Crystal structure of the ξ phase in the Al-Si-Mg-Fe system studied by electron channelling

2002 ◽  
Vol 82 (12) ◽  
pp. 681-686 ◽  
Author(s):  
S. Foss ◽  
C. J. Simensen ◽  
A. Olsen ◽  
J. Tafto
Author(s):  
David C. Joy

In a crystalline solid the regular arrangement of the lattice structure influences the interaction of the incident beam with the specimen, leading to changes in both the transmitted and backscattered signals when the angle of incidence of the beam to the specimen is changed. For the simplest case the electron flux inside the specimen can be visualized as the sum of two, standing wave distributions of electrons (Fig. 1). Bloch wave 1 is concentrated mainly between the atom rows and so only interacts weakly with them. It is therefore transmitted well and backscattered weakly. Bloch wave 2 is concentrated on the line of atom centers and is therefore transmitted poorly and backscattered strongly. The ratio of the excitation of wave 1 to wave 2 varies with the angle between the incident beam and the crystal structure.


2003 ◽  
Vol 59 (1) ◽  
pp. 36-42 ◽  
Author(s):  
S. Foss ◽  
A. Olsen ◽  
C. J. Simensen ◽  
J. Taftø

The crystal structure of the complex π-AlFeMgSi phase, which was previously thought to have the composition Al8FeMg3Si6, has been investigated. Microprobe analysis revealed that the phase has a different composition, Al9FeMg3Si5. The space group was determined and confirmed to be P\bar 62m with the use of parallel-beam electron diffraction (SAD) and convergent-beam electron diffraction (CBED). Owing to symmetry considerations the elements within the unit cell had to be rearranged. The rearrangement was confirmed using electron channelling. The z parameters of the elements were refined by examining the intensities from high-angle convergent-beam electron diffraction. Finally, the x parameters were adjusted slightly to arrive at acceptable interatomic distances.


1987 ◽  
Vol 51 (359) ◽  
pp. 3-19 ◽  
Author(s):  
Geoffrey E. Lloyd

AbstractBackscattered electrons (BSE) are incident electrons reflected back from a target specimen and imaged with the scanning electron microscope (SEM). Three distinct BSE signals exist: atomic number or Z-contrast, in which composition determines image contrast; orientation contrast, in which specimen crystal structure determines image contrast; and electron channelling patterns (ECP), which are unique for a particular crystal orientation. The origins of these three signals are described, with particular attention being given to the necessary SEM operational and specimen preparation requirements. Z-contrast images are relatively simple to obtain and also have a familiar appearance such that their usage should become commonplace. ECP in comparison require subsequent interpretation which depends on the crystal structure and the relationship between crystal and specimen coordinate systems. A general solution to ECP interpretation is therefore presented, involving the construction of reference ‘ECP-maps’ over the surface of a sphere. A brief summary of the applications and potential use of the three BSE signals in the geological sciences is also given.


1991 ◽  
Vol 55 (380) ◽  
pp. 331-345 ◽  
Author(s):  
G. E. Lloyd ◽  
N.-H. Schmidt ◽  
D. Mainprice ◽  
D. J. Prior

AbstractTo material scientists the term texture means the crystallographic orientation of grains in a polycrystal. In contrast, geologists use the term more generally to refer to the spatial arrangement or association of mineral grains in a rock. In this contribution we are concerned with the materials science definition. There are several established techniques available for the determination of crystallographic textures in rocks. It has also been realised that the scanning electron microscope (SEM) is applicable to the study of crystallographic textures via the electron channelling (EC) effect. This provides an image of mineral/rock microstructure (via orientation contrast), as well as a means of accurately indexing their crystal orientations (via electron channelling patterns, ECP). Both types of EC image result from the relationship between incident electron beam and crystal structure, and the subsequent modulation of the backscattered electron (BSE) emission signal according to Bragg's Law. It is a simple matter to switch between the two imaging modes. A related effect, electron backscattering, provides only the diffraction patterns, but has superior spatial resolution and pattern angles.Due to crystal symmetry restrictions, there is only a limited range of ECP configurations possible for any mineral. Individual patterns can therefore be identified by comparison with the complete ‘ECP-map’. The location of an individual pattern within the map area is determined by spherical angles, the exact definition of which depends on the type of fabric diagram (e.g. inverse pole figure, pole figure or orientation distribution function). Originally, these angles were measured manually. A computer program (CHANNEL) has been developed which uses a digitisation approach to pattern recognition, derives the required fabric diagrams and also constructs ECP-maps from standard crystal data (i.e. unit cell parameters etc.).The combination of SEM/EC and CHANNEL dramatically facilitates the study of crystal textures in minerals and rocks, making statistical crystallographic analysis from individual orientations a practicality. The following example applications are considered: (1) crystal structure representation of the Al2SiO5 polymorph system; (2) local crystal texture relationships (epitaxial nucleation) between andalusite and sillimanite grains; (3) bulk rock crystal textures of quartzites; and (4) physical properties (e.g. elastic constants and seismic velocities) determined from bulk rock texture.


