Microscopic Characterization of Cellulose Nanocrystals Isolated from Sisal Fibers

Isolation of cellulose nanocrystals (CNCs) was carried out by unrepeated or repeated alkalization and bleaching followed by sulfuric acid hydrolysis and air cooling (unrepeated) or ice cooling (repeated). The influence of unrepeated and repeated alkalization and bleaching, and cooling rate (cooling medium) after hydrolysis on the morphology and crystallinity of the isolated micro- and nano-celluloses were characterized. Scanning electron microscopy (SEM) showed that repeated alkalization and bleaching led to a higher degree of fibrillated microcellulose (~10 mm) with higher surface roughness than unrepeated alkalization and bleaching. Transmission electron microscopy (TEM) revealed that air and ice cooling after acid hydrolysis producing different CNCs morphologies; heterogeneous CNCs nanowhisker and nano-spherical (~50 nm), and homogenous CNCs nanowhiskers (~50 nm width and ~500 nm length), respectively. The homogeneous nano whisker was related to single phase monoclinic b-cellulose. Residual lignin agglutinating between the nanoparticles was observed in TEM image as well as in Fourier transform infrared (FTIR) spectra. The existence of residual lignin after hydrolysis is comparable in crystalinity (crystallinity index, I c : ~91%) with that of isolated CNCs, as confirmed by x-ray diffraction (XRD) analysis.