AbstractThis article describes a novel one-step method to prepare cellulose nanocrystals (CNCs) from bleached bagasse pulp via ammonium persulfate (APS) oxidation. The obtained persulfate oxidation cellulose nanocrystals (POCNs) were characterized for their microstructure, crystal properties, and chemical composition. The POCNs were successfully prepared with a total yield of 44.6%. Transmission electron microscopy (TEM) and atomic force microscopy (AFM) measurements indicated that the POCNs had an average length of 150 to 300 nm and an average width of 10 to 30 nm, as well as a rod-like morphology. Fourier transform infrared (FTIR) spectroscopy confirmed the introduction of carboxyl groups on the surface of cellulose. The X-ray diffraction (XRD) spectra proved the existence of cellulose type I, with a highly crystalline nature (79.2%), and thermogravimetric analysis (TGA) showed that the thermal stability decreased.