trimethylbenzene (ca. 100-164
degrees C), with or without added decomposition catalyst Ti(O-i-Pr)(4)
. Here the mean particle size (40-180 nm) and degree of aggregation of
the nano-Al depend on the mole percent of decomposition catalyst used
(0-1%). The nano-Al produced by method A contains 3-4 wt % each of C,
O, and Cl; whereas that produced by method B contains only less than
or equal to 0.25 wt % each of C, O, and Cl and is greater than or equa
l to 99 wt % Al. nano-Al produced by both methods has been consolidate
d by uniaxial pressing at 350 MPa for 1 h at 25, 100, or 300 degrees C
Rapid grain growth is observed at each pressing temperature in method
-B powders. The mean grain size doubles at 25 degrees C within 1 h and
continues to increase beyond the nanometer-size regime over longer pe
riods. The low-temperature grain-size instability of the chemically sy
nthesized (method-B) nano-Al contrasts markedly with the high-temperat
ure stability (greater than or equal to 300 degrees C) of nano-Al prep
ared by gas condensation or mechanical attrition. Facile grain growth
in the chemically synthesized (method-B) nano-Al is attributed to high
er grain-boundary purity and to aggregate structures that minimize adv
entitious oxidation. The results establish that barriers to grain grow
th in pure nano-Al are intrinsically low.