This study aims to overcome the limitations of powder catalysts in the photocatalytic degradation of organics in a marine environment. To achieve this, coconut shell activated carbon (AC) particles were utilized as a carrier to grow Ti(OH) 4 nanofibers. Er 3+ and Yb 3+ ions were introduced into the nanofibers through ion permeation, solving the problem of preparation caused by the mismatch of ionic radii and enhancing the utilization of infrared light in the solar spectrum. The results of photocatalytic degradation in seawater demonstrated that Er 3+ -Yb 3+ in the lattice enhanced the photocatalytic activity more effectively than supported Er 2 O 3 -Yb 2 O 3 . Additionally, during the calcination process, more oxygen vacancies (OVs) were conveniently introduced into TiO 2 through self-generated CO, further improving the separation of excited electron−hole pairs. The introduction of more OVs exhibited significantly higher generation rates and steady-state concentrations of 1 O 2 and • OH in seawater. Quenching experiments revealed that the presence of 1 O 2 , • OH, holes, and O 2•− all contributed to the degradation efficiency with their relative contributions depending on the specific compound. The AC-supported high-performance TiO 2 nanofibers display great potential for applications in the photocatalytic degradation of organics in a marine environment.