Crystallization and shear modulus of a forming biopolymer film determined by in situ x-ray diffraction and ultrasound reflection methods

The structure and the rigidity of a forming biopolymer film were determined using concurrent x-ray diffraction and ultrasonic reflection measurements. Film formation of a xylan solution (de-ionized water, 10g∕l xylan, 4g∕l glycerol) was studied during water evaporation at 24(±2)°C, 37(±5)%RH. X-ray diffraction (XRD) data showed the crystallization and ultrasonic data the increase of the shear modulus (G) during water evaporation. Xylan crystallized into small xylan dihydrate crystallites, the number of which increased as water evaporated. Crystallization began earlier than the increase in G during film formation. The increase in G also continued after the crystallites were fully formed, indicating still ongoing structural changes in the amorphous parts. The maximum value of G was 0.1–0.5GPa. XRD measurements performed ex situ showed a crystallinity of 16%–19% (±5%) and a fairly isotropic crystallite orientation in the surface plane of the films.