The plant cell wall is a dynamic network of several biopolymers and structural proteins including cellulose, pectin, hemicellulose and lignin. Cellulose is one of the main load bearing components of this complex, heterogeneous structure, and in this way, is an important regulator of cell wall growth and mechanics. Glucan chains of cellulose aggregate via hydrogen bonds and van der Waals forces to form long thread-like crystalline structures called cellulose microfibrils. The shape, size, and crystallinity of these microfibrils are important structural parameters that influence mechanical properties of the cell wall and these parameters are likely important determinants of cell wall digestibility for biofuel conversion. Cellulose-cellulose and cellulose-matrix interactions also contribute to the regulation of the mechanics and growth of the cell wall. As a consequence, much emphasis has been placed on extracting valuable structural details about cell wall components from several techniques, either individually or in combination, including diffraction/scattering, microscopy, and spectroscopy. In this review, we describe efforts to characterize the organization of cellulose in plant cell walls. X-ray scattering reveals the size and orientation of microfibrils; diffraction reveals unit lattice parameters and crystallinity. The presence of different cell wall components, their physical and chemical states, and their alignment and orientation have been identified by Infrared, Raman, Nuclear Magnetic Resonance, and Sum Frequency Generation spectroscopy. Direct visualization of cell wall components, their network-like structure, and interactions between different components has also been made possible through a host of microscopic imaging techniques including scanning electron microscopy, transmission electron microscopy, and atomic force microscopy. This review highlights advantages and limitations of different analytical techniques for characterizing cellulose structure and its interaction with other wall polymers. We also delineate emerging opportunities for future developments of structural characterization tools and multi-modal analyses of cellulose and plant cell walls. Ultimately, elucidation of the structure of plant cell walls across multiple length scales will be imperative for establishing structure-property relationships to link cell wall structure to control of growth and mechanics.

/pdf/progress-and-opportunities-in-the-characterization-of-3oihacrohg.pdf

Progress and Opportunities in the Characterization of Cellulose - An Important Regulator of Cell Wall Growth and Mechanics.

The functionalization methods of materials based on bacterial cellulose (BC) mainly focus on the chemical modification or physical coating of fermentation products, which may cause several problems, such as environment pollution, low reaction efficiency and easy loss of functional moieties during application. Here, we develop a modification method utilizing the in situ microbial fermentation method combined with 6-carboxyfluorescein-modified glucose (6CF-Glc) as a substrate using Komagataeibacter sucrofermentans to produce functional BC with a nonnatural characteristic fluorescence. Our results indicate that the microbial synthesis method is more efficient, controllable and environmentally friendly than traditional modification methods. Therefore, this work confirms that BC can be functionalized by using a microbial synthesis system with functionalized glucose, which provides insights not only for the functionalization of BC but also for the in situ synthesis of other functional materials through microbial synthetic systems.

/pdf/a-natural-in-situ-fabrication-method-of-functional-bacterial-17g0f1sckt.pdf

A natural in situ fabrication method of functional bacterial cellulose using a microorganism.

Interactions of water with cellulose are of both fundamental and technological importance. Here, we characterize the properties of water associated with cellulose using deuterium labeling, neutron scattering and molecular dynamics simulation. Quasi-elastic neutron scattering provided quantitative details about the dynamical relaxation processes that occur and was supported by structural characterization using small-angle neutron scattering and X-ray diffraction. We can unambiguously detect two populations of water associated with cellulose. The first is "non-freezing bound" water that gradually becomes mobile with increasing temperature and can be related to surface water. The second population is consistent with confined water that abruptly becomes mobile at ~260 K, and can be attributed to water that accumulates in the narrow spaces between the microfibrils. Quantitative analysis of the QENS data showed that, at 250 K, the water diffusion coefficient was 0.85 ± 0.04 × 10-10 m2sec-1 and increased to 1.77 ± 0.09 × 10-10 m2sec-1 at 265 K. MD simulations are in excellent agreement with the experiments and support the interpretation that water associated with cellulose exists in two dynamical populations. Our results provide clarity to previous work investigating the states of bound water and provide a new approach for probing water interactions with lignocellulose materials.

/pdf/dynamics-of-water-bound-to-crystalline-cellulose-5fd0dvd3sz.pdf

Dynamics of water bound to crystalline cellulose

Application of X-ray and neutron small angle scattering techniques to study the hierarchical structure of plant cell walls: a review.

