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In this work, neodymium substituted gadolinium-cobalt ferrite nanoparticles were synthesized by hy-drothermal method. The significant role of doping both the Nd3+ and Gd3+ ions to cobalt ferrite in manipulating the cation distribution and further in influencing structural and magnetic properties was experimentally studied and reported. The influence of Nd3+ substitution was investigated with step of 0.02-0.1 into the optimized Gd-Co compound. The crystal structure formation and crystallite size were explored by X-ray diffraction analysis in which the crystallite size and lattice constant decrease with increasing the Nd3+substitution. The microstructural properties were studied by field emission scanning electron microscopy and atomic force microscopy studies. The obtained structural and morphological results reveal that the substitution of Nd3+with more than 0.06 into the Gd-Co ferrites will change the material behavior and trends. The saturation magnetization and coercivity values were measured using a vibration sample magnetometer at room temperature. Comparative microwave absorption experiments demonstrate that the reflection loss properties enhance with increasing substitution of Nd3+cations in Gd-Co ferrite spinel structure. This research reports that the as-prepared Nd3+substituted Gd-Co ferrite compound stands as promising candidate for absorbing electromagnetic wave with a wider absorbing bandwidth of X-band.