Titanium oxide films and powders are attached onto carbon cloths via RF reactive sputtering and an epoxy resin mixture, respectively. TiO2/carbon composite materials were used to investigate the photoelectrochemical degradation of perchlorate ions in water. The energy band gaps of the RF-sputtered TiO2 thin films ranged from 3.35-3.44 eV. A photocurrent of the powdered TiO2 as illuminated by ultra-violet light for 30 min. was 2.79 mA/cm2. Perchlorate ions in water were shown to be degradable by a UV-illuminated TiO2 powder/carbon/Nafion/carbon composite.