The current investigation deals with the treatment of water pollution that is caused by the leaching of nickel ions from the metallurgical industry and new-energy batteries. Therefore, an eco-friendly treatment of nickel through the use of a composite of cotton stalk biochar with nanozerovalent copper has been presented in this investigation signifying the impact of zerovalent copper in enhancing the adsorption capacity of biochar for nickel adsorption. Thermogravimetric analysis data showed the adsorbent to be significantly stable in the higher thermal range, whereas transmission electron microscopy analysis confirmed the particles to be 27 nm and also showed the cubic geometry of the particles. A much closer scanning electron microscopy analysis shows the morphology of particles to be cubic in shape. Batch adsorption indicated a positive influence of pH increase on adsorption due to the electrostatic attraction between positive nickel ions and post point of zero charge (pHPZC) negative surface of copper biochar composite (pH > 5.5). A high adsorption rate was observed in the first 60 min, whereas adsorption increased with the increase in temperature from 303 to 318 K. Kinetic modeling confirmed the pseudo-first-order to fit best to the data. The apparent activation energy (11.96 kJ mol–1) is indicative of the chemical nature of the process. The adsorption data fitted well to the Langmuir adsorption model. The negative values of apparent ΔG° and the positive values of apparent ΔH° indicate the spontaneity and endothermicity of the process, respectively, whereas the positive values of apparent ΔS° point toward increased randomness during the process. Postadsorption XPS suggests the adsorption of nickel on the surface of biochar composites in the form of Ni(OH)2 and NiO(OH).