In this study, the synthesis and characterization of epoxidized natural rubber / Titanium dioxide (ENR-25/TiO2) composites in two different solvent (Toluene and Chloroform) via sonication technique was conducted using Fourier transform infrared spectroscopy (FTIR) and Field Emission Scanning Electron Microscopy (FESEM). Spectroscopy results showed new peak at 1662 cm-1 for both ENR-25/Titania composite films, which is related to weak C-O stretching vibration. Moreover, The peak at 3390.4 cm-1 and 3384.3 cm-1 of the composites are produced by Ti-OH stretching vibration shifts. The composite with toluene solvent showed poor dispersion of TiO2, which can be seen by the agglomeration embedded in the matrix. The composite with chloroform showed same trend of composite with toluene. The poor TiO2 dispersion in the composite can be observed by the surface as bright layers. These layers appeared because the TiO2 particles covered the surface of purified ENR-25 matrix.