A chitosan nanoscaffold in the form of a colloidal solution was obtained from the deacetylation of chitin whiskers under alkaline conditions by using a microwave technique in only 1/7 of the treatment time of the conventional method. Fourier-transform infrared spectroscopy (FTIR) and nuclear magnetic resonance ((1)H NMR) techniques confirm the degree of deacetylation to be above 90% within 3 h. The wide-angle X-ray diffraction (WAXD) pattern clearly shows that the highly crystalline chitin whiskers are changed to amorphous chitosan. SEM micrographs show the aggregation of branched nanofibers, whereas the TEM micrographs reveal the scaffold morphology.