In our previous study, we found that Ti(OH)(4) exhibited fluoride ion exchange properties. In order to improve the ion exchange capacity, mesoporous Ti oxohydroxide (TiOx(OH)y) had been prepared by using dodecylamine as template. Zirconia and silica had been introduced into the mesoporous Ti oxohydroxide to enhance the ion exchange capacity. The mesoporous structure and the morphology of the mesoporous materials obtained were confirmed using XRD and SEM, respectively. A fluoride ion exchange study was done on each sample. Results showed that mesoporous Ti oxohydroxide containing zirconia exhibited the highest fluoride ion exchange capacity, as it has the smallest particle size, with high uniformity among the mesoporous materials prepared.