The aim of this study was to investigate the effect of the diffusion layer of a gas diffusion cathode (GDC) on H 2 O 2 production to enhance carbamazepine removal using the electro-Fenton process. The diffusion layer was made by carbon black and polytetrafluoroethylene with sodium sulfate (Na 2 SO 4 ) as a pore former. Different ratios of Na 2 SO 4 to carbon black (w/w) (i.e., 0%, 50%, 100%, 150%, and 200%) in the diffusion layer were tested. With an increase of the ratio, the average pore size in the diffusion layer and the electro-activity in the GDC increased simultaneously, which resulted in a higher mass transfer coefficient ), mainly attributable to the diffusion layer modified by the pore former, which accelerated oxygen transfer and boosted H 2 O 2 production. The results from this study should be useful to remove carbamazepine from wastewater treatment using the electro-Fenton (EF) process with improvement of pore structure in the diffusion layer of GDC.