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  • Elsevier  (64,397)
  • International Union of Crystallography (IUCr)
  • 2020-2022
  • 1990-1994  (65,952)
  • 1980-1984
  • 1930-1934
  • 1991  (65,952)
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  • 2020-2022
  • 1990-1994  (65,952)
  • 1980-1984
  • 1930-1934
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  • 1
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 18-29 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A previously described method of synthesizing a real-space distribution of scattering points which will give rise to virtually any required diffraction pattern has been investigated from the point of view of trying to establish the rôle that the phase of individual modulations plays in determining the real-space structure. For an object involving continuous random variables, the choice of phase cannot affect the diffracted intensity and phases can be chosen freely. Although such variation of phases does not affect the diffracted intensity, the real-space amplitudes are no longer normally distributed and the structures will in general contain non-zero multisite correlations. For an object involving binary variables (such as site occupancy), it is shown that the phases of individual elementary volumes of reciprocal space not only contain information about multisite correlations, but also contain the information that the object is binary. It is also shown that the information concerning multisite correlations can be, at least partially, transferred to an object giving a different diffraction pattern by using a known set of phases with a different set of amplitudes.
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  • 2
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 63-63 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Establishment of absolute structures requires measurement of Bijvoet differences with a right-handed set of axes. There can be pitfalls in the satisfaction of this requirement, and a very simple method of assessing this hand is described.
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  • 3
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 66-70 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Restraint equations suitable for incommensurate (IC) structure refinement by least squares are defined. Other quantities used in the final results analysis are reviewed. The main purpose of such a restrained refinement is to prevent high local variations of stereochemical parameters (e.g. bond lengths and/or angles), leaving the corresponding average values to be refined. The method is a natural generalization of that commonly used for commensurate structures and in some cases does not require user-supplied parameters.
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  • 4
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 78-78 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
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  • 5
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 96-101 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Accurate measurement of the deviation from coincidence orientation for grain boundaries allows the intergranular dislocation structure to be predicted. For hexagonal symmetry, the deviation may generally be split into two components: a pure rotation and a deformation. This rotation may be determined directly by measuring the displacement of rational common zone axes across the grain boundary plane, independently of any coincidence site lattice (CSL). The precision on the elements of the rotation – axis and angle – depends strongly on the sharpness of the Kikuchi lines. For deformed and annealed magnesium, a precision of 10° on the axis position and of 0.2° on the rotation angle has been obtained.
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  • 6
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 196-196 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
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  • 7
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 197-202 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A complex standardless mineral-analysis method is described which determines both the concentrations and the chemistry of minerals in a batch of m ≤ w + t suitable rock samples, where w and t are the numbers of crystalline and amorphous minerals, respectively. The method is based on data from X-ray diffractometry and the bulk chemistry of the samples. Analytical examples are given. The problem of the accuracy of the analysis is discussed.
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  • 8
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 30-37 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The design and operation of a new small-angle X-ray scattering instrument, optimized for high throughput at a synchrotron source, high angular and wavelength resolution, large sample cross-sectional area, accurate energy tuning, excellent signal-to-noise ratio and harmonic rejection are presented. The principles of design and implementation are given, as are the details of primary calibration of absolute intensity and experimental desmearing. The instrument has been tested for application to anomalous-scattering measurements near the chromium K edge. Preliminary results on samples of a heat-treated steel are presented as a demonstration of the capability of this experiment to separate the microstructure evolution as a function of temperature of a chromium-rich precipitate from the thermal behavior of other precipitates in the steel.
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  • 9
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 61-63 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A new powder diffractometer has been designed which can be used for various experimental geometries such as the long-arm Bragg–Brentano method, Guinier method and parallel-beam method. The X-ray source, goniometer and scintillation counter are placed on rails so that the source-to-monochromator, monochromator-to-sample and sample-to-counter distances can be changed arbitrarily. A FWHM of 0.07° for the Kα1 peak of the silicon 111 reflection was obtained by lengthening the counter arm in the Bragg-Brentano method. Rather high angular resolution was achieved by the Guinier and parallel-beam methods for organic samples having poor crystallinity and low absorption.
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  • 10
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 266-266 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
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  • 11
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 286-292 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The crystal structure of magnesium boron nitride in the low-pressure phase, Mg3BN3(L), has been solved ab initio from X-ray powder data. The cell is hexagonal (space group P63/mmc, Z = 2) with a = 3.54453 (4), c = 16.03536 (30) Å. Initial positional parameters for the Mg atoms were obtained from Patterson functions generated by 50 integrated intensities derived from a whole-powder pattern decomposition. The remaining atoms were located by trial-and-error model building, followed by Rietveld refinements (Rwp = 8.5%). The structure can be described as consisting of ABB′BACC′CA... layers perpendicular to the c axis with linear N=B=N molecular anions at position A, Mg2+ at positions B and C and Mg2+ with three coordinating N atoms at positions B′ and C′, although Mg3BN3(L) is not a layer compound. A very similar structure has also been obtained by applying standard direct methods to the same intensity data. A high-quality electron-density map has been calculated from the structure factor data using the maximum-entropy method.
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  • 12
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 316-323 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Measurements of lattice distortion due to a slip band were carried out and compared with the theoretically estimated values. A simple model of a single-slip system with uniformly distributed dislocations in a narrow planar slip band was adopted. It was shown that both the effect of all dislocations in the slip band and the surface relaxation must be taken into account.
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  • 13
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 365-368 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A method is presented for indexing the powder diffraction lines from incommensurate structures by a systematic search of reciprocal space, choosing a propagation vector length derived from a satellite reflection in the powder diagram. An interactive computer program gives a graphical display of the direction of the propagation vector which gives the best fit to the pattern.
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  • 14
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 190-193 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The application of single-board microcomputers as programmable interfaces simplifies the construction of complex diffractometer control units. The amount of hardware components of the control units is reduced and the structure of the circuits is easy to survey. These intelligent multipurpose single-board microcomputers unburden the personal computer and simplify the development of the diffractometer measuring program. The presented solution is based on an Atari 1040 STF. The concept, however, can be applied to any type of personal computer.
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  • 15
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 193-195 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A Fortran computer program is described which performs three-dimensional electron-density cage contouring together with atomic structure model display on a Tektronix-4100 command graphics terminal hosted to a VAX/VMS computer. The program also supports ball-and-stick visualization of the model, on-line manipulation of the display and convenient hard-copy output. Such a program is useful in a research environment where an expensive graphics workstation is not readily available and hard copies of publication quality are often desired.
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  • 16
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 212-221 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The principles of the monolithic X-ray magnifier based on two successive asymmetric non-coplanar diffractions from the same crystal are analyzed from the geometrical point of view. The conditions of the distortion-free two-dimensional pattern magnification are formulated by means of matrix formalism. The general solution of the problem of determination of the crystal surface planes satisfying the conditions of distortion-free magnification is derived in the closed form. The calculation is performed on the basis of the kinematical theory of diffraction. It is shown that the number of solutions is infinite for any given pair of diffraction vectors and magnification. General properties of the solution are illustrated by some examples. The effect of the refraction of X-rays on the pattern distortion is estimated. The results suggest that the refractive index correction has a negligible influence on the distortion of the magnified pattern. The results presented enable us to prepare monolithic X-ray magnifiers or demagnifiers that can be used in various fields of X-ray optics, especially in X-ray topography and X-ray lithography.
