The increasing demand for improving the performance of optical devices and the development of nanotechnology have driven research on diffusion films. The preparation of diffusion films with welldefined microstructures can achieve uniform diffusion and scattering of light, thereby improving the efficiency and performance of optical devices. In this study, diffusion films with high transmittance and haze were prepared using PMMA@TiO 2 @SiO 2 (P@T@S) composite microspheres, and the PMMA microspheres and nanoparticles were combined through electrostatic attraction. As compared with PMMA microspheres, the P@T@S composite microspheres displayed better heat resistance as well as swelling resistance. Optical performance data showed that the P@T@S diffusion film had the perfect optical performance with a transmittance up to 90.5% and a haze of 88.3%. The excellent light diffusion effect of the P@T@S diffusion film was experimentally demonstrated, with the light through the film not only displaying the largest area but also maintaining a relatively high brightness. Our findings can provide reference and guidance for further development of light diffusion films, which are of potential application in optoelectronic devices.