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Amorphous carbon nitride (a-CN x ) films prepared by RF magnetron sputtering technique display a moderate electrochemical reactivity. However, after electrochemical activation by a cathodic pretreatment in acidic solution, they exhibit a quasimetallic behavior. This behavior has been notably assessed by scanning electrochemical microscopy (SECM). The approach curves show that the a-CN x electrode surfaces are made of active and inactive domains. These surfaces have also been characterized by atomic force microscopy (AFM) and XPS. AFM shows that the a-CN x surface roughness remains very low after the activation treatment. XPS analyses indicate that the electrochemical activation of the a-CN x materials is associated with a decrease in the number of superficial nitrogen atoms involved in sp 3 CN bonds.