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The structural, magnetic, and dielectric properties of Yb ions substituted Ca-hexaferrites (Ca-HFs) synthesized using the citrate sol–gel method were studied. XRD and SEM, techniques were used to evaluate the size and shape of the samples. X-ray powder diffraction (XRD) patterns of prepared samples revealed the production of a single M-type single phase hexagonal ferrite with space group 167: R-3c, hexagonal of P63/mmc for structural characterization. Using a scanning electron microscope, the surface morphology of the particle was investigated, and the particle size was determined (SEM). FTIR spectra confirmed the iron–oxygen bands of X-type hexagonal ferrites at tetrahedral and octahedral sites. The high influence of Yb+3 substitutions on the FTIR spectra further confirmed that the dopants play a significant role in these ferrites. The electrical and dielectric properties of Yb substituted Ca-HFs were investigated using the complex impedance spectroscopy technique at various temperatures, frequencies, and substitution ratios. Yb substitution was discovered to have a significant impact on dielectric loss, dielectric constant, Ac conductivity, and dissipation factor. It was fascinating to see how Ytterbium replacement resulted in a significant improvement in magnetic characteristics. With a given substitution ratio, activation energy levels can be altered to a certain level. The Verway Hopping Model, Maxwell Wagner Model, and Koop's theory were used to describe the conduction and polarization mechanisms. The trend was also influenced by the substitution of Yb. Eddy current losses, devices like Multi-Layer Chip Inductors (MLCI), and other microwave applications can benefit from the achieved ranges of both features. [ABSTRACT FROM AUTHOR]