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  • 17
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 232-238 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Triple junctions in polycrystalline silicon for solar cell applications have been studied by TEM (transmission electron microscopy). The typical characteristic of these junctions is the existence of high-symmetry interfaces, i.e. twins of different order. Whenever the triple junction contains two such interfaces, the intersection axis is a CSL (coincidence site lattice) symmetry axis. In this case the mutual relation of the grain boundaries of the triple junctions is revealed by symmetry rules, since the boundaries are described by symmetry elements of the corresponding CSL which do not belong to the symmetry group of the parent lattice. Therefore, the different variant orientations of these CSL symmetry elements, implied by the symmetry of the lattice, are used for the study of triple junctions. A junction is geometrically characterized by the point-group-symmetry properties. The observations concern symmetrically different triple junctions of the same type of macroscopically stable grain boundaries and faceted and microfaceted interfaces. It is shown that in silicon the thermodynamically favored twins are combined by specific symmetry rules. The results are discussed in accordance with the possible growth mechanisms.
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  • 18
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 243-254 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The theoretical predictions of the triple isotopic substitution (TIS) method in small-angle neutron scattering have been confirmed experimentally. A unique advantage of the method, namely the possibility to make part of a complex particle `invisible' in normal (H2O) buffer, is demonstrated. Particle association, the addition of `small' molecules (such as glycerol) or `large' molecules (such as pyruvate kinase) in the solutions under study have been shown not to influence the difference scattering curve obtained. The possibility of extracting normalized interparticle interference functions from the TIS data is discussed. This enables the detection of the presence of aggregates (e.g. dimers) in the solution, even in cases where the molar mass of a particle and/or its concentration are unknown. A simple internal test is suggested which checks whether or not sufficient conditions for the applicability of the method are fulfilled.
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  • 19
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 264-264 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
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  • 20
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 267-277 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The efficiency of data collection using the Laue technique varies with the wavelength range, the crystal symmetry, the orientation of the crystal in the X-ray beam, the crystal-to-film distance and the acceptance angle of the detector. By optimizing these parameters and by taking advantage of the diffraction symmetry represented by the Laue class, it is often possible to collect a nearly complete data set in one or two exposures. This paper discusses general strategies for data collection and presents results from a computer survey to find optimal crystal orientations for the eleven Laue classes.
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  • 21
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 293-297 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A method for empirical determination of TDS (thermal diffuse scattering) corrections in X-ray structure analysis is developed. Thermal diffuse scattering is introduced into the model suggested earlier [Chulichkov et al. (1987). Sov. Phys. Crystallogr. 32, 649–653; Laktionov, Chulichkov, Chulichkova, Fetisov, Pyt'ev & Aslanov (1989). J. Appl. Cryst. 22, 315–320] for measuring the Bragg reflection intensity profile with a four-circle diffractometer. The improved model in combination with the mathematical reduction method enables the extraction of TDS and background intensity values from the experimental intensity profile. Thus the problem of TDS correction in crystal structure refinement is solved without knowledge of the sample's elasticity constants. The comparison of TDS corrections obtained by this method with those calculated from elasticity constants for hexamethylenetetramine, C6H2N4, and sulfur, S8, crystals shows good agreement.
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  • 22
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 324-330 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The lattice distortion due to the head of the slip band at the grain boundary is measured by double-crystal topography. The head of the slip band is approximated by a macrodislocation situated at the grain boundary. To interpret the topographs, the relaxation due to the free surface is included. The Burgers vectors of macrodislocations, i.e. the number of accumulated dislocations, are found.
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  • 23
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 369-402 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
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  • 24
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 406-408 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
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  • 25
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 624-634 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Small-angle neutron scattering (SANS) provides a powerful tool in the non-destructive characterization of statistically representative microstructures in technologically important disordered materials. While qualitative microstructural models must be provided by other methods such as transmission electron microscopy (TEM), SANS quantifies the microstructural parameters and can characterize scale-invariant (fractal) disordered materials such as cements, clays and porous rocks. H2O/D2O contrast-variation methods have proved particularly useful for investigating the accessibility of different parts of the pore structure and in differentiating between pore-volume access (measured by other methods) and pore-surface accessibility (likely to control sorption and leaching processes). This paper describes SANS studies of disordered porous materials, particularly the hydration of cement and the real-time permeation of water in clay minerals. Other microstructural effects are also considered.
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  • 26
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    Applied crystallography online 24 (1991), S. 638-644 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The microstructure of a coating deposited onto a tungsten carbide layer by cathodic sputtering assisted by chemical vapour deposition (CVD) has been analysed by small-angle scattering of X-rays (SAXS) with a conventional laboratory set-up specially adapted for grazing incidence. Anomalous-scattering measurements have also been performed at LURE, the French synchrotron-radiation facility at Orsay with the aim of characterizing the structure of phases present in the coating. SAXS results reveal the existence of very small precipitates; the size of these precipitates determined from the use of the Guinier approximation is about 16 Å, the correlation length deduced from the position of the peak in the small-angle scattering pattern is about 36 Å. The value of the experimental integrated intensity and the variation of the observed intensities with photon energy lead to the conclusion that these nanocrystals are highly enriched in tungsten and embedded in a carbon-based matrix having a weak electronic density. Electron diffraction results support the assumption of the presence of β-WC1 − x, an unstable high-temperature phase. Furthermore, the low electronic density of the matrix is in agreement with face-centred-cubic carbon recently proposed in the literature.
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  • 27
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    Applied crystallography online 24 (1991), S. 679-684 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Lamellar microdomains formed in the solvent-cast films of a poly[styrene-block-(ethylene-alt-propylene)] (SEP) diblock polymer were studied by small-angle X-ray scattering (SAXS). The SAXS profiles, displaying a series of peculiar scattering maxima which cannot be ascribed to the higher-order diffraction maxima from a regular lamellar spacing, were analyzed based on a model of the one-dimensional paracrystal with a preferential orientation. The results suggest that these maxima are due to higher-order scattering maxima from single lamellar microdomains. The maxima suggest that the relative standard deviation for the distribution of the polystyrene lamellar size is much smaller than that of the lamellar spacing, giving rise to a situation in which the oscillation of the particle factor with scattering vector h persists up to high h values while that of the lattice factor damps to unity at low h values. The SAXS result was interpreted as being due to a bending distortion of the polystyrene lamella with a smaller thickness and a narrower thickness distribution than those of the poly(ethylene-alt-propylene) lamella. A study by transmission electron microscopy tends to support this result.
