High-Resolution Electron Microscopy of Silicon Carbide-Whisker-Reinforced Alumina Composite Interfaces in Specimens Subjected to Elevated Temperatures

1993 ◽  
Vol 76 (9) ◽  
pp. 2397-2400 ◽  
Author(s):  
Andrew A. Wereszczak ◽  
Azar Parvizi-Majidi ◽  
Karren L. More ◽  
Mattison K. Ferber
Author(s):  
Robert Sinclair

In recent years, there have been many dramatic recordings of dynamic behavior, taken at the atomic level by high-resolution electron microscopy. However in the majority of cases, reliance has been placed on the imaging electron beam to bring about the changes in question. There are many disadvantages to this approach, not the least of which is the lack of experimental control available to the operator. Accordingly we have developed the application of a heating holder to achieve stable elevated temperatures at which reactions can be followed under atomic imaging conditions. This article briefly reviews our progress to-date.Our microscope system is quite conventional, showing that there is no major impediment to hot-stage HREM. We have employed a Philips EM 430 ST (300kV) instrument equipped with a Gatan image pick-up device and a commercial video-recorder. The heating holder is the Philips single tilt sideentry model (PW 6592) which we have found works well up to about 875°C. Of course a double tilt holder is preferable but we overcome the tilting limitations by judicious positioning of cross-section specimens. Image stability can be achieved by heating to a temperature below that of the observation for several minutes before "ramping up" to the desired level.


1992 ◽  
Vol 295 ◽  
Author(s):  
K. Das Chowdhury ◽  
R. W. Carpenter ◽  
W. Braue

AbstractInterfaces in Reaction Bonded Silicon Carbide (RBSC) have been characterized by Analytical and High Resolution Electron Microscopy. Both Si/SiC and SiC/SiC interfaces were free of any oxygen impurity segregation, but contained metallic impurity precipitates. Oxygen was detected in the second phase particles in the SiC grains. A model is presented to explain the evolution of these second phase particles in the SiC grains.


2000 ◽  
Vol 652 ◽  
Author(s):  
K. L. Merkle ◽  
L. J. Thompson ◽  
Fritz Phillipp

ABSTRACTAtomic-scale grain boundary (GB) migration has been directly observed by high-resolution transmission electron microscopy (HREM). Atomic-scale motion of high-angle tilt GBs as well as twist and general GBs at gold island grains with a number of planar facets has been studied at ambient and elevated temperatures. GB migration mechanisms depend on GB structure and geometry. Strong indications for cooperative effects has been found. In this case, as has been proposed before, atoms may undergo small shifts in their lattice positions to be incorporated into the growing grain in a collective mode. At high temperature and in the absence of a strong driving force such small lattice regions are observed to fluctuate back and forth between the two grains. Faceted GBs typically move in spurts. This appears to be inherent to GB migration, whenever the motion is controlled by different structural entities. For some GB geometries the motion was found to proceed by the lateral propagation of atomic-scale steps.


1992 ◽  
Vol 280 ◽  
Author(s):  
Stuart Mckernan ◽  
C. Barry Carter

ABSTRACTIn the oxidation of iron-rich olivine (Mg,Fe)2SiO4 at elevated temperatures interfaces between olivine and the magnetite spinel (Fe3O4) are formed. The orientation relation between these structures is such that the planar spacing for the principal low index planes are very closely matched in the two materials. Regions of different contrast are observed in the olivine up to 5–10 nm from the interface. It is proposed that this contrast is due to enhanced iron concentration in this region caused by the strain field around the magnetite precipitates.


Author(s):  
W. H. Wu ◽  
R. M. Glaeser

Spirillum serpens possesses a surface layer protein which exhibits a regular hexagonal packing of the morphological subunits. A morphological model of the structure of the protein has been proposed at a resolution of about 25 Å, in which the morphological unit might be described as having the appearance of a flared-out, hollow cylinder with six ÅspokesÅ at the flared end. In order to understand the detailed association of the macromolecules, it is necessary to do a high resolution structural analysis. Large, single layered arrays of the surface layer protein have been obtained for this purpose by means of extensive heating in high CaCl2, a procedure derived from that of Buckmire and Murray. Low dose, low temperature electron microscopy has been applied to the large arrays.As a first step, the samples were negatively stained with neutralized phosphotungstic acid, and the specimens were imaged at 40,000 magnification by use of a high resolution cold stage on a JE0L 100B. Low dose images were recorded with exposures of 7-9 electrons/Å2. The micrographs obtained (Fig. 1) were examined by use of optical diffraction (Fig. 2) to tell what areas were especially well ordered.


Author(s):  
Robert A. Grant ◽  
Laura L. Degn ◽  
Wah Chiu ◽  
John Robinson

Proteolytic digestion of the immunoglobulin IgG with papain cleaves the molecule into an antigen binding fragment, Fab, and a compliment binding fragment, Fc. Structures of intact immunoglobulin, Fab and Fc from various sources have been solved by X-ray crystallography. Rabbit Fc can be crystallized as thin platelets suitable for high resolution electron microscopy. The structure of rabbit Fc can be expected to be similar to the known structure of human Fc, making it an ideal specimen for comparing the X-ray and electron crystallographic techniques and for the application of the molecular replacement technique to electron crystallography. Thin protein crystals embedded in ice diffract to high resolution. A low resolution image of a frozen, hydrated crystal can be expected to have a better contrast than a glucose embedded crystal due to the larger density difference between protein and ice compared to protein and glucose. For these reasons we are using an ice embedding technique to prepare the rabbit Fc crystals for molecular structure analysis by electron microscopy.


Author(s):  
J. C. Wheatley ◽  
J. M. Cowley

Rare-earth phosphates are of particular interest because of their catalytic properties associated with the hydrolysis of many aromatic chlorides in the petroleum industry. Lanthanum phosphates (LaPO4) which have been doped with small amounts of copper have shown increased catalytic activity (1). However the physical and chemical characteristics of the samples leading to good catalytic activity are not known.Many catalysts are amorphous and thus do not easily lend themselves to methods of investigation which would include electron microscopy. However, the LaPO4, crystals are quite suitable samples for high resolution techniques.The samples used were obtained from William L. Kehl of Gulf Research and Development Company. The electron microscopy was carried out on a JEOL JEM-100B which had been modified for high resolution microscopy (2). Standard high resolution techniques were employed. Three different sample types were observed: 669A-1-5-7 (poor catalyst), H-L-2 (good catalyst) and 27-011 (good catalyst).


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