scholarly journals The Determination of Crystallographic Textures From Selected Areas of a Specimen by Electron Diffraction

1983 ◽  
Vol 6 (1) ◽  
pp. 45-61 ◽  
Author(s):  
F. J. Humphreys

A technique for the determination of partial pole figures with an angular resolution of <3°, from selected areas of a thin foil, is described. A microcomputer, interfaced to an unmodified JEOL 100 CX TEMSCAN electron microscope is used to scan a diffraction pattern over a detector, tilt the specimen in steps of 1.5° over a range of ±50°, and plot the resulting data as a semiquantitative pole figure. The application of the technique to the study of materials which deform inhomogeneously is discussed, and examples are given of pole figures obtained from deformed single phase and two phase aluminium specimens.

2000 ◽  
Vol 33 (5) ◽  
pp. 1246-1252 ◽  
Author(s):  
Elizabeth J. Grier ◽  
Amanda K. Petford-Long ◽  
Roger C. C. Ward

Computer simulations of the electron diffraction patterns along the [\bar{1}10] zone axes of four ordered structures within the β-RH2+xphase, withR= Ho or Y, and 0 ≤x≤ 0.25, have been performed to establish whether or not the hydrogen ordering could be detected using electron diffraction techniques. Ordered structures within otherRH2+x(R= Ce, Tb) systems have been characterized with neutron scattering experiments; however, for HoH(D)2+x, neutron scattering failed to characterize the superstructure, possibly because of the lowxconcentration or lack of long-range order within the crystal. This paper aims to show that electron diffraction could overcome both of these problems. The structures considered were the stoichiometric face-centred cubic (f.c.c.) fluorite structure (x= 0), theD1 structure (x= 0.125), theD1astructure (x= 0.2) and theD022structure (x= 0.25). In the stoichiometric structure, with all hydrogen atoms located on the tetrahedral (t) sites, only the diffraction pattern from the f.c.c. metal lattice was seen; however, for the superstoichiometric structures, with the excess hydrogen atoms ordered on the octahedral (o) sites, extra reflections were visible. All the superstoichiometric structures showed extra reflections at the (001)f.c.c.and (110)f.c.c.type positions, with structureD1 also showing extra peaks at (½ ½ ½)f.c.c.. These reflections are not seen in the simulations at similar hydrogen concentrations with the hydrogen atoms randomly occupying theovacancies.


1999 ◽  
Vol 31 (4) ◽  
pp. 239-248 ◽  
Author(s):  
H. Ghildiyal ◽  
E. Jansen ◽  
A. Kirfel

The volume texture of a naturally deformed quartzite from the Kaoko belt, North-West Namibia, has been analysed by both universal stage microscopy and neutron diffraction. Universal stage microscopy is restricted to the determination of the base pinacoid preferred orientation in quartzite. For a more complete description of the texture, the orientations of additional crystal planes, such as first and second order prisms as well as positive and negative rhombs, must be known. Neutron methods allow the evaluation of pole figures of all Bragg reflecting planes, of which those of the first order prisms being considered to be the most active slip planes, are of particular interest. Drawbacks of neutron diffraction, i.e. the faking of an eventually absent inversion centre and lack of resolution, can be overcome by pole figure inversion and subsequent calculation of desired pole figures. Both, universal stage microscopy and neutron diffraction yield well comparable results, of course only with respect to the pole figure of the c-axis.


1979 ◽  
Vol 3 (2) ◽  
pp. 73-83 ◽  
Author(s):  
Ivan Tomov ◽  
H. J. Bunge

In order to evaluate pole-figure measurements quantitatively, one needs the normalization factor which reduces measured intensity values to multiples of the random density. This factor may be determined experimentally by measuring the intensities of a random sample or it may be calculated by integrating over the whole pole-figure or its asymmetric unit. If pole-figure values are not available in the whole angular range 0≤φ≤90° (incomplete pole-figures), then the calculation is in general much more difficult and it usually presumes the knowledge of several pole-figures.In the case of fiber textures (axial symmetry), consisting of only a few strongly preferred orientations with the crystal directions 〈uvw〉i parallel to the axis of symmetry, the normalization factor and hence the volume fractions of the components i may be calculated in a rather simple way requiring only one, possibly incomplete, pole figure.


