This research focuses on the isolation of MCC (microcrystalline cellulose) into NCC (nanocrystalline cellulose) by acid hydrolysis process. The sulfuric acid hydrolysis (44 wt.% H2SO4) aims to fibrillation from MCC into NCC material. NCC has good properties such as high-surface-area, high-aspect-ratio, weight light, and reactive materials. The morphology of NCC was characterized by SEM (Scanning Electron Microscope) and TEM. The physical characterization was tested using FTIR, XRD, and TGA. The morphological result showed that the particle size of NCC was more homogeneous with a diameter size of 25±3 nm with 310±5 nm in length. The physical properties of NCC better slightly than MCC, indicated by the increasing crystallinity index value from 74.8 to 76.4%, and it has a high thermal resistance of 330°C.