Studies of Material Reactions by In Situ High-Resolution Electron Microscopy

MRS Bulletin ◽  
1994 ◽  
Vol 19 (6) ◽  
pp. 26-31 ◽  
Author(s):  
Robert Sinclair

Processing has always been a key component in the development of new materials. Basic scientific understanding of the reactions and transformations that occur has obvious importance in guiding progress. Invaluable insight can be provided by observing the changes during processing, especially at high magnification by in situ microscopy. Now that this can be achieved at the atomic level by using high-resolution electron microscopy (HREM), atomic behavior can be seen directly. Accordingly, many deductions concerning reactions in materials at the atomic scale are possible.The purpose of this article is to illustrate the level reached by in situ HREM. The essential procedure is to form a high-resolution image of a standard transmission electron microscope (TEM) sample and then to alter the structure by some means in a controlled manner, such as by heating. Continual recording on videotape allows subsequent detailed analysis of the behavior, even on a frame-by-frame (1/30 second) basis. The most obvious advantage is to follow the atomic rearrangements directly in real time. However, in addition, by continuous recording no stages in a reaction are missed, which can often occur in a series of conventional ex situ annealed samples because of the limited number of samples that can realistically be examined by HREM. One can be sure that the same reaction, in the same area, is being studied. Furthermore, by changing the temperature systematically, extremely precise kinetic measurements can be made (e.g., for activation energies and kinetic laws) and the whole extent of a material transformation can be investigated in one sample, something that would take months of work if studied conventionally. The information provided by in situ HREM is often unique and so it can become an important technique for fundamental materials investigations.

1986 ◽  
Vol 41 (3) ◽  
pp. 478-482 ◽  
Author(s):  
G. W. Qiao ◽  
J. Zhou ◽  
K. H. Kuo

Application of high resolution electron microscopy (HREM) to the study of Pt-Sn/γ-Al2O3 supported catalyst, zeolites, iron catalyst for ammonia synthesis, rare-earth oxide catalysts, etc., is described. Micro-twins, dislocations and other crystallographic imperfections are observed. Moreover, the structure images of channels representing columns of cages in several kinds of zeolites as well as radiation damage processes in them have been recorded in situ. The observed images of zeolites were found to be in good agreement with the structure model projections and computer simulated images.


1986 ◽  
Vol 82 ◽  
Author(s):  
M. A. Parker ◽  
R. Sinclair

In situ kinetic measurements on the rate of solid—phase epitaxial regrowth of silicon in a conventional transmission electron microscope are described. The data compare well with those established for the sane material by high voltage electron microscopy and by Rutherford backscattering spectroscopy. High—resolution imaging at the same time provides direct information on atomic mechanisms. It is anticipated that this will beccme a more highly developed procedure in due course, especially for studies of interface reactions.


Author(s):  
Jan-Olle Malm ◽  
Jan-Olov Bovin

Understanding of catalytic processes requires detailed knowledge of the catalyst. As heterogeneous catalysis is a surface phenomena the understanding of the atomic surface structure of both the active material and the support material is of utmost importance. This work is a high resolution electron microscopy (HREM) study of different phases found in a used automobile catalytic converter.The high resolution micrographs were obtained with a JEM-4000EX working with a structural resolution better than 0.17 nm and equipped with a Gatan 622 TV-camera with an image intensifier. Some work (e.g. EDS-analysis and diffraction) was done with a JEM-2000FX equipped with a Link AN10000 EDX spectrometer. The catalytic converter in this study has been used under normal driving conditions for several years and has also been poisoned by using leaded fuel. To prepare the sample, parts of the monolith were crushed, dispersed in methanol and a drop of the dispersion was placed on the holey carbon grid.


1986 ◽  
Vol 77 ◽  
Author(s):  
Mary Beth Stearns ◽  
Amanda K. Petford-Long ◽  
C.-H. Chang ◽  
D. G. Stearns ◽  
N. M. Ceglio ◽  
...  

ABSTRACTThe technique of high resolution electron microscopy has been used to examine the structure of several multilayer systems (MLS) on an atomic scale. Mo/Si multilayers, in use in a number of x-ray optical element applications, and Mo/Si multilayers, of interest because of their magnetic properties, have been imaged in cross-section. Layer thicknesses, flatness and smoothness have been analysed: the layer width can vary by up to 0.6nm from the average value, and the layer flatness depends on the quality of the substrate surface for amorphous MLS, and on the details of the crystalline growth for the crystalline materials. The degree of crystallinity and the crystal orientation within the layers have also been investigated. In both cases, the high-Z layers are predominantly crystalline and the Si layers appear amorphous. Amorphous interfacial regions are visible between the Mo and Si layers, and crystalline cobalt suicide interfacial regions between the Co and Si layers. Using the structural measurements obtained from the HREM results, theoretical x-ray reflectivity behaviour has been calculated. It fits the experimental data very well.


1999 ◽  
Vol 571 ◽  
Author(s):  
N. D. Zakharov ◽  
P. Werner ◽  
V. M. Ustinov ◽  
A.R. Kovsh ◽  
G. E. Cirlin ◽  
...  

ABSTRACTQuantum dot structures containing 2 and 7 layers of small coherent InAs clusters embedded into a Si single crystal matrix were grown by MBE. The structure of these clusters was investigated by high resolution transmission electron microscopy. The crystallographic quality of the structure severely depends on the substrate temperature, growth sequence, and the geometrical parameters of the sample. The investigation demonstrates that Si can incorporate a limited volume of InAs in a form of small coherent clusters about 3 nm in diameter. If the deposited InAs layer exceeds a critical thickness, large dislocated InAs precipitates are formed during Si overgrowth accumulating the excess of InAs.


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