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The hydrothermal method was used to dope different amounts of Co2+, Mn2+, and Cu2+ in nano-nickel zinc ferrite powder. X-ray diffraction (XRD), a scanning electron microscopy (TEM), and a vector network analyzer (VNA) were used to explore the influence of doping on particle size, morphology, and electromagnetic wave absorption performance. Pure nanometer cobalt nickel zinc ferrite phase was prepared using the hydrothermal method with an increasing Co2+ content. Results showed that the grain type structure changed from a spherical structure to an irregular quadrilateral structure with the average particle size increasing from 35 nm to 60 nm. The lattice constant increased from 0.8352 to 0.8404 nm with Co2+ doping. The increasing Co2+ can change the position of the absorption peak, increase the bandwidth of the absorber, and improve the performance of the materials in GHz low frequency. The doping ratio of Mn2+ can affect the size of the lattice constant, but nanocrystals are easy to reunite without improving the electromagnetic loss. However, the absorbance performance decreases. For the doping of Cu2+, there is an agglomeration phenomenon. When the doping quantity is 0.15, the absorbing wave performance becomes better.