The structure and magnetic behavior of nanostructured powders of stoichiometric NiZn ferrite, Ni0.5Zn0.5Fe2O4, synthesized by coprecipitation, are investigated by extended x-ray-absorption fine structure spectroscopy (EXAFS), x-ray diffraction, Mossbauer spectroscopy, and vibrating sample magnetometry. Samples of high purity and high homogeneity were obtained by annealing at relatively low temperatures (300-800 degrees C) resulting in nanoparticles with average diameter between 9 and 90 nm, as determined by x-ray diffraction. EXAFS was applied to follow Ni, Zn, and Fe cations distribution and the evolution of the short range order of the samples with increasing annealing temperature. Our results show ferrimagnetic NiZn ferrite nanosized powders with high purity, 1:1 Ni to Zn stoichiometric ratio and superparamagnetic behavior. Moreover, the samples exhibit good structural ordering already after heat treatment at 400 degrees C. Analysis by vibrating sample magnetometry indicated a critical particle diameter for the transition from monodomain to multidomain behavior close to 40 nm. (C) 2000 American Institute of Physics. [S0021-8979(00)08309-2].