AbstractNatural fibers such as kenaf have been studied extensively as a reinforcing phase and received major attention recently due to their renewability, biodegradability, and high strength comparable to other synthetic fibers. In this study, nano-crystalline cellulose (NCC) was produced from kenafcore wood using the acid hydrolysis method. Kenaf core was alkali treated with a 4 wt% of sodium hydroxide solution and subsequently bleached using sodium chlorite in acidic buffer. The resulting white, bleached kenaf core was hydrolyzed in 64 wt% sulfuric acid (H2SO4) to obtain NCC. The resulting NCC suspension was characterized using X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Fourier transform infrared (FTIR) analysis, and scanning transmission electron microscope (STEM). Hydrolysis with highly concentrated H2SO4 further increased the crystallinity of bleached kenaf core cellulose and reduced the dimension of cellulose to nano scale. FTIR results showed that with each subsequent treatment, hemicellulose and lignin were removed, while the chemical functionalities of cellulose remained after the acid hydrolysis treatment. XRD peaks shown by bleached kenaf core were characteristic of cellulose I, which was reaffirmed by the DSC results. The diameters of NCC obtained from kenaf core were found to be in the range of 8.5 to 25.5 nm with an average aspect ratio of 27.8.