This study investigates the synthesis and characterization of Ni-Zr melamine based coordination polymer (CP) modified using charcoal by mechanochemical synthesis. The materials were analyzed using XRD, SEM-EDS, BET, TGA, and FTIR techniques. The results show that Ni-Zr melamine CP exhibit significantly enhanced surface area at (1178.176 m²/g) and porosity (2.800 nm) compared to the pure melamine ligand (83.803 m²/g). The incorporation of charcoal further increased the surface area to 1873.196 m²/g and pore diameter to 3.120 nm. TGA analysis indicated improved thermal stability of the CP, with total weight loss of 7% compared to 17% of the melamine ligand. X-ray diffraction analysis showed distinct peaks of Ni-Zr melamine at 27.7^o and 29.58^o, contrasting with pure melamine’s broader peak range (13-55^o) , which suggests new crystalline phases due to metal ligand interaction. The charcoal-modified composite exhibited a lower angle XRD peak (3-36^o), indicating increase disorder and charcoal-induced structural changes. Fourier transform infrared spectroscopy identified characteristic N-H, C≡N, and C=O vibrations, with new peaks in the composite (2849 cm^-1) indicating the influence of charcoal. Scanning electron microscopy revealed a complex, agglomerated morphology for the composite compared to the uniform crystalline structure of pure melamine, highlighted enhanced porosity. Energy-dispersive X-ray spectroscopy revealed dominant nitrogen (77.91%) and carbon (17.64%) content, consistent with melamine chemical composition (C₃H₆N₆), with trace impurities (Al, Na, Mg, Ti, Si) suggesting residual contaminants. The study highlighted the synergistic effects of combining CP with charcoal, leading to enhanced material properties and performance. Ni-Zr melamine CPs, especially those modified with charcoal, demonstrated promising characteristics for various environmental applications.