Abstract: In the present investigation, we successfully prepared superhydrophobic cotton fibers featured with rich micro-nano structure and sustained-release capability to fragrance via successive decoration of cotton fiber surface using TiO₂ particles formed by sol-gel approach and in-situ grown ZIF-67 crystals, followed by impregnation with heptane solution that contains polydimethylsiloxane (PDMS) and menthol. The static water contact angle of the as-prepared superhydrophobic fragrance sustained-release cotton fibers was measured to be 153.4°. The morphology, composition and hydrophobic properties of the as-prepared superhydrophobic cotton fibers were characterized by field emission scanning electron microscope (FESEM), X-ray photoelectron spectra (XPS) and contact angle goniometer. The sustained-release capabilities of the superhydrophobic cotton fibers to menthol were investigated. After the superhydrophobic cotton fibers containing menthol were stored in air for 10 days, the retention percentage of menthol in the superhydrophobic cotton fibers was still as high as 81.74%, with the average release rate of 1.83%/d. The sustained-release performances of our superhydrophobic cotton fibers were significantly better than those of pristine cotton fibers (the average release rate: 6.77%/d). After washed with water, the loss of menthol in the superhydrophobic cotton fibers was only 2.93%, which was substantially lower than that in the washed pristine cotton fibers (72.08%).