AbstractIn this work, α-cellulose was extracted from Phyllostachys nidularia Munro using an acidified sodium chlorite treatment followed by alkali treatments, and cellulose nanofibers (CNFs) were then extracted from α-cellulose via the combination of sulfuric acid (64 wt%) and low-intensity ultrasonication. The results showed that superior CNFs were successfully extracted and their diameters were in the range of 5 to 20 nm. Fourier transform infrared spectroscopy (FTIR) suggested that a majority of the hemicellulose and lignin were removed from the original material and that the chemical constituents of α-cellulose and CNFs were similar. X-ray diffraction (XRD) analysis indicated that the relative crystallinity of CNFs was significantly increased to approximately 69.32% and all specimens presented a typical cellulose I crystal form. Thermogravimetric analysis (TGA) showed that the thermostability of the CNFs was greatly increased.