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  • 28
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    Applied crystallography online 24 (1991), S. 436-443 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A survey is given of recent work on the use of small-angle neutron scattering to examine colloidal dispersions. Particular attention is given to the determination of particle size and polydispersity, the determination of particle morphology and the behaviour of concentrated colloidal dispersions, both at rest and under the influence of an applied shear field.
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  • 29
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    Applied crystallography online 24 (1991), S. 910-912 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The results of intensity profile analysis of Bragg reflections are used for the calculation of the reflectivity Q(Δθij, σij) = W(Δθij, σij)(|F|2Lp)ij in the energy transfer equation for multiwave X-ray diffraction in crystals. The diffraction profiles in the profile analysis are fitted by different analytical functions and the fitting results are used for modelling the multiwave diffraction. The results of modelling multiwave diffraction in Si and V3Si crystals with different grades of perfection demonstrate that the method suggested here is sensitive to the content of defects in crystals and can be used not only for simultaneous reflection correction in X-ray structure analysis but also for estimation of single-crystal perfection.
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    Applied crystallography online 24 (1991), S. 928-930 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: While the deviations from linearity of ε−sin2ψ curves in the case of two welded hot-rolled C40 steel bars were being studied, this paper was prompted by the observation that, at ψ = 0°, the diffraction angle 2θ depends on φ, the inclination angle of the diffraction plane with respect to an arbitrarily chosen reference plane attached to the specimen. This result is unexpected and cannot be explained by bulk structural or microstructural factors. A surface effect is offered as a possible explanation.
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    Applied crystallography online 24 (1991), S. 946-950 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The MOLSCRIPT program produces plots of protein structures using several different kinds of representations. Schematic drawings, simple wire models, ball-and-stick models, CPK models and text labels can be mixed freely. The schematic drawings are shaded to improve the illusion of three dimensionality. A number of parameters affecting various aspects of the objects drawn can be changed by the user. The output from the program is in PostScript format.
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  • 32
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    Applied crystallography online 24 (1991), S. 961-962 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
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    Notes: Modifications to the high-stability mounting device for the closed-cycle helium cryostat as developed by Henriksen, Larsen & Rasmussen [J. Appl. Cryst. (1986). 19, 390–394] are described. They allow use of the cryostat on the smaller Huber 511.1 diffractometer circle with a smaller source-to-sample distance and reduced blind and collision zones.
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 972-973 
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    Applied crystallography online 24 (1991), S. 6-13 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A double-channel X-ray standing-wave technique has been suggested. It reduces to simultaneous recording of photoelectrons and fluorescence radiation coming from a crystal under the conditions of X-ray diffraction. The use of a coincidence circuit allows one to obtain fluorescence radiation from small depths of electron escape and to eliminate distortions of fluorescence angular dependence owing to X-ray extinction. The double-channel X-ray standing-wave method was used to record the fluorescence yield curves free of extinction distortions from gadolinium and gallium atoms occupying different lattice positions in gallium-gadolinium garnet. The positions of impurity terbium atoms in yttrium–aluminium garnet have been determined. The influence of indirect excitation of a secondary radiation on the angular yield curves obtained has also been considered.
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 38-47 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The breakdown of Friedel's law has been observed in backscatter Kikuchi diffraction patterns (BKDP) obtained in the scanning electron microscope (SEM) from a series of zincblende structures including GaAs, InP, GaSb, CdHgTe and the minerals sphalerite (ZnS), chalcopyrite (CuFeS2) and tetrahedrite (Cu12Sb4S13). Differences in intensities were observed between the reflections 51{\bar 1} and 5{\bar 1}{\bar 1} in InP, GaSb, CdHgTe and sphalerite, thus allowing the non-centrosymmetric point group {\bar 4}3m to be determined. In GaAs, differences in intensities were noted between {\bar 5}11 and {\bar 4}{\bar 1}. In chalcopyrite and tetrahedrite, non-equivalent intensities were observed between {\bar 2}15 and 2{\bar 1}{\bar 5} and between 3{\bar 1}{\bar 2} and 31{\bar 2}, respectively. In addition, BKDPs obtained from chalcopyrite revealed a small displacement at the point where the pair of equivalent reflections {\bar 4}06 and 460 intersect within the Kikuchi band 02{\bar 2}. The presence of this displacement together with observation of the breakdown of Friedel's law confirmed the tetragonal point group {\bar 4}2m for chalcopyrite. Although the point groups of GaAs, chalcopyrite and tetrahedrite were derived successfully using BKDPs, determination of their space groups proved unsuccessful. The superstructure reflections were invisible because the structure factors are very small. The behaviour of the invisible 200 reflection in GaAs is investigated using many-beam dynamical intensity profiles calculated across the h00 systematic row of reflections. Dynamical intensity profiles calculated across the h00 systematic rows of reflections for Ge, InP and sphalerite are also discussed.
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  • 36
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    Applied crystallography online 24 (1991), S. 70-72 
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    Notes: A method of determining possible reflection conditions (systematic absences) from a list of indexed powder diffraction peaks and assigning a significance rank to them is suggested. The reflection conditions for the crystal system may be used to suggest possible space groups. A program, POWABS, based on this method is described. Two applications of the program are given.
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    Applied crystallography online 24 (1991), S. 77-78 
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  • 38
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    Applied crystallography online 24 (1991), S. 91-95 
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    Notes: A method for the determination of a symmetry-constrained least-squares orientation matrix and unit cell is described. The method retains the simplicity of early iterative techniques since it avoids the use of cumbersome constraining equations resulting from the application of Lagrange multipliers, yet it does not require the evaluation of numerical derivatives. The straightforward nature of simplex optimization makes the algorithm extremely easy to program in Fortran, Pascal and Basic.
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  • 39
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    Applied crystallography online 24 (1991), S. 108-110 
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    Notes: Compounds of niobium and aluminium and of niobium, aluminium and germanium which crystallize in the A15 structure were prepared by sintering and by floating-zone methods. Single crystals of up to 1 × 1 × 1 mm were obtained for the composition Nb0.78Al0.17Ge0.05. Transition temperatures to superconductivity ranged from midpoint values of 18.6 to 19.4 K over intervals of 3 K. Single-crystal X-ray diffraction measurements were made at 293 and at 11–12 K. Powder diffractometer data were obtained at 293 K. The structure was refined with both powder data (Rietveld technique) and single-crystal data. Photographic powder patterns were obtained from room temperature down to 11.7 K. No phase transition was observed. No evidence was found for deviations from the A15 structure.
