In the present study, hybrid decatungstate based photocatalysts, [(C16H33)N(CH3)3]4[W10O32], were synthesized by the reaction of hexadecyltrimethylammonium surfactant (CTAB) and Na4W10O32.2.6H2O (W10), with different molar ratio W10:CTAB (1:1 for compound 1 and 1:3 for compound 2). In order to verify that the materials have been formed, FTIR, UV-visible spectroscopy, TGA, XRD, and SEM tests were conducted. Comparing and analyzing the influences of molar ratios on band gap energy, photocatalytic activity, and material morphology is discussed. FTIR spectroscopy showed that CTAB reacted with W10 to produce an insoluble product in aqueous media. According to UV-visible spectroscopy, the hybrid material with a low amount of CTAB absorbs more light in the visible region than the other, with the optical band gap decreasing to 2.42 eV for compound 1. After 7 hours of exposure, both compounds, compound 1 and 2, demonstrated a 46 and 88% degradation of carbamazepine in aqueous solution using UV-visible photocatalysis.