In order to functionally finish diacetate fibers using supercritical CO2 fluid technology, which gives high added value to diacetate fibers, the effects of supercritical CO2 fluid treatment time on surface morphology, chemical structure,aggregation structure,thermal property and tensile strength of diacetate fiber were investigated by means of scanning electron microscope, Fourier infrared spectrometer, X-ray polycrystalline diffractometer, thermogravimetric analyzer, differential scanning calorimetry and universal strength tester. Results show the particulate impurities are removed on the surface of the diacetate fiber treated by supercritical CO2 fluid for 60, 90 and 120 min, and the order of the molecular chain decreased, as well as the crystallinity of diacetate fibers decreases from 39.41% of untreated fiber to 35.33%, 31.57%, 36.10% respectively, and the breaking strength of fiber decreased first and then increased. After 120 min of supercritical CO2 fluid treatment, the breaking strength of hydrogen bond between molecular chains of diacetate fibers shows a slight decrease. The melting point of the diacetate fibers is basically the same, and the mass loss rate of fiber increase from 89.52% to 95.66% in high temperature.