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The main objective of this research is to utilize fiber waste from palm empty fruit bunch provided very abundant in Aceh. For that needs to be studied and researched other benefits are more valuable. Among them is a source of raw material to produce nanocrystalline cellulose (NCC), a material in nanometer dimensions which can be used as fillers or reinforcing a matrix in order to provide bionanocomposites. NCC isolated from palm empty bunch fiber through the hydrolysis of sulfuric acid, using a solvent mixture of DMAC/LiCl, were passed on activated dialysis membrane after centrifugated to release it from solvent. NCC will be characterized include aspect ratio, morphology, thermal, structural test, and several other physical parameters. The end product is characterized by means of thermogravimetric analysis (TGA), Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD), Differential Scanning Calorimetry (DSC) and Scanning Electron Microscopy (SEM). From XRD and FTIR analysis showed that the nanocrystalline cellulose formed was nanocellulose I with an average size of 72 nm. DSC and TGA thermal test showed that the glass transition, melting point, and decomposition temperature of NCC were 109.59 o C, 191.28 ° C, 210 oC, respectively.