1987 ◽  
Vol 51 (359) ◽  
pp. 71-86 ◽  
Author(s):  
D. J. Barber ◽  
M. Riaz Khan

AbstractRecent TEM observations of two-phase microstructures and associated crystal defects in selected, rare dolomites have been extended to calcite-structured (R3̄c) carbonates and to other natural and synthetic carbonates that crystallize with the dolomite (R3̄) structure. The samples included siderites (FeCO3), smithsonites (ZnCO3), ankerites (Ca[Mg,Fe](CO3)2), and kutnahorites (Ca[Mn,Fe](CO3)2).TEM methods show that the forms of second phases which result from the presence of common, divalent, metallic impurities are morphologically similar in R3̄c and R3̄ carbonates and occur more widely than hitherto realized. The most common form consists of thin ribbons of second phase which are coherent with and have the same crystallographic orientation as the host carbonate. Another form of microstructure, manifest as modulations in diffraction contrast, appears to be associated with incipient breakdown of single-phase carbonate. The results of extensive TEM/EDS microanalyses show that in siderite and ankerite the formation of ribbons is promoted by Ca impurity or Ca excess (with respect to R3̄c stoichiometry). In smithsonite, Cu and Ca impurities can play similar roles in relation to modulated microstructures. In kutnahorites, the perfection of grains and the absence of second-phase effects is strongly dependent on the ratio of Fe to Mn but is also affected by Ca in excess of the stoichiometric requirement. Electron diffraction results from several of the minerals show c-type spots, which can be interpreted as indicating ordering within basal layers of cations.The results show that, by correlating analytical TEM data with the study of second phases and incipient two-phase microstructures, it should be possible to determine the limits of solid solubility in carbonate systems.


1957 ◽  
Vol 1 ◽  
pp. 131-142
Author(s):  
Otto Renius

AbstractWork at the Detroit Arsenal has shown that techniques similar to those employed for the determination of pole figures of metals can be utilized for studying organic materials such a a stretched rubber latex. The rubber, when stretched, forms a preferred orientation pattern which is proportional in intensity to the degree of elongation, and which can be used to plot a pole figure.A Geiger-counter spectrometer was used to study samples of rubber stretched 600 to 1000 per cent. Using a transmission technique, the specimens were tilted to the impinging X-ray beam in five degree increments while rotating through 360 degrees to allow the measurement of the diffracted beam from the selected atomic planes at various angles within the specimen. The intensities of the diffracted beam at these angles were plotted on a stereographic net to form the pole figures of the (002) and (012) planes of the stretched rubber. The geometry of the sample arrangements permitted the outer portion of the pole figure to be plotted from alpha angle 0 degrees to alpha angle 45 degrees.


1983 ◽  
Vol 16 (1) ◽  
pp. 99-102 ◽  
Author(s):  
O. S. Mayall

The f.c.c. + tetragonal two-phase region of the Cu–Ni–Zn system has been delineated, and unit-cell parameters along the boundaries determined. Apparently anomalous parameter measurements prevented the determination of the tie lines. A pattern of diffraction broadening from the tetragonal phase common to both the two-phase and single-phase regions was related to the variation in lattice spacing of the tetragonal phase along the boundary. Reasons for this broadening are discussed.


1997 ◽  
Vol 3 (S2) ◽  
pp. 755-756
Author(s):  
D. C. Dufner ◽  
R. A. Zingaro ◽  
A. P. Murphy ◽  
C. D. Moody

Since the early 1980s, Se toxicity in wildlife has created a great deal of interest and concern. Reservoirs, marshes, and wetlands in which excessive amounts of Se have been found are considered to be the source of their toxicity problems. Thus, an effective and inexpensive treatment of Se-contaminated waters which significantly lowers the concentration of this element is needed. One such method for removing selenites and selenates from water utilizes iron (II) hydroxide as a reducing agent. In this work, the reduction products are analyzed in the transmission electron microscope (TEM) using electron diffraction and energy-dispersive spectroscopy (EDS) to determine the presence of Se.A “standard” aqueous solution was prepared by the addition of KOH to distilled water to pH 8.8. Sufficient quantities of Na2SeO3 or Na2SeO4 were weighed and dissolved in the “standard” solution to yield SeO3-2 or SeO4-2 ions. A weighed quantity of Fe(NH4)2(SO4)2 was then added to the SeO3-2 or SeO4-2 “standard” solution to form a precipitate of iron hydroxide.


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