Prospecting for gold in a VG STEM

Author(s):  
G. L Shoemaker ◽  
W. M. Sherman ◽  
R. H. Duff ◽  
D. R. Rothbard

A calcined pyritic gold ore concentrate was examined using both ion–milled and ultramicrotomed samples to determine the distribution of gold and the porosity of the matrix supporting the gold. Examinations of the same specimen prepared by different techniques yielded complementary information about the overall characteristics of the material.Figure 1 is a secondary electron image (SEI) of a piece of roasted pyritic ore. The particles are highly porous with morphology suggesting that the iron pyrite (FeS2) particles virtually exploded when labile sulfur was released during oxidative calcination. The particles produced by this process are not large enough to permit ordinary solid specimen preparation techniques. Therefore, a compacted bar of material was made by compressing the powder with a binder to form a disk which was subsequently impregnated with epoxy in a PARR bomb under isostatic pressure of a few thousand psi. From this dense material two types of specimen were prepared, one by diamond knife ultramicrotomy and the other by standard thin foil techniques. For the latter, the sample was sliced with a diamond saw, core–drilled into 3mm disks, polished to about 100μm, dimple ground, and Argon ion milled to perforation. This yielded specimens which show the porosity and connectivity of the iron oxide frameworks formed during calcination. Figure 2 is a 10,000X annular dark field (ADF) image of an ion–milled particle taken with a VG HB501 STEM. The channel structures evident in this image are easily related to the SEI image in Figure 1. Figure 3 is a 200,000X ADF image which illustrates the connectivity of individual iron oxide crystallites that form the skeletal structure. This sample was electron transparent only near the central perforation and did not have a large usable area. Also, the outer surfaces ot the particles may have been milled away during specimen preparation and therefore it is not easy to determine where the remaining structures were located in the original particles.

Author(s):  
F. Shaapur ◽  
M.J. Kim ◽  
Seh Kwang Lee ◽  
Soon Gwang Kim

TEM characterization and microanalysis of the recording media is crucial and complementary to new material system development as well as quality control applications. Due to the type of material generally used for supporting the medium, i.e., a polymer, conventional macro- and microthinning procedures for thin foil preparation are not applicable. Ultramicrotorny (UM) is a viable option and has been employed in previous similar studies. In this work UM has been used for preparation of XTEM samples from a magneto-optical (MO) recording medium in its original production format.The as-received material system consisted of a 4-layer, 2100 Å thick medium including a 300 Å TbFeCo layer enveloped by silicon nitride protective layers supported on a 1.2 mm thick × 135 mm (5.25 in.) diameter polycarbonate disk. Recording tracks had an approximate pitch of 1.6 μm separated by 800 Å deep peripheral grooves. Using a Buehler Isomet low-speed diamond saw, 1 mm wide and 20 mm long strips were cut out of the disk along the recording tracks.


2009 ◽  
Vol 24 (8) ◽  
pp. 2596-2604 ◽  
Author(s):  
Sašo Šturm ◽  
Makoto Shiojiri ◽  
Miran Čeh

The microstructure in AO-excess SrTiO3 (A = Sr2+, Ca2+, Ba2+) ceramics is strongly affected by the formation of Ruddlesden-Popper fault–rich (RP fault) lamellae, which are coherently intergrown with the matrix of the perovskite grains. We studied the structure and chemistry of RP faults by applying quantitative high-resolution transmission electron microscopy and high-angle annular dark-field scanning transmission electron microscopy analyses. We showed that the Sr2+ and Ca2+ dopant ions form RP faults during the initial stage of sintering. The final microstructure showed preferentially grown RP fault lamellae embedded in the central part of the anisotropic perovskite grains. In contrast, the dopant Ba2+ ions preferably substituted for Sr2+ in the SrTiO3 matrix by forming a BaxSr1−xTiO3 solid solution. The surplus of Sr2+ ions was compensated structurally in the later stages of sintering by the formation of SrO-rich RP faults. The resulting microstructure showed RP fault lamellae located at the surface of equiaxed BaxSr1-xTiO3 perovskite grains.


2018 ◽  
Vol 2018 ◽  
pp. 1-12
Author(s):  
N. Baladés ◽  
D. L. Sales ◽  
M. Herrera ◽  
A. M. Raya ◽  
J. C. Hernández-Garrido ◽  
...  

This paper explores the capability of scanning transmission electron microscopy (STEM) techniques in determining the dispersion degree of graphene layers within the carbon matrix by using simulated high-angle annular dark-field (HAADF) images. Results ensure that unmarked graphene layers are only detectable if their orientation is parallel to the microscope beam. Additionally, gold-marked graphene layers allow evaluating the dispersion degree in structural composites. Moreover, electron tomography has been demonstrated to provide truthfully 3D distribution of the graphene sheets inside the matrix when an appropriate reconstruction algorithm and 2D projections including channelling effect are used.