Author(s):  
Douglas L. Dorset ◽  
Anthony J. Hancock

Lipids containing long polymethylene chains were among the first compounds subjected to electron diffraction structure analysis. It was only recently realized, however, that various distortions of thin lipid microcrystal plates, e.g. bends, polar group and methyl end plane disorders, etc. (1-3), restrict coherent scattering to the methylene subcell alone, particularly if undistorted molecular layers have well-defined end planes. Thus, ab initio crystal structure determination on a given single uncharacterized natural lipid using electron diffraction data can only hope to identify the subcell packing and the chain axis orientation with respect to the crystal surface. In lipids based on glycerol, for example, conformations of long chains and polar groups about the C-C bonds of this moiety still would remain unknown.One possible means of surmounting this difficulty is to investigate structural analogs of the material of interest in conjunction with the natural compound itself. Suitable analogs to the glycerol lipids are compounds based on the three configurational isomers of cyclopentane-1,2,3-triol shown in Fig. 1, in which three rotameric forms of the natural glycerol derivatives are fixed by the ring structure (4-7).


Author(s):  
George G. Cocks ◽  
Louis Leibovitz ◽  
DoSuk D. Lee

Our understanding of the structure and the formation of inorganic minerals in the bivalve shells has been considerably advanced by the use of electron microscope. However, very little is known about the ultrastructure of valves in the larval stage of the oysters. The present study examines the developmental changes which occur between the time of conception to the early stages of Dissoconch in the Crassostrea virginica(Gmelin), focusing on the initial deposition of inorganic crystals by the oysters.The spawning was induced by elevating the temperature of the seawater where the adult oysters were conditioned. The eggs and sperm were collected separately, then immediately mixed for the fertilizations to occur. Fertilized animals were kept in the incubator where various stages of development were stopped and observed. The detailed analysis of the early stages of growth showed that CaCO3 crystals(aragonite), with orthorhombic crystal structure, are deposited as early as gastrula stage(Figuresla-b). The next stage in development, the prodissoconch, revealed that the crystal orientation is in the form of spherulites.


Author(s):  
F.-R. Chen ◽  
T. L. Lee ◽  
L. J. Chen

YSi2-x thin films were grown by depositing the yttrium metal thin films on (111)Si substrate followed by a rapid thermal annealing (RTA) at 450 to 1100°C. The x value of the YSi2-x films ranges from 0 to 0.3. The (0001) plane of the YSi2-x films have an ideal zero lattice mismatch relative to (111)Si surface lattice. The YSi2 has the hexagonal AlB2 crystal structure. The orientation relationship with Si was determined from the diffraction pattern shown in figure 1(a) to be and . The diffraction pattern in figure 1(a) was taken from a specimen annealed at 500°C for 15 second. As the annealing temperature was increased to 600°C, superlattice diffraction spots appear at position as seen in figure 1(b) which may be due to vacancy ordering in the YSi2-x films. The ordered vacancies in YSi2-x form a mesh in Si plane suggested by a LEED experiment.


Author(s):  
A. F. Marshall ◽  
J. W. Steeds ◽  
D. Bouchet ◽  
S. L. Shinde ◽  
R. G. Walmsley

Convergent beam electron diffraction is a powerful technique for determining the crystal structure of a material in TEM. In this paper we have applied it to the study of the intermetallic phases in the Cu-rich end of the Cu-Zr system. These phases are highly ordered. Their composition and structure has been previously studied by microprobe and x-ray diffraction with sometimes conflicting results.The crystalline phases were obtained by annealing amorphous sputter-deposited Cu-Zr. Specimens were thinned for TEM by ion milling and observed in a Philips EM 400. Due to the large unit cells involved, a small convergence angle of diffraction was used; however, the three-dimensional lattice and symmetry information of convergent beam microdiffraction patterns is still present. The results are as follows:1) 21 at% Zr in Cu: annealed at 500°C for 5 hours. An intermetallic phase, Cu3.6Zr (21.7% Zr), space group P6/m has been proposed near this composition (2). The major phase of our annealed material was hexagonal with a point group determined as 6/m.


Author(s):  
H.-J. Ou ◽  
J. M. Cowley

Using the dedicate VG-HB5 STEM microscope, the crystal structure of high Tc superconductor of YBa2Cu3O7-x has been studied via high resolution STEM (HRSTEM) imaging and nanobeam (∽3A) diffraction patterns. Figure 1(a) and 2(a) illustrate the HRSTEM image taken at 10' times magnification along [001] direction and [100] direction, respectively. In figure 1(a), a grain boundary with strong field contrast is seen between two crystal regions A and B. The grain boundary appears to be parallel to a (110) plane, although it is not possible to determine [100] and [001] axes as it is in other regions which contain twin planes [3]. Following the horizontal lattice lines, from left to right across the grain boundary, a lattice bending of ∽4° is noticed. Three extra lattice planes, indicated by arrows, were found to terminate at the grain boundary and form dislocations. It is believed that due to different chemical composition, such structure defects occur during crystal growth. No bending is observed along the vertical lattice lines.


Author(s):  
L.R. Wallenberg ◽  
J.-O. Bovin ◽  
G. Schmid

Metallic clusters are interesting from various points of view, e.g. as a mean of spreading expensive catalysts on a support, or following heterogeneous and homogeneous catalytic events. It is also possible to study nucleation and growth mechanisms for crystals with the cluster as known starting point.Gold-clusters containing 55 atoms were manufactured by reducing (C6H5)3PAuCl with B2H6 in benzene. The chemical composition was found to be Au9.2[P(C6H5)3]2Cl. Molecular-weight determination by means of an ultracentrifuge gave the formula Au55[P(C6H5)3]Cl6 A model was proposed from Mössbauer spectra by Schmid et al. with cubic close-packing of the 55 gold atoms in a cubeoctahedron as shown in Fig 1. The cluster is almost completely isolated from the surroundings by the twelve triphenylphosphane groups situated in each corner, and the chlorine atoms on the centre of the 3x3 square surfaces. This gives four groups of gold atoms, depending on the different types of surrounding.


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