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    Applied crystallography online 24 (1991), S. 129-134 
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    Notes: The growth of gypsum, CaSO4.2H2O, under pressure was studied starting from a dense suspension of CaSO4.0.67H2O in water. Pressures of 150, 300 or 600 MPa were applied at different times from the beginning of hydration of the initial material and were maintained constant for 15 min. The crystallized material was examined by DTA, X-ray and SEM techniques. Whether the hemihydrate or gypsum crystallizes depends on the time of initial hydration, i.e. whether it is short (less than about 15 min) or longer. When the time of hydration is less than 5 min and the pressure is low, only partially dissolved crystals of the hemihydrate are found in the sample. When the pressure increases, the hemihydrate partially recrystallizes as well formed elongated crystals. When both the time of hydration and pressure increase, more and more gypsum crystals form with typical habit. At constant hydration time, an increase in pressure favours the occurrence of gypsum. When the hydration time is about 30 min, only gypsum crystals occur. When the pressure is applied 30 min after the time of hydration, most of the gypsum crystals are broken in the solid texture.
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    Applied crystallography online 24 (1991), S. 149-155 
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    Notes: High-resolution powder diffraction coupled with the total-pattern-fitting technique revealed unusual and hitherto unreported diffraction effects for samples of copper(II) oxide. Data were obtained with a conventional diffractometer and strictly monochromatic Cu Kα1 radiation and also with the Daresbury Laboratory synchrotron source (9.1 HRPD). It was found that most lines are skewed, by varying amounts, towards higher or lower angles and there is a small amount of line broadening, which is mainly order dependent. It is shown that the line profile asymmetry varies systematically throughout reciprocal space and that the magnitude of the effect is sample dependent. No significant peak displacements were detected, but the skewing of lines is consistent with a distribution in the dimensions of the unit cell and hence Cu—O bond lengths.
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    Applied crystallography online 24 (1991), S. 146-148 
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    Notes: It is shown that Laue diffraction patterns may be obtained from a protein crystal using the continuous radiation emitted by a tungsten sealed-tube X-ray source and that precise structure amplitudes may be extracted from these patterns.
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  • 43
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    Applied crystallography online 24 (1991), S. 178-183 
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    Notes: Multiple-crystal diffraction profiles and multiple-crystal topography have been combined to characterize semiconductor materials. X-ray topographs have been measured on the same region of the sample as the diffraction profiles and diffraction space maps, by insetting a film cassette in the diffracted beam path of a high-resolution diffractometer. This has proved to be a very powerful combination for providing a deeper understanding of the structural features that give rise to the high-resolution diffraction profiles. The data collection mode is discussed and the problems associated with interpreting `rocking curves' of imperfect materials. The misorientation and nature of the mosaic blocks in semi-insulating GaAs have been revealed by this method.
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    Applied crystallography online 24 (1991), S. 187-189 
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    Notes: A function for finding the voids in a crystal structure by means of a single Fourier synthesis is described. The function handles the atoms as spheres with known radius and supplies, for each grid point of the Fourier map, the volumetric fraction of the search atom centered at this point that interpenetrates the neighbouring atoms. In this way, the time-consuming calculation of distances is avoided. Its application to a solid-state ionic conductor is shown.
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    Applied crystallography online 24 (1991), S. 196-196 
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    Applied crystallography online 24 (1991), S. 239-242 
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    Notes: If thermal-expansion-tensor components αij are determined from temperature-induced changes in d values, most authors first calculate the unit-cell parameters at different temperatures. From these, the αij are computed. It is shown that this procedure involves a reduced precision if compared with the direct least-squares determination of αij from changes in the d values.
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    Applied crystallography online 24 (1991), S. 261-262 
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    Notes: A practical equation is presented to determine the deadtime τd in conventional X-ray counting systems when the amount of deadtime is greater than that which can be accounted for by non-extended deadtime theory. The use of this equation to determine the deadtime increases the practical range over which conventional X-ray detection systems can be used.
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    Applied crystallography online 24 (1991), S. 263-263 
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    Applied crystallography online 24 (1991), S. 265-266 
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    Applied crystallography online 24 (1991), S. 304-311 
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    Notes: The contrast of dislocation images in X-ray section topographs of curved crystals has been investigated both experimentally and by computer simulation. Good agreement is found between experiment and simulation in both symmetric and asymmetric Laue geometries. Very little change is observed in the symmetric Laue images for radii of curvature as small as 18 m. In the asymmetric geometry, the background intensity rises and the Kato fringe visibility decreases as the curvature increases. The dynamical image becomes more localized and dominates the image as the direct image visibility falls. Our results explain the reversal of dislocation contrast in Lang projection topographs of curved crystals taken in asymmetric geometry.
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    Applied crystallography online 24 (1991), S. 331-339 
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    Notes: The orientation contrast at the head of slip bands at a grain boundary was studied by a modified Schulz technique. The images on the topographs were simulated using kinematical intensity calculations. The stress field of the macrodislocation, which represents the head of the slip band, includes the surface stress relaxation. The Burgers vectors of the macrodislocations were determined.
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    Applied crystallography online 24 (1991), S. 355-364 
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    Notes: A crystallographic orientation analysis to study heterogeneous polycrystalline samples is reported. A specific arrangement was realised to explore the total surface of large wafers or ribbons without destructive sampling. The surface texture is determined by X-ray diffraction using reflection geometry. Approximate size and orientation of crystallites at the sample surface are evaluated from a method taking iterative comparisons of intensities as a basis. For each explored (hkl) pole, two intensities are measured by reflection on the surface element studied: the first when the reflective surface is fixed at the (hkl) Bragg angle; the second when the surface is rocked around this position. The same measurements, obtained from an even surface of (hkl) monocrystals, provide calibration curves. Generally the exploration of five or six different (hkl) poles is enough to obtain a valid description of polycrystalline silicon materials elaborated for photovoltaic conversion.
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    Applied crystallography online 24 (1991), S. 403-404 
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    Notes: The spatial intensity profile of an X-ray beam reflected by a crystal with microdefects in the Bragg case is considered. A practically pure diffuse component was measured at the tail of the intensity distribution. From these data, static Debye–Waller factors of nearly perfect silicon crystals were obtained.
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    Applied crystallography online 24 (1991), S. 413-413 
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    Applied crystallography online 24 (1991), S. 444-456 
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    Notes: The use of X-ray and neutron small-angle scattering in the study of microstructural changes in inorganic materials is reviewed, with emphasis on recent developments. In the kinetics of diffusion-controlled phase separation, reliable data on the evolution of size and shape of the decomposition products may be obtained especially from in situ ageing experiments. Magnetic neutron scattering is discussed for inhomogeneous ferromagnets. While for the structural characterization of binary systems single-wavelength experiments are sufficient, variable X-ray wavelengths now available at synchrotron-radiation facilities open possibilities for the study of partial structure functions in systems containing several components. The combined use of small-angle scattering and complementary techniques is of particular value in more complex cases. These points are illustrated by a survey of recent results on phase separation and precipitates in binary and ternary crystalline alloys and on radiation-induced microstructural changes in metallic and semiconducting materials.
