In this work, iminodiacetic acid-functionalized poly(glycidyl methacrylate)grafted carbon fibers (CCFs) were prepared by electrochemically mediated atom transfer radical polymerization (eATRP) for nano-nickel recovery from spent electroless nickel (EN) plating baths. The adsorption behaviors of Ni2+ were investigated at CCFs in the spent EN plating baths. The adsorption kinetics perfectly fitted pseudo-second order model with a chemisorption process. The thermodynamic parameters suggested that adsorption was feasible, spontaneous, and endothermic. The adsorption maximum capacity was 0.908 mM g(-1) under optimum conditions (pH 5.2, 50 A degrees C and 40 min). The present materials were carefully characterized by the Fourier transform infrared spectroscopy, X-ray diffraction, field emission scanning electron microscope, and electrochemical techniques. Experimental results showed that CCFs were successfully prepared, which were efficient adsorbent and support for nano-nickel recovery from the spent EN plating baths.