Book•
X-ray diffraction procedures for polycrystalline and amorphous materials
01 Jan 1954-
About: The article was published on 1954-01-01 and is currently open access. It has received 6295 citations till now. The article focuses on the topics: Electron backscatter diffraction & Selected area diffraction.
Citations
More filters
TL;DR: In this paper, an empirical method for determining the crystallinity of native cellulose was studied with an x-ray diffractometer using the focusing and transmission techniques, and the influence of fluctuations in the primary radiation and in counting and recording processes have been determined.
Abstract: An empirical method for determining the crystallinity of native cellulose was studied with an x-ray diffractometer using the focusing and transmission techniques. The influence of fluctuations in the primary radiation and in the counting and recording processes have been determined. The intensity of the 002 interference and the amor phous scatter at 2θ = 18° was measured. The percent crystalline material in the total cellulose was expressed by an x-ray "crystallinity index." This was done for cotton cellulose decrystallized with aqueous solutions containing from 70% to nominally 100% ethylamine. The x-ray "crystallinity index" was correlated with acid hydrolysis crys tallinity, moisture regain, density, leveling-off degree of polymerization values, and infrared absorbance values for each sample. The results indicate that the crystallinity index is a time-saving empirical measure of relative crystallinity. The precision of the crystallinity index in terms of the several crystallinity criteria is given. Bas...
6,189 citations
TL;DR: In this article, the Scherrer constants of simple regular shapes have been determined for all low-angle reflections (h2 + k2 + l2 ≤ 100) for four measures of breadth.
Abstract: Existing knowledge about Scherrer constants is reviewed and a summary is given of the interpretation of the broadening arising from small crystallites. Early work involving the half-width as a measure of breadth has been completed and Scherrer constants of simple regular shapes have been determined for all low-angle reflections (h2 + k2 + l2 ≤ 100) for four measures of breadth. The systematic variation of Scherrer constant with hkl is discussed and a convenient representation in the form of contour maps is applied to simple shapes. The relation between the `apparent' crystallite size, as determined by X-ray methods, and the `true' size is considered for crystallites having the same shape. If they are of the same size, then the normal Scherrer constant applies, but if there is a distribution of sizes, a modified Scherrer constant must be used.
3,018 citations
IBM1
TL;DR: The reported procedure can be used as a general approach to various ferrite nanoparticles and nanoparticle superlattices.
Abstract: Monodisperse magnetite nanoparticles have been synthesized by high-temperature solution-phase reaction of Fe(acac)3 in phenyl ether with alcohol, oleic acid, and oleylamine. Seed-mediated growth is used to control Fe3O4 nanoparticle size, and variously sized nanoparticles from 3 to 20 nm have been produced. The as-synthesized Fe3O4 nanoparticles have inverse spinel structure, and their assemblies can be transformed into γ-Fe2O3 or α-Fe nanoparticle assemblies, depending on the annealing conditions. The reported procedure can be used as a general approach to various ferrite nanoparticles and nanoparticle superlattices.
2,605 citations
TL;DR: Four different techniques incorporating X-ray diffraction and solid-state 13C nuclear magnetic resonance (NMR) were compared using eight different cellulose preparations and it was found that the simplest method, which is also the most widely used, and which involves measurement of just two heights in the X- Ray diffractogram, produced significantly higher crystallinity values than did the other methods.
Abstract: Although measurements of crystallinity index (CI) have a long history, it has been found that CI varies significantly depending on the choice of measurement method. In this study, four different techniques incorporating X-ray diffraction and solid-state 13C nuclear magnetic resonance (NMR) were compared using eight different cellulose preparations. We found that the simplest method, which is also the most widely used, and which involves measurement of just two heights in the X-ray diffractogram, produced significantly higher crystallinity values than did the other methods. Data in the literature for the cellulose preparation used (Avicel PH-101) support this observation. We believe that the alternative X-ray diffraction (XRD) and NMR methods presented here, which consider the contributions from amorphous and crystalline cellulose to the entire XRD and NMR spectra, provide a more accurate measure of the crystallinity of cellulose. Although celluloses having a high amorphous content are usually more easily digested by enzymes, it is unclear, based on studies published in the literature, whether CI actually provides a clear indication of the digestibility of a cellulose sample. Cellulose accessibility should be affected by crystallinity, but is also likely to be affected by several other parameters, such as lignin/hemicellulose contents and distribution, porosity, and particle size. Given the methodological dependency of cellulose CI values and the complex nature of cellulase interactions with amorphous and crystalline celluloses, we caution against trying to correlate relatively small changes in CI with changes in cellulose digestibility. In addition, the prediction of cellulase performance based on low levels of cellulose conversion may not include sufficient digestion of the crystalline component to be meaningful.
2,522 citations
TL;DR: In this paper, powder diffraction patterns from cellulose Iα, Iβ, II, IIII, and IIIII were calculated based on the published atomic coordinates and unit cell dimensions contained in modified "crystal information files" that are supplied in the Supplementary Information.
Abstract: Cellulose samples are routinely analyzed by X-ray diffraction to determine their crystal type (polymorph) and crystallinity. However, the connection is seldom made between those efforts and the crystal structures of cellulose that have been proposed with synchrotron X-radiation and neutron diffraction over the past decade or so. In part, this desirable connection is thwarted by the use of different conventions for description of the unit cells of the crystal structures. In the present work, powder diffraction patterns from cellulose Iα, Iβ, II, IIII, and IIIII were calculated based on the published atomic coordinates and unit cell dimensions contained in modified “crystal information files” (.cif) that are supplied in the Supplementary Information. The calculations used peak widths at half maximum height of both 0.1 and 1.5° 2θ, providing both highly resolved indications of the contributions of each contributing reflection to the observable diffraction peaks as well as intensity profiles that more closely resemble those from practical cellulose samples. Miller indices are shown for each contributing peak that conform to the convention with c as the fiber axis, a right-handed relationship among the axes and the length of a < b. Adoption of this convention, already used for crystal structure determinations, is also urged for routine studies of polymorph and crystallinity. The calculated patterns are shown with and without preferred orientation along the fiber axis. Diffraction intensities, output by the Mercury program from the Cambridge Crystallographic Data Centre, have several uses including comparisons with experimental data. Calculated intensities from different polymorphs can be added in varying proportions using a spreadsheet program to simulate patterns such as those from partially mercerized cellulose or various composites.
1,825 citations
Cites background or methods from "X-ray diffraction procedures for po..."
...There, the undisputed convention is to have a and b equal, with c unique (Klug and Alexander 1974)....
[...]
...Their values have been divided by two in this work to represent their two-chain cell. that was grounded in statements by Klug and Alexander (1974) and used by Woodcock and Sarko (1980)....
[...]