scholarly journals The application of X-rays to the study of alloys

Since the middle of last century it has been known that the alloys, obtained by melting together two or more metals, are conglomerates of small crystals. As it is impossible to study them under the polarizing microscope because of their high absorbing power for light, and as they are seldom obtained in crystals with faces sufficiently well developed to allow a measurement of their angles, our crystallographic knowledge has been, until recently, extremely small. When, therefore, the X-ray methods came to the assistance of the metallurgist they were sure of a welcome. In 1922, Bain, using the powder-photograph method of Debye and Hull, carried out some very important pioneering work. In 1924, Owen and Preston, of the National Physical Laboratory, working in conjunction with Rosenhain studied the Cu-Al and Cu-Zn systems. They used a powder method with an ionization spectrometer. Their work marked a great advance, on account of the precision of their measurements and their detailed description of the preparation of the samples of alloys. At the same time Westgren and Phragmen, working in Stockholm with a photographic method, studied independently the same systems as Owen and Preston, and obtained results of equal precision. They extended the work in certain directions by making a more thorough investigation of single crystals. They have now undertaken an extensive research on several alloys and on steels.

In a paper published in the ‘Philosophical Transactions’ in 1908, the writer described some experiments on the X-rays emitted by a variety of metals when used as anticathodes in an X-ray bulb. Among the results established was the homogeneity of a large proportion of the X-rays when the bulb was very “soft.” The absorption curves of the several homogeneous radiations revealed their identities with the characteristic “secondary” radiations which Barkla and Sadler had then recently discovered. The experiments described in the present paper are an extension of the above, and were carried out partly at the Cavendish Laboratory in 1908 and partly at the National Physical Laboratory just prior to the war. The writer’s military duties have prevented the continuation of the work, and the results are now put on record in the hope that they may help to further the progress of the subject, to which the more precise method of the crystal-spectrometer has given a great impetus from a different point of view.


In a previous paper were recorded the results of an investigation into the effects of repetitions of stress on the micro-structure of various metals in the form of crystalline aggregates, the main purpose of the investigation being a study of the causes of fracture under repeated stresses of relatively low magnitude. One important conclusion derived from the experiments was that the action of slipping was not, as had been previously stated, a weakening process in itself. Up to a point the effect of slip was actually to increase the resistance of the metal to further slip. Eventually, however, this strengthening action was exhausted, and failure commenced by the formation of a crack. It was suggested that failure occurred when the amount of strain-hardening by slip exceeded a certain limiting amount. No definite evidence could be obtained on this point, but it was considered that further information might be obtained if attention was directed to a material more simple in structure than a crystalline aggregate. In particular, it was desired to eliminate the effects of the crystal boundaries, whose nature is at present unknown. This could be accomplished if specimens cut entirely from one crystal were employed. Further, it should be possible to verify the assumption, commonly made, that slip bands represent the traces of actual “slip planes” on the surface of the specimen, and to relate these with the atomic structure of the material. Through the kindness of Prof. Carpenter and Miss Elam a number of large single crystals of aluminium were prepared and presented and have been used throughout this work. At that time the necessary experimental facilities for X-ray work were not available to the authors at the National Physical Laboratory. Prof. Carpenter offered to arrange for the X-ray analyses to be undertaken by his assistant, Miss C. F. Elam, at the Royal School of Mines. This offer was gratefully accepted and the authors are greatly indebted to Miss Elam for carrying out this section of the work.


1985 ◽  
Vol 40 (6) ◽  
pp. 726-729 ◽  
Author(s):  
Klaus Güde ◽  
Christoph Hebecker

Abstract Single crystals of KSc2F7 have been prepared from a mixture of KF and ScF3 . The samples were investigated by X-ray methods. KSc2F7 crystallizes orthorhombically with a = 10.643(2), b = 6.540(1), c = 4.030(1) Å. These data indicate a close crystallographic connection to the monoclinic unit cell of KIn2F7 [1], But in contrast to KIn2F7 , KSc2 F7 crystallizes in space group No. 65. Cmmm - D192h. The R-value for 341 observed independent reflections is 0.060.


1984 ◽  
Vol 39 (5) ◽  
pp. 582-585 ◽  
Author(s):  
Klaus Brodersen ◽  
Manfred Cygan ◽  
Hans-Ulrich Hummel

Single crystals of SrHg(SeCN)4 · 4 pyridine are prepared by reaction of K2Hg(SeCN)4 with SrCl2 in CH3OH/C2H5OH in the presence of pyridine.The crystal structure was solved with X-ray methods (Mr = 1024.1, space group P4̄n2, Z = 2, a = 9.552(2) Å, c = 17.610(7) Å, V = 1606.7 Å3, λ(AgKα) = 0.5583 Å, dc = 2.12 g cm-3, μ(AgKα) = 57.40 cm-1, F(000) = 943.7, T = 298 K. Final R = 0.043 for 1050 independent reflections).The structure consists of nearly tetrahedral Hg(SeCN)4-units. The SeCN-group is linear within the experimental error. The N-atoms of SeCN and pyridine contribute to the Archimedean antiprismatic coordination of strontium


2019 ◽  
Vol 88 (1) ◽  
pp. 35-58 ◽  
Author(s):  
Henry N. Chapman

X-ray free-electron lasers provide femtosecond-duration pulses of hard X-rays with a peak brightness approximately one billion times greater than is available at synchrotron radiation facilities. One motivation for the development of such X-ray sources was the proposal to obtain structures of macromolecules, macromolecular complexes, and virus particles, without the need for crystallization, through diffraction measurements of single noncrystalline objects. Initial explorations of this idea and of outrunning radiation damage with femtosecond pulses led to the development of serial crystallography and the ability to obtain high-resolution structures of small crystals without the need for cryogenic cooling. This technique allows the understanding of conformational dynamics and enzymatics and the resolution of intermediate states in reactions over timescales of 100 fs to minutes. The promise of more photons per atom recorded in a diffraction pattern than electrons per atom contributing to an electron micrograph may enable diffraction measurements of single molecules, although challenges remain.


