The spherical NiZn ferrite particles were prepared by ultrasonic spray pyrolysis with mixed solution of aqueous metal nitrates. The NiZn ferrite particle was observed with nano-sized primary particles of about 10 nm or less before annealing which represented as paramagnetic behavior measured at 77 K and room temperature. The typical abnormal growth of primary particles like polyhedral primary particles was observed by annealing at 1273 K with Zn-concentration dependency. The XRD patterns showed good crystallinity of NiZn ferrite powder after annealing. In annealing process, the intra-particle sintering phenomenon was observed and the spherical particle morphology was collapsed at 1673 K. The saturation magnetization of NiZn ferrite powder for each annealing temperature was decreased with measuring temperature of $77{sim}$300K.