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    Applied crystallography online 24 (1991), S. 457-466 
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    Notes: Structure self-assembling in the spinodal decomposition (SD) of polymer blends in its late stage has been explored for a near-critical mixture of polybutadiene and polyisoprene by a time-resolved light scattering technique, with a particular emphasis on the time evolution of the interface structure. By analysis of a scaled structure factor F(x, t) ≡ I(q, t)qm(t)3 over wide ranges of a reduced scattering vector x ≡ q/qm(t) and time, it was found relevant to divide the late stage of SD into two stages, I and II. Here, I(q, t) denotes the scattered intensity as a function of the scattering vector q and time t. In the intermediate stage preceding the late one, F(x, t) became sharper with its peak at x = 1 increasing with t. However, as time elapsed, F(x, t) turned out to be universal for t, first in the range of x smaller than about 2 and then over the entire range of x accessible by the present experiment. The time interval in which the former occurred is defined as late stage I and the one in which the latter was realised is called late stage II. In late stage I, the average thickness of phase-phase interfaces decreases towards an equilibrium value and the time evolution of the interfacial area density Σ(t) does not scale with qm(t), i.e. the exponents γ and α in the power laws Σ(t) ̃t−γand qm(t) ̃t−α do not coincide (actually, α 〈 γ). Late stage II corresponds to the process in which these exponents become equal and the interface thickness reaches equilibrium. Such conditions probably ensure the establishment of a complete dynamical scaling law in the SD process.
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    Applied crystallography online 24 (1991), S. 526-530 
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    Notes: The wavelet transform has recently received much attention in the fractals world due to its ability to characterize the scaling properties of multifractal aggregates. This paper is devoted to the optical version of the wavelet transform, with a special emphasis on instrumental aspects. The optical wavelet transform amounts to a series of distinct bandpass filterings of the optical Fourier spectrum of the system under study. One wavelet component is given by one filtered image of the system. The way in which the intensity at any point depends on the filter size directly gives the local scaling behavior around this point.
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    Applied crystallography online 24 (1991), S. 555-561 
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    Notes: A triple-axis diffractometer has been constructed and optimized in our laboratory. It is used on an X-ray point source, using the principle which was pioneered by Bonse and Hart 25 years ago. A triple-reflection channel-cut Ge crystal is used as monochromator and the same as analyser. The width of the direct beam is about FWHM = 17′′ for Cu Kα radiation. Owing to the low background, the stability of the mechanics and the two triple Ge reflections, a signal-to-noise ratio of 107 has been achieved between the direct beam and the parasitic scattering without sample. These characteristics allow routine measurement of scattering to be performed for Bragg spacings up to 6000 Å for typical colloidal samples in semilinear collimation.
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    Applied crystallography online 24 (1991), S. 568-570 
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    Notes: A brief description and characterization is given of the three small-angle neutron scattering instruments (SANS) in the new guide laboratory at the Jülich FRJ-2 reactor, namely two 40 m slit-collimation instruments and a very high-resolution double-crystal diffractometer. The combination of the two instruments allows one to cover a range of scattering vectors Q of nearly four orders of magnitude.
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    Applied crystallography online 24 (1991), S. 593-597 
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    Notes: In the last decades, the kinetics of phase separation following a quench into the miscibility gap have been studied in a variety of systems by small-angle scattering techniques. A scaling behavior in the late stages of coarsening, first observed in computer simulations, was found to be a `universal' feature of the small-angle scattering intensity S(k,t) with S(k,t) = S[km(t),t]F[k/km(t)], where km(t) is the value of the modulus k of the scattering vector at which S(k,t) has its maximum. Furthermore, it was observed recently that, for many systems ranging from liquid and polymer mixtures to solid alloys and computer simulation models, the scaling function F(x) does not change appreciably from one system to another when the volume fraction is kept constant. This paper first reviews work carried out jointly with J. L. Lebowitz and O. Penrose, discussing various features of the scaling function F leading to a simple analytical expression suitable to fit experimental data. New small-angle X-ray scattering results on the shape of the scaling function for dilute Al–Ag and Cu–Fe systems are then presented and compared with the predictions of the model.
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    Applied crystallography online 24 (1991), S. 635-637 
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    Notes: A series of active C atoms was prepared by combination of activation (by steam, at 1173 K) and by heat treatment (at 1523 K, 2 h under nitrogen) and the structures of the samples were investigated by gas adsorption (nitrogen adsorption isotherms) and by X-ray scattering. An agreement is observed between the average chord length of segments in the solid phase measured by SAXS and the average micropore size determined by gas adsorption, suggesting that the diameters of micropores formed during the activation and the heat treatment have nearly the same size as the crystallites.
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    Applied crystallography online 24 (1991), S. 659-664 
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    Notes: Surprisingly, molecular weight can be determined from small-angle scattering data without using absolute intensities and the contrast factor. The formula underlying this novel procedure is illustrated by model calculations. Several examples of the successful use of the procedure applied to polymer solutions together with those where the method has failed are given.
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    Applied crystallography online 24 (1991), S. 692-701 
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    Notes: Five interpenetrating polymer network (IPN) epoxy-acrylate samples of the same composition synthesized with variable conditions – temperature and initiator rate – were studied by small-angle X-ray scattering (SAXS). The scattering curves, at first sight showing little detail, were meticulously analysed. The entire scattering curve of an IPN compound was analysed using new methods for background subtraction and desmearing. The treatment suggests a fractal behaviour of the internal surface, associated with this two-phase system, on a scale between 100 and 10 nm and, in the tail end of the SAXS curves, reveals maxima corresponding to those of two regular spheres with radii of the order of 7 and 14 nm. Analysis of the beginning of the curves yields one or two correlation lengths according to the conditions of the synthesis, close to 100 and 20 nm. These results are consistent with the general model of IPN structures as revealed by other physico-chemical techniques.
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    Applied crystallography online 24 (1991), S. 709-711 
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    Notes: Aramid fibres show elongated microvoids parallel to the direction of the fibre axis, resulting in an equatorial streak in the small-angle X-ray scattering (SAXS) pattern. The scattered intensity in the equatorial direction has been measured for three samples of the same fibre: an untreated yarn specimen, yarn in which Ag2S was precipitated and a single filament of the latter. In the case of the untreated yarn, the interpretation of the SAXS pattern is hindered by the presence of residual water in the voids, resulting in a three-phase system. The SAXS pattern of the yarn with precipitated Ag2S follows the theoretical pattern (adapted for the two-dimensional case) for a system with random pores, but the interface between aramid and Ag2S shows fractal properties. The single filament with Ag2S shows a SAXS pattern analogous to that of the fibre with Ag2S, indicating that multiple scattering and interfilament scattering is negligible. It was also found that the Ag2S precipitates in the fibre with preferred orientation.
