Development of electrospun EVOH fibres reinforced with bacterial cellulose nanowhiskers. Part I: Characterization and method optimization

In the present study, hybrid electrospun EVOH fibres reinforced with bacterial cellulose nanowhiskers (BCNW) were developed and characterized. The nanowhiskers, obtained by sulphuric acid digestion of native bacterial cellulose mats generated by Gluconacetobacter xylinum, were morphologically characterized by SEM and optical microscopy with polarized light and revealed a highly crystalline structure of nanofibrils aggregates. XRD analyses suggested a crystalline structure corresponding to the cellulose I allomorph. It was also confirmed by means of FT-IR spectroscopy that amorphous regions were preferentially digested by the acid treatment, whereas TGA analyses showed a decrease in the thermal stability of the nanowhiskers most likely due to incorporation of sulphate groups and the inherent acidity remaining in the filler even after extensive washing cycles. A method was developed for improving the incorporation of BCNW within the EVOH electrospun fibres, consisting on the addition of the BCNW in the form of a centrifuged precipitate, versus the most conventionally employed freeze-dried nanowhiskers. DSC analyses showed a significant increase in the glass transition temperature of the composites during the second heating run, which may be related to the acidic character of the nanofiller. Finally, sonication was seen to enhance interfacial interaction but to reduce the incorporation of the filler in the matrix in the case of the centrifuged material.