Abstract: Electrocatalytic reduction of oxygen for in-situ electrogeneration of H₂O₂ remains a challenge, but it is attractive for potential applications in advanced oxidation processes. In this study, in order to overcome the limitation of working pH for traditional Fenton and electro-Fenton processes, we successfully synthesized a self-supporting nitrogen-doped carbon material (X/N@C-CC, X=550, 750, 950) via calcination at a specified temperature, using Cd as the sacrificial metal and carbon cloth as the substrate. The cathode made with this material is capable of generating H₂O₂ in-situ in a wide pH range (3-10), and the combination of the cathode with UV for carbamazepine (CBZ) degradation was investigated. The results show that: (1) The prepared cathode material has high content of doped nitrogen, which is greatly affected by the calcination temperature. For the investigated temperatures, 750 ℃ is the optimal one, at which Cd is almost completely volatilized, the nitrogen content is 8.89%, and only pyridine nitrogen and graphitic nitrogen are present. In addition, the increase in calcination temperature has little effect on the oxygen content of carbon materials. (2) The C=O and —COOH functional groups are detected at all temperatures, which may guarantee the superior performance of electrogeneration of H₂O₂ at alkaline pH condition. (3) Under the optimum conditions, the H₂O₂ yield of 750/N@C-CC can reach 73.09 mg/(L·h). In addition, the coupled UV-electrocatalytic H₂O₂ system can completely degrade 10 µmol/L CBZ within 20 minutes at pH 3, 6, or 10. The results of free radical scavenging experiments and electron paramagnetic resonance (EPR) spectra tests show that the main oxidative species responsible for CBZ destruction is ·OH. In conclusion, this system can effectively avoid the problems of sludge production, pH limitation, and formation of toxic by-products associated with the traditional Fenton process. It shows promises for treating wastewater containing emerging organic pollutants (e.g., CBZ).