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    Applied crystallography online 24 (1991), S. 732-739 
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    Notes: Calcium carbonate dispersions stabilized by an adsorbed surfactant layer are used to regulate the acidity of lubricating oils for internal combustion engines. Three typical commercial samples have been examined using a combination of X-ray and neutron scattering techniques. The solid active material was extracted from the samples and redispersed in heptane and mixtures of toluene and toluene-d8 and n-octane and n-octane-d18. The results were in broad agreement with the core/shell model proposed by Ottewill [Markovic, Ottewill, Cebula, Field & Marsh (1984). Colloid Polym. Sci. 262, 648–656]. The core radius ( ̃12–28 Å) was obtained from SAXS data. The polydispersity was about 25% on all samples and the distribution skewed to larger sizes. The hydrogenated-solvent SANS data were too weak to be used to determine the core size. The total particle radius ( ̃20–50 Å) and hence the shell thickness were obtained by model fitting to the deuterated-solvent and 65% deuterated-solvent SANS data with the core radius from the X-ray data. In determining the best fit, the core density, amount of solvent in the shell and polydispersity were also adjusted to give fits with a shell-to-core-volume ratio and a volume fraction that agreed with the expected values. The SANS data were weaker than expected assuming a simple monodisperse core/shell model with a calcite core. This is consistent with the observed polydispersity and in addition implies diffuse boundaries. Although WAXS (wide-angle X-ray scattering) confirmed that the cores were non-crystalline the best model fits were obtained with a core scattering density not much less than that calculated for calcite. The absolute intensities suggested that some solvent was incorporated into the shells of all the samples and one sample showed a preference for uptake of octane as compared to toluene.
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    Applied crystallography online 24 (1991), S. 759-764 
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    Notes: The influence of pH, cations, F− and temperature on the aggregation, gelation and ageing of aqueous silica gels has been investigated using small-angle X-ray scattering (SAXS). At both low and intermediate pH (pH = 4 and 6–8, respectively), fractal aggregates are formed during gelation from silicic monomers or small oligomers. The fractal dimensionality is 2.20 (5), to be expected for reaction-limited cluster–cluster aggregates. During ageing silicic ions dissolve from the more soluble peripheral primary particles and condense in the crevices of the core of the aggregates. This process results in an increase in the size of the scattering primary particles and in a decrease in the fractal dimensionality of the silica aggregates from D = 2.25 to D = 2.0 or D = 1.85. The ageing processes are strongly enhanced by a slight increase in the pH of the solution, addition of fluorine anions and a rise in temperature. The aged silica gel is constructed of an ensemble of densified aggregates of which the density variation within the aggregates is larger than that of the freshly prepared aggregates. The primary particles of which the aggregates are built grow during ageing from molecular size to dense particles in the nanometer range, the ultimate radius depending on the type and duration of the ageing process.
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  • 67
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    Applied crystallography online 24 (1991), S. 815-821 
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    Topics: Geosciences , Physics
    Notes: Structural information of clathrin-coated vesicles has been achieved by small-angle X-ray, neutron and dynamic light scattering studies. A characteristic peak in the X-ray and neutron scattering profile (in D2O) from intact coated vesicles is consistent with the polygonic structure of the clathrin coat. Neutron as well as dynamic light scattering gives a coated vesicle size close to 1000 Å. Dynamic light scattering detects a distribution of sizes for the coated vesicles demonstrating polydispersity of the samples. Quick freezing and slow thawing cause breakdown of the polygonic coat and production of large aggregates, as observed by dynamic light scattering and the reduction of the peak in the X-ray scattering profile as well as an increase in the scattering intensity at the lowest angles in the neutron scattering profile.
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  • 68
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    Applied crystallography online 24 (1991), S. 836-842 
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    Topics: Geosciences , Physics
    Notes: A new experimental technique to investigate the structural rearrangements associated with thermal phase transitions of phospholipids is outlined. The method utilizes the changes in small-angle X-ray powder diffraction patterns, monitored with a time resolution of down to 1 ms, following fast temperature jumps of about 10 K height in 1–2 ms. This heating rate, effected by an erbium infrared laser pulse, provides a synchronous disequilibration of the lipid samples and the ensuing structural relaxation processes are observed by using the high-flux X-ray beam from a synchrotron source in combination with a rapid position-sensitive-detection and data-acquisition system. For the two symmetry heterologous phase transitions, the lamellar (Lβ')-to-monoclinic (Pβ') `pretransition' of synthetic phosphatidylcholines and the lamellar (Lα)-to-inverted hexagonal (HII) transition of phosphatidylethanolamines, this method provides the first evidence for the existence of transient intermediate ordered structures. In the pretransition, the first step is the rapid (〈 2 ms) formation of a second lamellar lattice, with a decreased repeat distance, which coexists for up to about 100 ms with the original Lβ' lattice. In a second, slower process, these two lattices merge and transform to the Pβ' structure within several seconds. In the Lα–HII transition, the first rapid step (τ ̃5 ms) consists of a uniform shrinkage of the lamellar lattice; this is followed after about 20 ms by the first appearance of a distorted hexagonal lattice and a slow transformation into the final HII lattice. Comparison of these results with X-ray diffraction data obtained under near-equilibrium conditions, where these intermediates cannot be detected, shows that the systems respond to the high thermodynamic driving force which exists under non-linear non-equilibrium conditions by formation of correlated intermediate structures which provide efficient pathways for relaxation.
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  • 69
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    Applied crystallography online 24 (1991), S. 874-877 
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    Topics: Geosciences , Physics
    Notes: Model calculations have been performed on displacement disorder effects in equatorial X-ray diffraction patterns of skeletal muscle. Powder patterns are calculated for single-site standard deviations (σ) up to 0.3 × lattice constant. The area ratio of the 11 and 10 peaks in the powder patterns is discussed. Line broadening in these patterns as a function of correlation length shows paracrystal-like behaviour for sufficiently large σ. Asymmetric line shapes and peak shifts in the direction of the central beam occur for values of σ larger than 0.2 × lattice constant and small correlation lengths.
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  • 70
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    Applied crystallography online 24 (1991), S. 893-909 
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    Notes: A method for calculating the flux at the sample position and the resolution function based on the general description of synchrotron X-ray beamlines in position–angle–wavelength space has been developed. A mathematical formulation is presented, in which source, transmission function for the slits and acceptance windows of the monochromator crystals are approximated by Gaussian functions. These approximations allow all of the algebra in connection with combining the different contributions to be done analytically. When the beam passes the various components of the beamline, such as flight paths, monochromators and mirrors, it results in coordinate transformations in parameter space. By inserting the transformations in the intensity distribution of the source, transmission functions of the slits and acceptance windows of the monochromators, these are transformed to the position of the sample. Their product gives the intensity distribution at this position and from this the resolution function in reciprocal space is calculated. The resolution of the detector is easily included by a convolution. The transmissions of the slits and the acceptance windows of the monochromator crystals have been normalized to give the same integrated transmission and reflectivities as the functions they approximate. Therefore the flux at the sample position can be calculated by multiplication of the brilliance of the source and the result obtained from an integration of the distribution over the two position parameters, the two angle parameters and the wavelength. The theory has been applied to an example and gives reasonable results for sample intensity and resolution function.
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  • 71
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    Applied crystallography online 24 (1991), S. 931-935 
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    Notes: Xenon gas can be used as a heavy atom for determining phases in a protein. We demonstrate that an interpretable electron density map can be obtained for sperm whale metmyoglobin from a single xenon derivative using iterative single isomorphous replacement with the anomalous scattering method.