The recent work of Carpenter and Elam on the growth of single crystals of large dimensions has rendered possible the study of the physical constants of single crystals of the commoner metals, and the present communication describes the determination of the thermal and electrical conductivity of aluminium in the form of an isolated crystal. The form of the crystal investigated is shown in fig. 1. This crystal had been prepared at the National Physical Laboratory employing the technique described by Carpenter in “Nature,” p. 266, August 21, 1926, which briefly is as follows:— The test specimen is machined and subjected to three treatments, thermal, mechanical, and thermal. The first treatment is necessary to soften the metal completely and produce new equiaxed crystals of so far as possible uniform size, the average diameter being 1/150 inch. The second consists in straining these crystals to the required amount, and the third in heating the strained crystals to the requisite temperature, so that the potentiality of growth conferred by strain could be brought fully into operation.


1995 ◽  
Vol 50 (4) ◽  
pp. 577-580 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum

Single crystals of (Cu0.22Mg0.78)BaNd2Mo4O16 have been prepared by crystallization from melts and investigated by X-ray methods. The compound crystallizes monoclinically, space group C62h - C12/c1, Z = 4, a = 5.351(1), b = 12.891(2), c = 19.391(4) Å,β = 90.899(14)° and is isotypic to CuKHo2Mo4O16. The crystal structure is dominated by BaO10 and NdO8 polyhedra forming a three-dimensional polyhedra network, which is filled by axially distorted (Cu,Mg)O6 octahedra and MoO4 tetrahedra.


2014 ◽  
Vol 70 (a1) ◽  
pp. C1737-C1737
Author(s):  
Pawel Grochulski ◽  
Miroslaw Cygler ◽  
Michel Fodje ◽  
Shaunivan Labiuk ◽  
James Gorin ◽  
...  

The Canadian Macromolecular Crystallography Facility (CMCF) at the Canadian Light Source (CLS) is a suite of fully automated beamlines, 08ID-1 and 08B1-1 [1]. It serves over 60 Canadian groups plus academic and commercial users in the US. Besides remote data collection, we offer Mail-In service where data are collected by CMCF staff. Beamline 08B1-1 has been in operation since 2011 and beamline 08ID-1 since 2006. When beamline 08ID-1 was designed, over 10 years ago, small crystals were defined as having sizes of 50-100 μm. Today, the most challenging experiments require more intense X-ray beams that can be focused to accommodate much smaller crystal sizes of less than 5 μm with flux on the order of 10^11 photons/s. To reach these stringent parameters, a new more powerful source of X-rays will be required, which will be provided by a longer small-gap in-vacuum undulator (SGU). To accommodate the higher power levels and to focus X-rays to a smaller focal spot with a high degree of spatial and temporal stability, the existing X-ray optical elements need to be upgraded. The remaining components of the project include a 5-axis alignment table for improving alignment of small samples with the microbeam, a high-efficiency robotic sample-changer and a single-photon X-ray detector. Several options for the new design will be discussed. These developments are consistent with the current direction of structural biology research at the CLS [2]. Since 2006 over 225 (240) papers and 400 (444) PDB deposits reported data collected at beamline 08ID-1. Parentheses indicate the total number for the CMCF. Many of these have been published in very high impact journals such as N. Engl. J. Med., Nature, Cell, Science, PNAS, among others (http://cmcf.lightsource.ca/publications/).


2009 ◽  
Vol 42 (3) ◽  
pp. 496-501 ◽  
Author(s):  
A. I. Rykov ◽  
M. Seto ◽  
Y. Ueda ◽  
K. Nomura

Since it is not always feasible to synthesize single crystals of novel materials, the orientation of layered polycrystals has become an attractive basis for studying the angular dependence of inelastic scattering of X-rays or neutrons. Utilizing Rietveld analysis, the anisotropic properties of layered structures in novel manganites and cuprates have been studied with oriented powders instead of single crystals. The phonon density of states (DOS) and atomic thermal displacement are anisotropic in theA-site-ordered manganites LnBaMn2Oyfor the seriesy= 5 andy= 6 (Ln = Y, La, Sm and Gd). This article establishes the angular dependence of the DOS on texture of arbitrary strength, links the textures observed by X-ray and γ-ray techniques, and solves the problem of disentanglement of the Goldanskii–Karyagin effect and texture in Mössbauer spectra.


The Copley Medal is awarded to Sir Lawrence Bragg, O.B.E., M.C., F.R.S. Bragg’s career has precisely coincided with the growth of a major field of science—the X-ray diffraction analysis of crystal structures. This had its beginning in his own early researches, and he has throughout played a principal role by his leadership at a series of laboratories, at Manchester, at the National Physical Laboratory, at Cambridge and at the Royal Institution, and in many other ways. He was the first to determine the atomic arrangement in a crystal (sodium chloride), and this work marked the introduction of a technique which has since been successfully applied to increasingly complicated molecules, culminating in the complete structure determination of the protein lysozyme at the Royal Institution a year before his retirement. Bragg has been prominent in the development of methods, beginning with the Law named after him; he also pioneered or encouraged the application of these methods in several fields—ionic crystals, elementary oxides, silicates, metals and proteins. The striking characteristic of Bragg as a scientist has been his direct and simple approach to complicated physical situations; his solutions of problems have a lucidity and simplicity which, in retrospect, make one forget how baffling they often seemed in advance.


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