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.

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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.

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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.

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Humanity needs to increase use of renewable sources of materials and energy. Biomass can be used for both of these needs. Cellulose is the main component of biomass. Understanding the multi-level hierarchical structure of cellulose holds the key tomultiple applications of this material. One of the promising applications of lignocellulsic biomass is the production of bioethanol as a replacement for fossil fuels. Yearly production of biomass could potentially supply enough bio-ethanol to completely replace gasoline. However, it would require dramatic increase in the efficiency of the bioethanol production. The main obstacle to the development of bioethanol production into a sustainable process is the recalcintrance of cellulose which was developed throughout entire plant evolution. In order to overcome this obstacle an important step was incorporated into the process, i.e. pretreatment of biomass. Amultitude of pretreatments have been developed and applied to disrupt the structure of lignocellulosic biomass. However it is still not clear, which structural parameters are responsible for the success of a certain pretreatment technique.@en

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.

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Submicron- and micron-scale structures of composite hydrogels based on bacterial cellulose (BC) and polyacrylamide (PAAm) were studied by spin-echo small-angle neutron scattering (SESANS) and cryo-scanning electron microscopy (cryo-SEM). These hydrogels possessing the structure of interpenetrating polymer network were synthesized via free-radical polymerization of acrylamide carried out in the pellicle of BC swollen in the reaction solution. No neutron scattering was observed for the samples swollen in heavy water to the equilibrium state, but the SESANS signal appeared when TbCl3 salt was added to the solvent. It is the unusual effect, which may be very helpful for SESANS studying of other hydrogel systems. The SESANS dependences obtained for these samples revealed the anisotropy of mesostructure for the hydrogels under investigation. Density inhomogeneities on the characteristic scale of 11.5 ± 0.5 μm were detected in one fixed orientation of the sample, i.e., with the growth plane of BC parallel to the plane formed by the neutron beam and the spin-echo length. The uniaxial anisotropy revealed agrees with a recently proposed model, which attributes this behavior to the existence of tunnel-like oriented structures inside BC. The evidence of such type of mesostructure anisotropy of BC and BC-PAAm hydrogels was obtained by using the cryo-SEM method.@en

Small-angle neutron scattering (SANS) on nuclei of chicken erythrocytes demonstrates the cubic dependence of the scattering intensity Q−3 in the range of momentum transfer Q∈10−3–10−2nm−1. Independent spin-echo SANS measurements give the spin-echo function, which is well described by the exponential law in a range of sizes (3×102)–(3×104) nm. Both experimental dependences reflect the nature of the structural organization of chromatin in the nucleus of a living cell, which corresponds to the correlation function γ(r)=ln(ξ/r) for r<ξ, where ξ=(3.69±0.07)×103 nm, the size of the nucleus. It has the specific scaling property of the logarithmic fractal γ(r/a)=γ(r)+ln(a), i.e., the scaling down by a gives an additive constant to the correlation function, which distinguishes it from the mass fractal, which is characterized by multiplicative constant.@en