NiCuZn ferrites were prepared by the sol-gel self-combustion method. Nanosized, homogeneous and highly reactive powders were obtained at relatively low temperatures. In present work the variations of structural, magnetic, and microwave properties of NiCuZn ferrite nanoparticles were studied as a function of the annealing temperature. The analysis of XRD patterns showed that only the spinel phase is present. Cell parameters slightly vary with thermal treatment while a crystalline size increases. Magnetic nanoparticles were mixed with an epoxy resin for reflectivity studies with a microwave vector network analyzer using the microwave-guide method in the range of 7.5 to 13.5GHz. Static saturation magnetization value (measured by SQUID) and microwave absorption show clear dependence on the annealing temperature/particle size and the absorption maximum moves towards the higher frequencies with an increase in the average size of the particles.