Fe-C materials are made from powder Fe and graphite carbon powder, then determine thecharacteristics of surface morphology, structure, composition by Scanning electron microscopy (SEM),X-ray diffraction (XRD), Energy Dispersive X-ray Spectroscopy (EDX). Materials Fe-C is usedremoval of phenol from aqueous solution by internal microelectrolysis. The results show that withoptimal conditions for phenol decomposition is pH of 4, contact time of 12 hourss, material weight of2,5 g, shaking rate of 200 revolutions per minute (rpm), phenol removal efficiency is 91,54%, with theinitial concentration is 102,90 mg/L. The results show that materials Fe-C can be applied to removephenol from aqueous solution by internal microelectrolysis.Keywords. Internal microelectrolysis, Fe-C, Removel, phenol, Aqueous solution.