Titanium dioxide (TiO2) has fascinating properties such as chemical stability, corrosion resistance and non –toxicity. Tiatanium dioxide which exists in four crystal forms namely, anatase, rutile, brookite and titanium dioxide (B), is one of the most frequently used photocatalysts. Activated carbon is an important carrier and support for the titanium dioxide. Using activated carbon as a catalyst support will improve the photocatalytic properties of titanium dioxide nanoparticles by increasing their degree of exposure to neighboring materials. High surface area and porous structure of activated carbon nanofibers make them an ideal photocatalyst carrier. The preparation of the titanium dioxide nanoparticles in the nanometer range can be conducted through the hydrolysis and condensation of titanium alkoxides. Titanium isopropoxide (TIPP) is one of the most widely used titanium alkoxides as a titanium source. In the present work, titanium dioxide nanoparticles were generated in–situ, in activated carbon nanofibers. In an in - situ formation process, the metal oxide particles are generated from the precursors, already embedded in the matrix polymer. In-situ process has advantages such as, high content of titanium dioxide nanoparticles in activated carbon/titanium dioxide nano composite nanofibers as well as low aggregation of titanium dioxide nanoparticles.