Liquid-feed flame spray pyrolysis (LFFSP) of metalloorganic [N(CH2CH2O)3Al, alumatrane, and Al(Acac)3] and inorganic alumina [AlCl3 and Al(NO3)3·9H2O] precursors dissolved in 1:1 ethanol/THF, aerosolized with O2 and ignited can produce quite different alumina nanopowders during the ensuing combustion process. The metalloorganics appear to volatilize and combust easily to give nano-alumina, with particle sizes 70 nm and surface areas of ≈12 m2/g. AlCl3 appears to volatilize easily but does not hydrolyze rapidly in the flame leading to mixtures of alumina and recovered AlCl3. The resulting nanopowders consist of a mixture of transition alumina phases, primarily δ*, that could only be successfully identified and quantified by Rietveld refinement. Because the δ phase is...