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  • 72
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    Applied crystallography online 24 (1991), S. 950-955 
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    Notes: A program has been developed to help design a geometric representation of the atomic structure of interfaces between two crystalline structures. The C-language program run on a graphics-oriented computer has proved to be a simple precise tool to use. It provides a clear picture of the atomic positions at the interface and, simultaneously, a stereographic projection and diffraction pattern for each crystal and bicrystal. Examples of multiple twinning in the sphalerite structure and of various metal–ceramic interfaces are presented.
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  • 73
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    Applied crystallography online 24 (1991), S. 955-958 
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    Notes: With DEMUX and MUX, a pair of subroutines is provided that allows for the straightforward removal of multiple scattering from small-angle scattering data (DEMUX) or the simulation of the effect of multiple scattering (MUX). The data may be given in an arbitrary scaling. The parameter that must be given to fix the amount of multiple scattering is the transmission reduction of the sample due to small-angle scattering. The algorithm used is based on the method of Schelten & Schmatz [J. Appl. Cryst. (1980), 13, 385–390]. It is valid for a plane flat sample exhibiting scattering of significant intensity at small angles only.
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  • 74
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    Applied crystallography online 24 (1991), S. 968-971 
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    Notes: In the KTiOPO4 (KTP) structure, it is shown that there are hole sites related by pseudosymmetry to the inequivalent potassium sites K(1) and K(2). The formation of twin domains is through a twofold rotation with the principal feature of the twinning being the displacements of the K atoms onto their respective hole sites thus reversing the polarity of the crystal. Ionic diffusion paths for K+ along [001] involving both potassium and hole sites are described and are used to explain the enhanced ionic conductivity seen along this direction in KTP crystals. With this structural model, an explanation is also given for the reported phenomenon of domain inversion which is known to occur in the modified layer when Rb+ and Ba2+ are substituted into one of the {001} surfaces of KTP. It is shown from structural principles that ion exchange should be more efficient at the −Z end of the crystal, as is indeed observed in practice.
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  • 75
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    Applied crystallography online 24 (1991), S. 974-974 
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  • 76
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    Applied crystallography online 24 (1991), S. 982-986 
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    Notes: A new method for complete determination of polarization state in the hard X-ray region is described. The system consists of a perfect-crystal phase retarder and a linear polarization analyzer. This method gives not only the amplitude ratio of mutually perpendicular electric vector components and the phase shift between them but also the proportion of unpolarized radiation.
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  • 77
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    Applied crystallography online 24 (1991), S. 994-998 
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    Notes: The problem of the optimization of small-angle neutron scattering instruments installed at steady neutron sources is discussed. The optimum solution is shown to be that in which full use is made of either the available luminous area of the source or the available hall space and not necessarily that corresponding to the equal-flight-paths design. Design criteria and their implementation are discussed taking into account space constraints on the instrument's layout. It is shown that the performance of currently operating SANS facilities can be substantially improved by following the optimization procedure proposed by the authors.
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  • 78
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    Applied crystallography online 24 (1991), S. 987-993 
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    Notes: The dichotomy method for indexing powder diffraction patterns for low-symmetry lattices is studied in terms of an optimization of bound relations used in the comparison of observed data with the calculated patterns generated at each level of the analysis. A rigorous mathematical treatment is presented for monoclinic and triclinic cases. A new program, DICVOL91, has been written, working from the cubic end of the symmetry sequence to triclinic lattices. The search of unit cells is exhaustive within input parameter limits, although a few restrictions for the hkl indices of the first two diffraction lines have been introduced in the study of triclinic symmetry. The efficiency of the method has been checked by means of a large number of accurate powder data, with a very high success rate. Calculation times appeared to be quite reasonable for the majority of examples, down to monoclinic symmetry, but were less predictable for triclinic cases. Applications to all symmetries, including cases with a dominant zone, are discussed.
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  • 79
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    Applied crystallography online 24 (1991), S. 1009-1014 
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    Notes: Real-time neutron powder diffraction and small-angle scattering techniques have been developed on the TOF diffractometer DN-2 at the IBR-2 pulsed reactor at JINR (Dubna) with a total flux on the sample of 107 neutrons cm−2 s−1 and a resolution of about 1%. A special arrangement of the detector system ensures a high counting rate of diffracted neutrons. Depending upon sample type and experimental conditions, the measuring time ts of one neutron pattern varies from a few minutes to several seconds. The performance of the diffractometer is discussed and typical data are shown to demonstrate current achievements using real-time techniques at a pulsed reactor.
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  • 80
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    Applied crystallography online 24 (1991), S. 999-1004 
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    Notes: A simple method and simple camera of small size for obtaining X-ray topographs with a microfocus X-ray source are described and initial results and their interpretation are given for an LiF crystal. The method is based on scanning a Kossel line across the recording film by simultaneously translating the crystal and film relative to the source and to a stationary mask that blocks most of the scattered and fluorescence radiation. The mask, which is located between the specimen and the film, is made by using the Kossel line recorded on a film in the mask plane as a pattern; this provides self-alignment of the system. Theoretical calculations are given that indicate the potential angular resolution of the method when applied to nearly perfect crystals. The advantages of this method over similar methods using the X-ray continuum diverging from a point source are discussed.
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    Applied crystallography online 24 (1991), S. 1005-1008 
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    Notes: In the past, crystal structure determination of solids consisting of molecules (or atom groups) whose geometry and size are known approximately has often been attempted using neutron powder diffraction profile refinement techniques, but without inclusion of this information. A method of structure solution has therefore been developed to include it. The proposed method does not require a set of structure factors and thus avoids the problems encountered in separating peaks in a powder diffraction scan. A successful test was conducted with a previously determined (yet treated as unknown) crystal structure, where direct methods had failed to solve the structure due to incorrect peak separation. Two computer programs, MODEL and PARAM, that implement the method are described.
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    Applied crystallography online 24 (1991), S. 1023-1026 
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    Notes: The crystal structures of Zr2CO11 and HfCo7 intermetallic compounds were examined by transmission electron microscopy using both selected-area and convergent-beam electron diffraction. Results show that both have an orthorhombic crystal structure, space group Pcna. The unit cells of both compounds appear to be comprised of two long-period superlattices in antiphase relation to one another along [001].
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    Applied crystallography online 24 (1991), S. 1042-1050 
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    Notes: Very high-energy resolution measurements using X-rays can be achieved by extreme backreflection (Bragg angle close to 90°) from perfect crystals. This technique, combined with the high intensity of X-rays emitted by synchrotron-radiation sources, allowed the development of the instrument INELAX for inelastic scattering experiments. The principles and test results are discussed.
