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Nanocomposite fibers were prepared from chitin whiskers (ChWs) as the reinforcing phase and poly(vinyl alcohol) (PVA) as the matrix. Colloidal suspensions of ChWs, obtained by acid hydrolysis of chitin from crab shell, were thoroughly mixed with aqueous PVA. The homogeneous PVA-ChW suspensions were gel-spun into a methanol coagulating bath. Wide-angle X-ray diffraction patterns evidenced the orientation of ChWs along the fiber axis. From differential scanning calorimetry, the crystallinity of the PVA component was found to increase with ChW loading due to the possible dragging of PVA chains adhering to ChWs during vertical extrusion. The non-isothermal crystallization peak of PVA was observed to shift to lower temperature with ChW loading indicating interfacial interactions between PVA and ChW. Further interaction between PVA and ChW was evidenced by the shifting of the Fourier transform infrared bands of PVA to lower wavenumber and the dynamic tan δ peak, corresponding to α-relaxation of PVA, shifting to higher temperature. The interaction of ChWs with the matrix PVA yielded a significant enhancement in the mechanical properties of the nanocomposites. Copyright © 2012 Society of Chemical Industry [ABSTRACT FROM AUTHOR]