The preparation of NiCo/NPC composites and their wave absorbing properties were studied. With the rapid development of electronic communication equipment, electromagnetic pollution has become a significant problem. Metal–organic frameworks (MOFs) have advantages such as simple synthesis, low cost, large specific surface area, and high porosity. The derived porous carbon/magnetic metal particle composites (NPC) overcome the problem of uneven dispersion of magnetic particles. In this study, NiCo-MOF-74 was synthesized by solvothermal method and then carbonized to prepare NiCo/NPC composites. The effects of Ni/Co molar ratio on the morphology, graphitization degree, magnetic properties, and wave absorption properties of the composite were investigated. The results showed that with increasing Co content, the graphitization degree of the carbon component increased, leading to enhanced ferromagnetic properties. The wave absorption properties of NiCo/NPC composites first increased and then decreased with increasing Co content. When the paraffin filling ratio was 50% (mass fraction) and the Ni/Co molar ratio was 1:1, the NiCo/NPC composites had the best wave absorption properties. The optimal reflection loss of Ni1Co1/NPC composite at 16.96 GHz with a thickness of 2 mm was -50.8 dB, and the effective absorption bandwidth was 4.56 GHz (13.44–18 GHz). MOFs materials, as precursors, contain magnetic metal ions and organic ligands that can serve as metal and carbon sources. By undergoing carbonization treatment, magnetic metal/carbon composites can be obtained, offering a simple and efficient synthesis process. MOFs materials are highly ordered crystalline materials with distinct pore structures. After carbonization, MOFs materials can undergo in situ transformation to yield well-dispersed metal nanoparticles within the carbon matrix, which is advantageous for enhancing impedance matching and attenuation properties of the composite materials. Although magnetic metal/carbon composites prepared by MOFs-derived methods have demonstrated significant advantages in the field of electromagnetic wave absorption, there are still issues with uneven distribution of magnetic metal particles and variations in particle size within the composite materials. Therefore, based on MOFs-derived methods, the regulation of chemical composition ratios and optimization of material structures have become the research focus and challenges in this direction. In this paper, the MOFs derivatization method was used to optimize the microstructure of bimetallic NiCo-MOF-74 material by carbonizing the magnetic metal core wrapped in porous carbon. At the same time, the ferromagnetism of the material was optimized by changing the molar ratio of Ni and Co ions. NiCo/NPC composites were prepared by using the synergistic effect between metal ions to make the magnetic metal particles evenly distributed. XRD, SEM and TEM were used to study the effect of Ni/Co molar ratio on the structureThe preparation of NiCo/NPC composites and their wave absorbing properties were studied. With the rapid development of electronic communication equipment, electromagnetic pollution has become a significant problem. Metal–organic frameworks (MOFs) have advantages such as simple synthesis, low cost, large specific surface area, and high porosity. The derived porous carbon/magnetic metal particle composites (NPC) overcome the problem of uneven dispersion of magnetic particles. In this study, NiCo-MOF-74 was synthesized by solvothermal method and then carbonized to prepare NiCo/NPC composites. The effects of Ni/Co molar ratio on the morphology, graphitization degree, magnetic properties, and wave absorption properties of the composite were investigated. The results showed that with increasing Co content, the graphitization degree of the carbon component increased, leading to enhanced ferromagnetic properties. The wave absorption properties of NiCo/NPC composites first increased and then decreased with increasing Co content. When the paraffin filling ratio was 50% (mass fraction) and the Ni/Co molar ratio was 1:1, the NiCo/NPC composites had the best wave absorption properties. The optimal reflection loss of Ni1Co1/NPC composite at 16.96 GHz with a thickness of 2 mm was -50.8 dB, and the effective absorption bandwidth was 4.56 GHz (13.44–18 GHz). MOFs materials, as precursors, contain magnetic metal ions and organic ligands that can serve as metal and carbon sources. By undergoing carbonization treatment, magnetic metal/carbon composites can be obtained, offering a simple and efficient synthesis process. MOFs materials are highly ordered crystalline materials with distinct pore structures. After carbonization, MOFs materials can undergo in situ transformation to yield well-dispersed metal nanoparticles within the carbon matrix, which is advantageous for enhancing impedance matching and attenuation properties of the composite materials. Although magnetic metal/carbon composites prepared by MOFs-derived methods have demonstrated significant advantages in the field of electromagnetic wave absorption, there are still issues with uneven distribution of magnetic metal particles and variations in particle size within the composite materials. Therefore, based on MOFs-derived methods, the regulation of chemical composition ratios and optimization of material structures have become the research focus and challenges in this direction. In this paper, the MOFs derivatization method was used to optimize the microstructure of bimetallic NiCo-MOF-74 material by carbonizing the magnetic metal core wrapped in porous carbon. At the same time, the ferromagnetism of the material was optimized by changing the molar ratio of Ni and Co ions. NiCo/NPC composites were prepared by using the synergistic effect between metal ions to make the magnetic metal particles evenly distributed. XRD, SEM and TEM were used to study the effect of Ni/Co molar ratio on the structure