2010 ◽  
Vol 16 (S2) ◽  
pp. 1836-1837
Author(s):  
M Takeguchi ◽  
M Okuda ◽  
A Hashimoto ◽  
K Mitsuishi ◽  
M Shimojo ◽  
...  

Extended abstract of a paper presented at Microscopy and Microanalysis 2010 in Portland, Oregon, USA, August 1 – August 5, 2010.


1999 ◽  
Vol 589 ◽  
Author(s):  
R. Vanfleet ◽  
D.A. Muller ◽  
H.J. Gossmann ◽  
P.H. Citrin ◽  
J. Silcox

AbstractWe report measurements of the distribution of Sb atoms in σ-doped Si, over a wide 2-D concentration range. Both annular dark-field imaging and electron energy loss spectroscopy proved sufficiently sensitive to locate Sb atoms at the atomic scale. Improvements in both detector sensitivities and specimen preparation were necessary to achieve these results, which offer a surprising explanation for the dramatic difference in electrical activity between 2-D and 3-D dopant distributions at the same effective volume concentrations. The prospects for the general identification of individual dopant atoms will be discussed.


Author(s):  
L. Gandolfi ◽  
J. Reiffel

Calculations have been performed on the contrast obtainable, using the Scanning Transmission Electron Microscope, in the observation of thick specimens. Recent research indicates a revival of an earlier interest in the observation of thin specimens with the view of comparing the attainable contrast using both types of specimens.Potential for biological applications of scanning transmission electron microscopy has led to a proliferation of the literature concerning specimen preparation methods and the controversy over “to stain or not to stain” in combination with the use of the dark field operating mode and the same choice of technique using bright field mode of operation has not yet been resolved.


Author(s):  
F. I. Grace ◽  
L. E. Murr

During the course of electron transmission investigations of the deformation structures associated with shock-loaded thin foil specimens of 70/30 brass, it was observed that in a number of instances preferential etching occurred along grain boundaries; and that the degree of etching appeared to depend upon the various experimental conditions prevailing during electropolishing. These included the electrolyte composition, the average current density, and the temperature in the vicinity of the specimen. In the specific case of 70/30 brass shock-loaded at pressures in the range 200-400 kilobars, the predominant mode of deformation was observed to be twin-type faults which in several cases exhibited preferential etching similar to that observed along grain boundaries. A novel feature of this particular phenomenon was that in certain cases, especially for twins located in the vicinity of the specimen edge, the etching or preferential electropolishing literally isolated these structures from the matrix.


Author(s):  
M. Kelly ◽  
D.M. Bird

It is well known that strain fields can have a strong influence on the details of HREM images. This, for example, can cause problems in the analysis of edge-on interfaces between lattice mismatched materials. An interesting alternative to conventional HREM imaging has recently been advanced by Pennycook and co-workers where the intensity variation in the annular dark field (ADF) detector is monitored as a STEM probe is scanned across the specimen. It is believed that the observed atomic-resolution contrast is correlated with the intensity of the STEM probe at the atomic sites and the way in which this varies as the probe moves from cell to cell. As well as providing a directly interpretable high-resolution image, there are reasons for believing that ADF-STEM images may be less suseptible to strain than conventional HREM. This is because HREM images arise from the interference of several diffracted beams, each of which is governed by all the excited Bloch waves in the crystal.


Author(s):  
Prakash Rao

Image shifts in out-of-focus dark field images have been used in the past to determine, for example, epitaxial relationships in thin films. A recent extension of the use of dark field image shifts has been to out-of-focus images in conjunction with stereoviewing to produce an artificial stereo image effect. The technique, called through-focus dark field electron microscopy or 2-1/2D microscopy, basically involves obtaining two beam-tilted dark field images such that one is slightly over-focus and the other slightly under-focus, followed by examination of the two images through a conventional stereoviewer. The elevation differences so produced are usually unrelated to object positions in the thin foil and no specimen tilting is required.In order to produce this artificial stereo effect for the purpose of phase separation and identification, it is first necessary to select a region of the diffraction pattern containing more than just one discrete spot, with the objective aperture.


Author(s):  
D.I. Potter ◽  
A. Taylor

Thermal aging of Ni-12.8 at. % A1 and Ni-12.7 at. % Si produces spatially homogeneous dispersions of cuboidal γ'-Ni3Al or Ni3Si precipitate particles arrayed in the Ni solid solution. We have used 3.5-MeV 58Ni+ ion irradiation to examine the effect of irradiation during precipitation on precipitate morphology and distribution. The nearness of free surfaces produced unusual morphologies in foils thinned prior to irradiation. These thin-foil effects will be important during in-situ investigations of precipitation in the HVEM. The thin foil results can be interpreted in terms of observations from bulk irradiations which are described first.Figure 1a is a dark field image of the γ' precipitate 5000 Å beneath the surface(∿1200 Å short of peak damage) of the Ni-Al alloy irradiated in bulk form. The inhomogeneous spatial distribution of γ' results from the presence of voids and dislocation loops which can be seen in the bright field image of the same area, Fig. 1b.


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