Functionalized biomass waste sources of cellulose have drawn attention due to their high availability and sustainability properties. In this work we characterize the structural and flow properties of high-pressure homogenized citrus fiber cellulose dispersions, employing SAXS, rheology and rheo-MRI techniques. The high-pressure treatment disrupts the microfibrillar network within the citrus fibers, but leaves the individual microfibrils intact. Under moderate shear (0.1-100 s^-1) in a confined (<1 mm) geometry, these functionalized citrus fiber cellulose dispersions exhibit thixotropic shear-banding behavior accompanied by cooperative flow of microfibril flocs with correlation lengths ξ ~ 100 μm. The presented findings form a basis towards understanding and manipulating the structural and rheological properties of non-wood biomass cellulose microfibrils under industrially-relevant conditions.

Phospholipid gum mesostructures formed in crude soybean oil after water degumming (WD) and enzymatic degumming (ED) were studied at a range of phospholipid and water concentrations. For ED, phospholipase C (PLC), phospholipase A2 (PLA2) and a mixture of phospholipases Purifine 3G (3G) were used. Both WD and ED resulted in lamellar liquid-crystalline phases, however, of different topology. The dependence of the bilayer spacings (as observed by SANS and SAXS) on the ratio between amount of water and amphiphilic lipids differed for WD and PLA2 ED vs PLC and 3G ED. This difference was also observed for dynamics at molecular scale as observed by time-domain (TD) NMR and attributed to partial incorporation of diglycerides and free fatty acids into gum bilayers after PLC and 3G ED. Feasibility of using TD-NMR relaxometry for quantification of the gum phase and estimation of degumming efficiency was demonstrated.

Pronounced fibres are formed through simple shearing of a dense calcium caseinate dispersion. Both mechanical tests and scanning electron microscopy images demonstrate that the material is anisotropic. It is hypothesised that calcium caseinate aggregates, under shear, align into micro-fibres and bundle further into a hierarchical structure. Yet no direct evidence at the sub-micron length scale can support the assumption. Small angle neutron scattering (SANS) experiments were conducted on calcium caseinate samples prepared at different conditions. Analysis of the SANS data revealed that the micro-fibres have a diameter of ∼100nm and a length of ∼300nm. The addition of enzyme and air contributed to longer and thinner micro-fibres. Furthermore, the extent of fibre alignment at the micro-scale and the macroscopic anisotropy index followed the same trends with varying processing conditions. It is concluded that the material does indeed possess a hierarchical structure and the micro-fibres are responsible for the anisotropy on the macro-scale.

A versatile cell for X-ray and neutron scattering experiments on samples under shear has been designed. To our knowledge, it is the first shear cell which can be used for both SAXS and SANS in respectively synchrotron or reactor beamlines. The cell is mainly intended for scattering experiments in so-called “1–2 plane geometry” but can also be modified into cone–plate and plate–plate rheological geometries, giving access to the 1–3 scattering plane. The latter two geometries, however, can only be used with neutron scattering. The final cell design is compact, which allows it to be used even with lab-based X-ray sources. A special thermostatic shell allows for the temperature control of the samples under investigation in the range from 5 up to 100 °C. Several X-ray and neutron scattering experiments performed with the cell have helped in better understanding of the structuring under shear of food materials, such as: cellulose suspensions, fat crystal networks and milk proteins.