Cellulose constitutes the most abundant renewable polymer resource available today. As a chemical raw material, it is generally well-known that it has been used in the form of fibers or derivatives for nearly 150 years for a wide spectrum of products and materials in daily life. What has not been known until relatively recently is that when cellulose fibers are subjected to acid hydrolysis, the fibers yield defect-free, rod-like crystalline residues. Cellulose nanocrystals (CNs) have garnered in the materials community a tremendous level of attention that does not appear to be relenting. These biopolymeric assemblies warrant such attention not only because of their unsurpassed quintessential physical and chemical properties (as will become evident in the review) but also because of their inherent renewability and sustainability in addition to their abundance. They have been the subject of a wide array of research efforts as reinforcing agents in nanocomposites due to their low cost, availability, renewability, light weight, nanoscale dimension, and unique morphology. Indeed, CNs are the fundamental constitutive polymeric motifs of macroscopic cellulosic-based fibers whose sheer volume dwarfs any known natural or synthetic biomaterial. Biopolymers such as cellulose and lignin and † North Carolina State University. ‡ Helsinki University of Technology. Dr. Youssef Habibi is a research assistant professor at the Department of Forest Biomaterials at North Carolina State University. He received his Ph.D. in 2004 in organic chemistry from Joseph Fourier University (Grenoble, France) jointly with CERMAV (Centre de Recherche sur les Macromolecules Vegetales) and Cadi Ayyad University (Marrakesh, Morocco). During his Ph.D., he worked on the structural characterization of cell wall polysaccharides and also performed surface chemical modification, mainly TEMPO-mediated oxidation, of crystalline polysaccharides, as well as their nanocrystals. Prior to joining NCSU, he worked as assistant professor at the French Engineering School of Paper, Printing and Biomaterials (PAGORA, Grenoble Institute of Technology, France) on the development of biodegradable nanocomposites based on nanocrystalline polysaccharides. He also spent two years as postdoctoral fellow at the French Institute for Agricultural Research, INRA, where he developed new nanostructured thin films based on cellulose nanowiskers. Dr. Habibi’s research interests include the sustainable production of materials from biomass, development of high performance nanocomposites from lignocellulosic materials, biomass conversion technologies, and the application of novel analytical tools in biomass research. Chem. Rev. 2010, 110, 3479–3500 3479

Cellulose nanocrystals: chemistry, self-assembly, and applications.

The crystal and molecular structure together with the hydrogen-bonding system in cellulose Iβ has been determined using synchrotron and neutron diffraction data recorded from oriented fibrous samples prepared by aligning cellulose microcrystals from tunicin. These samples diffracted both synchrotron X-rays and neutrons to better than 1 A resolution (>300 unique reflections; P21). The X-ray data were used to determine the C and O atom positions. The resulting structure consisted of two parallel chains having slightly different conformations and organized in sheets packed in a “parallel-up” fashion, with all hydroxymethyl groups adopting the tg conformation. The positions of hydrogen atoms involved in hydrogen-bonding were determined from a Fourier-difference analysis using neutron diffraction data collected from hydrogenated and deuterated samples. The hydrogen atoms involved in the intramolecular O3···O5 hydrogen bonds have well-defined positions, whereas those corresponding to O2 and O6 covered a wider v...

Crystal Structure and Hydrogen-Bonding System in Cellulose Iβ from Synchrotron X-ray and Neutron Fiber Diffraction

The purpose of this article is to describe the basic physical processes involved in the nucleation and growth of thin films of materials on solid surfaces. In this introduction the three modes of crystal growth which are thought to occur on surfaces in the absence of interdiffusion are described, and the relationships between the thermodynamics of adsorption and the kinetics of crystal growth are explored in general terms. This is followed by a brief review of atomistic nucleation theory, explaining the relations of such theories to experimental observables. In the next three sections, recent experimental examples of these three growth modes are given, which are interpreted where possible in terms of nucleation and growth theory. The last section discusses observations on the shapes of growing crystallites and the relation of such observations to nucleation and surface diffusion processes.

https://iopscience.iop.org/article/10.1088/0034-4885/47/4/002/pdf

Nucleation and growth of thin films

Review of Recent Research into Cellulosic Whiskers, Their Properties and Their Application in Nanocomposite Field

This article attempts to bring together basic and complex information which has been gathered on cellulose structure, principally that of native cellulose, over the last few decades. Even though advances have been made in the field of crystallography, powder crystallography cannot yield a definitive cellulose structure and single crystal diffraction is not possible due to the lack of suitable crystals. Knowledge obtained on the biosynthesis of native cellulose and on the polymorphy of cellulose and its derivatives help our understanding of ultrastructure. Many inconsistencies between early crystallographic studies of native cellulose have been clarified by the discovery that two polymorphs (α and β) of cellulose I exist. Models of the possible ultrastructural arrangements within native cellulose have been put forward over the decades; with advancement in technology, computer simulations of small and large systems are being created to test the viability of these ultrastructural models. It is hoped that this review will aid in the understanding of the complexity and uncertainties that still exist in this subject

Cellulose: the structure slowly unravels

Direct observation of the phase transition between the (7 × 7) and (1 × 1) structures of clean (111) silicon surfaces

Reflection electron microscopy of clean and gold deposited (111) silicon surfaces

Thin single crystal films of barium titanate prepared by chemical thinning of single crystal plates are studied by transmission electron microscopy and electron diffraction. The films as thin as 1000 A are found to have the same lattice parameters as the bulk crystals, giving no evidence for the existence of the anomalous surface layer proposed by Kanzig et al. The surface of barium titanate is found to change substantially when heated above 500°C in air and vacuo, invalidating their evidence for an unusually high Curie temperature of their anomalous surface layer. Ferroelectric 90° and 180° domains are observed by electron microscopy. The contrast of 90° domains is simple diffraction contrast. The contrast of 180° domains is due to the failure of Friedel's law, which is known to be possible to take place in electron diffraction by dynamical diffraction effect. Dislocations, tracks of fission fragments from uranium and their interaction with domains are observed.

Electron Optical Studies of Barium Titanate Single Crystal Films

UHV transmission electron microscopy on the reconstructed surface of (111) gold: I. General features

In-situ observations of growth processes of multiply twinned particles

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