Elemental Analysis of Matrix Grain Boundaries in Sic Whisker Reinforced Si3N4 Based Composites

1992 ◽  
Vol 287 ◽  
Author(s):  
J. Liu ◽  
K. Das Chowdhury ◽  
R. W. Carpenter ◽  
W. Braue

ABSTRACTThe structures of SiC/Si3N4 interfaces and Si3N4 matrix grain boundaries in Ceramic Matrix Composites (CMC) were investigated by high resolution electron microscopy. The light element chemistry of the interfaces was analyzed by high spatial resolution (∼3 nm) position resolved EELS in a field emission TEM and by high spatial resolution EDS in a dedicated scanning transmission electron microscope (STEM). High-angle annular dark-field (HAADF) imaging (resolution < 1 nm) technique was used to determine the distribution of yttrium atoms at matrix grain boundaries and at SiC/Si3N4 interfaces. HAADF images suggest that yttrium might diffuse into Si3N4 crystals bounding the interfacial and grain boundary regions.

Author(s):  
Earl J. Kirkland ◽  
Robert J. Keyse

An ultra-high resolution pole piece with a coefficient of spherical aberration Cs=0.7mm. was previously designed for a Vacuum Generators HB-501A Scanning Transmission Electron Microscope (STEM). This lens was used to produce bright field (BF) and annular dark field (ADF) images of (111) silicon with a lattice spacing of 1.92 Å. In this microscope the specimen must be loaded into the lens through the top bore (or exit bore, electrons traveling from the bottom to the top). Thus the top bore must be rather large to accommodate the specimen holder. Unfortunately, a large bore is not ideal for producing low aberrations. The old lens was thus highly asymmetrical, with an upper bore of 8.0mm. Even with this large upper bore it has not been possible to produce a tilting stage, which hampers high resolution microscopy.


Author(s):  
R.D. Leapman ◽  
S.Q. Sun ◽  
S-L. Shi ◽  
R.A. Buchanan ◽  
S.B. Andrews

Recent advances in rapid-freezing and cryosectioning techniques coupled with use of the quantitative signals available in the scanning transmission electron microscope (STEM) can provide us with new methods for determining the water distributions of subcellular compartments. The water content is an important physiological quantity that reflects how fluid and electrolytes are regulated in the cell; it is also required to convert dry weight concentrations of ions obtained from x-ray microanalysis into the more relevant molar ionic concentrations. Here we compare the information about water concentrations from both elastic (annular dark-field) and inelastic (electron energy loss) scattering measurements.In order to utilize the elastic signal it is first necessary to increase contrast by removing the water from the cryosection. After dehydration the tissue can be digitally imaged under low-dose conditions, in the same way that STEM mass mapping of macromolecules is performed. The resulting pixel intensities are then converted into dry mass fractions by using an internal standard, e.g., the mean intensity of the whole image may be taken as representative of the bulk water content of the tissue.


1999 ◽  
Vol 589 ◽  
Author(s):  
Y Kotaka ◽  
T. Yamazaki ◽  
Y Kikuchi ◽  
K. Watanabe

AbstractThe high-angle annular dark-field (HAADF) technique in a dedicated scanning transmission electron microscope (STEM) provides strong compositional sensitivity dependent on atomic number (Z-contrast image). Furthermore, a high spatial resolution image is comparable to that of conventional coherent imaging (HRTEM). However, it is difficult to obtain a clear atomic structure HAADF image using a hybrid TEM/STEM. In this work, HAADF images were obtained with a JEOL JEM-2010F (with a thermal-Schottky field-emission) gun in probe-forming mode at 200 kV. We performed experiments using Si and GaAs in the [110] orientation. The electron-optical conditions were optimized. As a result, the dumbbell structure was observed in an image of [110] Si. Intensity profiles for GaAs along [001] showed differences for the two atomic sites. The experimental images were analyzed and compared with the calculated atomic positions and intensities obtained from Bethe's eigen-value method, which was modified to simulate HAADF-STEM based on Allen and Rossouw's method for convergent-beam electron diffraction (CBED). The experimental results showed a good agreement with the simulation results.


