Abstract: To improve mechanical properties of microcapsules and reduce the release rate of core materials, neroli oil microcapsules were prepared by fabricating a melamine formaldehyde resin shell modified by poly(vinyl alcohol) (PVA) filled with Fe3+-, Zr4+- and Ce4+-doped TiO2 nanoparticles through in-situ polymerization. The effect of doped TiO2 nanoparticles on morphology and mechanical and thermal properties of the resulting microcapsules were investigated by Fourier-transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy and transmission electron microscopy. The results indicated that the release rate of the core material was reduced with the addition of doped TiO2 nanoparticles into the wall material. When 0.5 wt % of Fe3+-doped TiO2 nanoparticles was incorporated into the wall, the microcapsules achieved a cracking rate of 18.1 % and a release rate of 4.5 %.