Fine powders of ZnFe2O4 with an average particle size of 10 nm and inversion parameter of 0.21 were synthesized by the aerogel procedure. Portions of the powders were calcined in air at 500 and 800 degrees C and other portions were ball-milled for 10 h. The materials were characterized by x-ray diffractometry, vibrating sample, and SQUID magnetometry, Mossbauer spectrometry, and low temperature calorimetry. Upon calcination the powders underwent significant changes in grain size, inversion parameter; and hence magnetic properties. The magnetic state of the as-produced and calcined samples is best described as disordered and highly dependent on temperature. Upon ball-milling the grain size varied widely and the inversion parameter attained a value of 0.55. The magnetic properties of the ball-milled sample are similar to those of ferrimagnetic MgFe2O4 powders having comparable grain size and inversion parameters. (C) 1997 American Institute of Physics

The cation site occupancy of a mechanically activated nanocrystalline zinc ferrite powder was determined as (Zn0.552+Fe0.183+)tet[Zr0.452+Fe1.823+]octO4 through analysis of extended x-ray absorption fine structure measurements, showing a large redistribution of cations between sites compared to normal zinc ferrite samples. The overpopulation of cations in the octahedral sites was attributed to the ascendance in importance of the ionic radii over the crystal energy and bonding coordination in determining which interstitial sites are occupied in this structurally disordered powder. Slight changes are observed in the local atomic environment about the zinc cations, but not the iron cations, with respect to the spinel structure. The presence of Fe3+ on both sites is consistent with the measured room temperature magnetic properties.

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