Concentration effect of TEMPO-oxidized nanofibrillated cellulose aqueous suspensions on the flow instabilities and small-angle X-ray scattering structural characterization

The rheological behavior of 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO)-oxidized nanofibrillated cellulose (NFC) suspensions at different concentrations were examined using Couette with smooth and serrated surfaces and vane-in-cup geometries. A slippage against the walls of rheometer rotor or/and stator (wall-slip) as well as flow localization within a specific volume of the sample (shear banding) took place. These phenomena were visualized using a technique based on introduction of titanium dioxide pigment into the specific volume of NFC suspension and monitoring its deformation. The flow instabilities appeared more pronounced with an increase of the NFC concentration. It was shown that the use of serrated geometry is necessary to compete with the wall-slip but is not sufficient to prevent it completely. Serrated Couette was found to be the most appropriate geometry (among the tested) to measure the rheological properties of NFC suspensions. Small-angle X-ray scattering was used to provide a supplementary information about the structural organization of NFC suspensions. The statistical average diameter of 4.8 nm was determined from the scattering data for the NFC swollen in water.