The interaction mechanism of two plant cell wall polysaccharides, arabinoxylan and xyloglucan, with cellulose has been investigated by means of bacterial cellulose fermentation to mimic the cell wall biosynthesis process. The combination of small angle scattering techniques with XRD and SEM has enabled the identification of different structural features comprising hierarchically-assembled bacterial cellulose, i.e. cellulose microfibrils and ribbons. The SANS results have been described by a core–shell formalism, which accounts for the presence of regions with different solvent accessibility and supports the existence of microfibril sub-structure within the ribbons. Additionally, SAXS and XRD results suggest that the microfibril packing and crystalline structure are not affected by arabinoxylan, while xyloglucan interferes with the crystallization and assembly processes, resulting in less crystalline Iβ-rich microfibrils. This specific interaction mechanism is therefore crucial for the cellulose microfibril cross-linking effect of xyloglucan in plant cell walls. It is proposed that the distinct interaction mechanisms identified have their origin in the differential structural role of arabinoxylan and xyloglucan in plant cell walls.

Evidence for differential interaction mechanism of plant cell wall matrix polysaccharides in hierarchically-structured bacterial cellulose

Isotopic enrichment has been widely used for investigating the structural and dynamic properties of biomacromolecules to provide information that cannot be carried out with molecules composed of natural abundance isotopes. A media formulation for controlled incorporation of deuterium in bacterial cellulose synthesized by Gluconacetobacter xylinus subsp. sucrofermentans is reported. The purified cellulose was characterized using Fourier Transform Infra-Red spectrophotometry and mass spectrometry which revealed that the level of deuterium incorporation in the perdeuterated cellulose was greater than 90 %. Small-angle neutron scattering analysis demonstrated that the overall structure of the cellulose was unaffected by the substitution of deuterium for hydrogen. In addition, by varying the amount of D-glycerol in the media it was possible to vary the scattering length density of the deuterated cellulose. A large disk model was used to fit the curves of bacterial cellulose grown using 0 and 100 % D-Glycerol yielding a lower bound to the disk radii, R
 min = 1,132 ± 6 and 1,154 ± 3 A and disk thickness, T = 128 ± 1 and 83 ± 1 A for the protiated and deuterated forms of the bacterial cellulose, respectively. This agrees well with the scanning electron microscopy analysis which revealed stacked sheets in the cellulose pellicles. Controlled incorporation of deuterium into cellulose will enable new types of experiments using techniques such as neutron scattering to reveal information about the structure and dynamics of cellulose and its interactions with proteins and other (bio) polymers.

Controlled incorporation of deuterium into bacterial cellulose

The Hayabusa2 spacecraft has returned samples from the Cb-type asteroid (162173) Ryugu to Earth. Previous petrological and chemical analyses support a close link between Ryugu and CI chondrites that are presumed to be chemically the most primitive meteorites with a solar-like composition. However, Ryugu samples are highly enriched in Ca compared to typical CI chondrites. To identify the cause of this discrepancy, here we report stable Ca isotopic data (expressed as δ 44/40 Ca SRM915a ) for returned Ryugu samples collected from two sites. We found that samples from both sites have similar δ 44/40 Ca SRM915a (0.58 ± 0.03 ‰ and 0.55 ± 0.08 ‰ , 2 s.d.) that fall within the range defined by CIs. This isotopic similarity suggests that the Ca budget of CIs and Ryugu samples is dominated by carbonates, and the variably higher Ca contents in Ryugu samples are due to the abundant carbonates. Precipitation of carbonates on Ryugu likely coincided with a major episode of aqueous activity dated to have occurred ∼ 5 Myr after Solar System formation. Based on the pristine Ryugu samples, the average δ 44/40 Ca SRM915a of the Solar System is defined to be 0.57 ± 0.04 ‰ (2

pdf/the-solar-system-calcium-isotopic-composition-inferred-from-2gttl1lf.pdf

The Solar System calcium isotopic composition inferred from Ryugu samples

Development of biohybrid solar energy conversion systems

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Controlled incorporation of deuterium into bacterial cellulose

The Solar System calcium isotopic composition inferred from Ryugu samples

Development of biohybrid solar energy conversion systems