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    Applied crystallography online 24 (1991), S. 1035-1041 
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    Notes: Methods, implemented into a computer program (LSABS), are described which calculate transmission factors and their first derivatives with respect to the positions of the faces of a convex polyhedral monocrystal. Both Gaussian and analytical integration procedures are considered in detail. LSABS has been implemented as a module of the Xtal system of programs. It functions independently of the instrument used to collect the intensity data. Test results obtained with this program are compared with standard literature values. Correlation coefficients of an absorption-corrected intensity data set of calcite, CaCO3 are reported. The need for transmission factor derivatives in the refinement of crystal shape and in the elimination of correlated absorption-corrected structure amplitudes is explained.
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    Applied crystallography online 24 (1991), S. 1027-1034 
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    Notes: A large rapidly decreasing intensity called the `scattering tail' is generally observed at the smallest recorded angles during small-angle measurements of metallic alloys. Since this tail was interpreted as caused by a bimodal phase separation in Cu–Ni–Fe alloys and by long-wavelength concentration fluctuations in Invar alloys, these two systems were re-examined with anomalous X-ray scattering. The variation of the alloying atomic contrasts allows a discrimination between the different types of particles or defects. In neither of the two systems can the tails be interpreted as caused by large-scale concentration fluctuations. In Cu–Ni–Fe alloys, the tail is due to some kind of superficial defect (surface roughness etc.). In Invar alloys, the tail is probably due to residual impurity particles.
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    Applied crystallography online 24 (1991), S. 1015-1022 
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    Notes: X-ray diffraction studies are made on proton conducting polar lithium hydrazinium sulfate and ferroelectric lithium ammonium sulfate. The X-ray rocking curves recorded with in situ electric field along the polar b axis of lithium hydrazinium sulfate (direction of proton conductivity) show a strong enhancement of the 0k0 diffraction intensity. The corresponding 0k0 X-ray topographs reveal extinction contrast consisting of striations parallel to the polar axis. They disappear when the electric field is switched off. The effect is very strong in 0k0 but invisible in h0l reflections. It is present only if the electric field is parallel to the polar axis b. This unusual X-ray topographic contrast is correlated with the proton conduction. It is supposed that, under electric field, an inhomogeneous charge distribution develops, distorting the crystal lattice. Similar experiments on lithium ammonium sulfate also show contrast variations, but of quite different behaviour than before. In this case they result from changes of the ferroelectric domain configuration under electric field.
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    Applied crystallography online 24 (1991), S. 1051-1059 
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    Notes: The intensity profile of the X-ray reflection from a crystalline material is related to the lattice disorder and the distribution of crystal sizes through its Fourier cosine coefficients. However, existing methods of obtaining these structural parameters from the coefficients require more than one order of reflection and this is seldom available with polymer fibres. They also rely heavily on the low-order harmonics which are those determined with least accuracy. The development and testing of a method which overcomes this weakness and which is suitable for use with a single order is described. The coefficients are calculated for a model with paracrystalline disorder and an assumed distribution of crystal sizes and the parameters describing this model are refined to minimize the discrepancy between the calculated and experimental values of the coefficients. Provided the distribution of lengths is asymmetric this discrepancy is no greater than would be expected from experimental error and so the assumed model cannot be rejected on the evidence available. Since a range of model parameters all gave equally good agreement with experiment, it was not possible with a single order to obtain a well defined set of values. Diffraction patterns displaying two orders had been chosen and results from the second order were consistent with the first, only a narrow range satisfying both simultaneously. The method was further developed by calculating the intensity profile from the harmonics and using this in the refinement. There was no advantage over using harmonics; indeed, on occasions the refinement algorithm was unstable producing unreliable results.
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    Applied crystallography online 24 (1991), S. 1060-1062 
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    Notes: The application of an ultrafast analogue-to-digital converter and a high-performance-single board microcomputer permits the construction of a very fast and versatile multichannel analyser (MCA) at low cost. With the powerful instruction set of the microprocessor MC 68000, an intelligent all-round MCA could be realised with useful correction software on the single-board microcomputer. This MCA was used successfully for a data collection by Laue techniques with a four-circle diffractometer.
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    Applied crystallography online 24 (1991), S. 1067-1070 
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    Notes: A new version of DIRECT*SEARCHER (DIRECT-SEARCHER automatic system) for personal computers (PC) consisting of several crystallographic programs has been developed for automatic structure analysis of organic compounds as an innovation of the DS*SYSTEM [Koyama & Okada (1975). Acta Cryst. A31, S18]. Each program is improved and rewritten in Fortran77 for the 32 bit PC. The PC version of DS*SYSTEM is used by organic chemists rather than professional crystallographers.
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    Applied crystallography online 24 (1991), S. 1062-1062 
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    Notes: Owing to a typsetting error, the heading ER was wrongly mis-set as Eg in Table 1 of the paper by Misra, Bisoyi, Khan & Patel [J. Appl. Cryst. (1991), 24, 712–714]. The correct table is given.
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    Applied crystallography online 24 (1991), S. 1071-1072 
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    Notes: A program for the automatic definition of an asymmetric unit is described. Starting from the space-group symbol, an asymmetric unit is automatically calculated by means of a simple algorithm in the case of space groups up to the orthorhombic system. For higher symmetry a tabulation is used.
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    Applied crystallography online 24 (1991), S. 1063-1066 
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    Notes: An automatic processing program system of the molecular replacement method AUTOMR is presented. The program solves the initial model of the target crystal structure using a homologous molecule as the search model. It processes the structure-factor calculation of the model molecule, the rotation function, the translation function and the rigid-group refinement successively in one computer job. Test calculations were performed for six protein crystals and the structures were solved in all of these cases.
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    Applied crystallography online 24 (1991), S. 1072-1073 
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    Applied crystallography online 24 (1991), S. 1079-1079 
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    Applied crystallography online 24 (1991), S. 1074-1075 
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    Applied crystallography online 24 (1991), S. 1073-1074 
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    Notes: A novel method of heavy-atom equilibration with protein crystals is presented. This method utilizes a central drop of mother liquor containing the crystal surrounded by a locus of small drops containing the heavy-atom reagent.
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    Applied crystallography online 24 (1991), S. 1079-1080 
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    Applied crystallography online 24 (1991), S. 1080-1081 
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    Applied crystallography online 24 (1991), S. 1076-1078 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Converse-transformation theory and NIST*LATTICE open a new approach to study many theoretical and practical problems in crystallography. In this approach a new operator, the converse-transformation operator, is defined. The focus of this approach is based on the calculation of groups of matrices relating two lattices and subsequent analysis of these matrices to deduce crystallographic relationships. An efficient algorithm has been designed that has the ability to find all matrices (H) that relate ANY two cells (no matter how skewed) to within any specified tolerances (t) of the cell parameters. A Fortran program, NIST*LATTICE, that enables this new approach to be used is available to the scientific community. There are many immediate applications of converse-transformation analysis including the full automation of the single-crystal diffractometer and phase characterization using lattice-matching techniques.
    Type of Medium: Electronic Resource
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    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 24 (1991), S. 1082-1082 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Type of Medium: Electronic Resource
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