Rj. Willey et al., PREPARATION AND CHARACTERIZATION OF MAGNESIUM CHROMITE AND MAGNESIUM FERRITE AEROGELS, Chemical engineering communications, 123, 1993, pp. 1-16
A supercritical drying process has been used to prepare MgO-Cr2O3 and
MgO-Fe2O3 powders from a mixture of magnesium acetate and the metallic
acetylacetonates hydrolyzed in a methanolic solvent. The resultant ae
rogels have small particle sizes in the range of 10 to 20 nm and high
surface areas in the range of 50 to 250 m2/g. After removal from the a
utoclave, characterization by X-ray diffraction (XRD) showed that the
MgO-Cr2O3 was amorphous and that the MgO-Fe2O3 was readily in the form
of a spinel structure for magnesioferrite (MgFe2O4). Fourier transfor
m infrared spectroscopy (FTIR) and thermogravimetric and differential
thermal analyses (TG-DTG-DTA) showed a high level of retained surface
methoxy and carboxylate species for the MgO-Cr2O3 aerogel (over 40% by
weight). The MgFe2O4, on the otherhand, had less than 10% organic mat
ter. The differences observed between MgO-Cr2O3 and MgFe2O4 have been
attributed to the formation of Cr+6 in the former case. After heating
in air at 970K. MgO-Cr2O3 crystallized to the spinel structure MgCr2O4
. The IR transmittance of pressed disks of MgFe2O4 aerogel showed beha
vior typical for a n-type semiconductor. The MgCr2O4, however, was a p
-type semiconductor due to mainly Cr+6 present on the surface. Lewis a
cid centers were prevalent on both materials. The acid strength was fo
und to be higher on the MgFe2O4 compare to the MgCr2O4.