2010 ◽  
Vol 44 (1) ◽  
pp. 111-121 ◽  
Author(s):  
K. Z. Baba-Kishi

Electron diffraction patterns recorded using a scanning transmission electron microscope (STEM) from PbMg1/3Nb2/3O3(PMN) crystallites and PbZn1/3Nb2/3O3(PZN) crystals show weak and systematic continuous diffuse streaking along the 〈110〉 directions. Detailed high-angle annular dark-field (HAADF) images recordedviaan aberration-corrected STEM show that theB-site cations in PMN and PZN undergo correlated and long-range displacements towards the Pb2+ions on the (110) planes. The planarB-site displacement measured from the centres of the octahedra is about 0.3–0.5 Å in PMN and about 0.20–0.4 Å in PZN. In the HAADF images of the PMN crystallites and PZN crystals studied, there is insufficient evidence for systematic long-range planar displacements of the Pb2+ions. The observed Pb2+ion displacements in PMN and PZN appear randomly distributed, mostly displaced along 〈110〉 towards theB-site columns. There is also evidence of possible stress-related distortion in certain unit cells of PMN. In the relaxors studied, two distinct types of displacements were observed: one is the long-range planarB-site spatial displacement on the (110) planes, correlated with the Pb2+ions, possibly resulting in the observed diffuse streaking; the other is short-range Pb2+ion displacement on the (110) planes. The observed displacement status indicates a mutual attraction between the Pb ions and theB-site cations in which theBsites undergo the largest spatial displacements towards the Pb ions along 〈110〉.


1997 ◽  
Vol 3 (S2) ◽  
pp. 443-444
Author(s):  
J. C. Yang ◽  
A. Singhal ◽  
S. Bradley ◽  
J. M. Gibson

Knowledge of catalysts' sizes and shapes on their support material is crucial in understanding catalytic properties. With increasing interest in nanosized catalytic materials, it is vital to obtain structural information at the nanometer level in order to understand their catalytic behavior. We have recently demonstrated that very high angle (˜100mrad) annular dark-field (HAADF) images in a dedicated scanning transmission electron microscope (STEM) can be used to quantitatively measure the number of atoms of individual nano-sized clusters on a support material We are presently applying this technique to a bimetallic catalyst, PtRu5, where our data suggest that the shape of the PtRu5 particle is, surprisingly, oblate on the carbon substrate.PtRu5 is of interest for methanol oxidation for applications in batteries. PtRu5 compounds were produced by a molecular precursor method. Imaging was performed on a Field Emission Gun (FEG) Vacuum Generators HB501 STEM operated at 100kV.


Author(s):  
M. K. Lamvik ◽  
J. M. Pullman ◽  
A. V. Crewe

Negative staining and high resolution shadowing have been extensively used for structural studies in electron microscopy. However, these techniques cover the specimen with a layer of heavy salt or metal, and hence do not allow determination of true mass distribution or localization of specific sites using heavy atom markers. A prerequisite for such structural studies is an examination of unstained specimens. For thin specimens dark field microscopy must be used to obtain adequate contrast. The scanning transmission electron microscope is preferred for such studies since elastic, energyloss, and unscattered electrons can be recorded and analyzed quantitatively to form images with a minimum of beam-induced damage.


Author(s):  
D.D. Perovic ◽  
J.H. Paterson

With the development of crystal growth techniques such as molecular beam epitaxy (MBE), it is now possible to fabricate modulation-doped superlattices consisting of alternating ultrathin layers of n-and/or p-type material abruptly separated by undoped material. At sufficiently high dopant concentrations these abrupt layers may be imaged in cross section by electron microscopy. Pennycook et al. and Treacy et al. have used high angle annular dark-field (HAAD) imaging in the scanning transmission electron microscope (STEM) to image low levels of dopants (∼1 at. %) in semiconductors. This work is concerned with imaging boron and arsenic doped layers in silicon at levels « 1 at.%.Fig. 1 shows a HAAD image of a B-Si superlattice at the <110> zone-axis orientation taken at 100 kV using a VG HB501UX STEM. The bright vertical layers are the B-doped regions, containing ∼4 x 1020 B/cm3. The horizontal lines are due to beam instability while the image was recorded. Fig.2 shows a line scan across the same superlattice, recorded by scanning the beam across the specimen in a direction perpendicular to the layers.


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