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Effects of a modified fluorination treatment (F-treatment), ball-milling in a fluoride solution, on structural and electrochemical characteristics of Zr0.9Ti0.1Mn0.6V0.2Co0.1Ni1.1 alloy were investigated. As a result, it was found that the modified F-treatment improved charge–discharge characteristics such as the initial activation property, discharge capacity and high-rate dischargeability of the alloy. It was also found that the modified F-treatment could effectively deposit Ni species on the alloy surface, compared with the conventional F-treatment. These results suggest that the combination of F-treatment and ball-milling is very effective in forming a Ni-rich surface layer with catalytic activity, leading to improved charge–discharge characteristics. [Copyright &y& Elsevier]