Fine powders of ZnFe2O4with 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 °C and other portions were ball-milled for 10 h. The materials were characterized by x-ray diffractometry, vibrating sample, and SQUID magnetometry, Mo¨ssbauer 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 MgFe2O4powders having comparable grain size and inversion parameters. ©1997 American Institute of Physics.