This work deals with the investigation and optimization of the crystalline phases, magnetic properties, chemical composition and morphology of Nd-(Fe1-xCox)-B oxide magnetic particles (where x = 0, 0.05, 0.1, 0.15, 0.2, 0.3, 0.4, and 0.5) synthesized by Pechini method that can be used as a precursor for the production of Nd2(Fe,Co)14B hard magnetic phase. The polymerization mechanism of Pechini process was investigated by Fourier transform infrared (FTIR) and Raman spectroscopy to confirm the formation of metal-CA complexes and successive esterification reactions between citric acid (CA) and ethylene glycol (EG). The chemical composition of the synthesized samples was studied via energy dispersive (EDS) and X-ray photoelectro (XPS) spectroscopy methods. The structure, morphology, and the crystalline phase of resulting Nd-(Fe1-xCox)-B oxide magnetic particles were characterized by Rietveld refinement of X-ray diffraction (XRD) patterns, scanning electron microscopy ( SEM), and high-resolution transmission electron microscopy (HR-TEM) and its selected area electron diffractograms (SAED). The results obtained from the Rietveld refinement of XRD patterns show that (Fe2O3/Fe3O4) phase ratio decreases with the amount of cobalt that can be attributed to the reduction of enthalpy . The SEM micrographs indicate that the oxide particles have an elongated structure with irregular shapes supported by TEM observations. The results of structural analysis by HR-TEM and SAED are consistent with the Rietveld results which confirms the presence of different oxide phases in Nd-(Fe1-xCox)-B oxide particles. The magnetic behaviorstudied by VSM was interpreted by the variances of the morphology, structure and chemical composition of Nd-(Fe1-xCox)-B oxide particles, all of which were influenced by the cobalt content. First‐Order Reversal Curve (FORC) diagrams show that the magnetic interaction between oxide particles decreases as the cobalt content increases.