On the oriented conversion of Ca(OH)2 to CaO

Author(s):  
S. Chatterji ◽  
J. W. Jeffery

SummaryIn order to study the orientational relationship between Ca(OH)2 and CaO, the transformation was carried out in stages inside an electron microscope by condensing the electron beam, and the process was monitored by electron diffraction. It has been found that at the initial stage all the hexagonal spots of Ca(OH)2 split into two ; on further heating one set of spots disappear. The remaining set of spots corresponds to the CaO structure, which has an orientational relationship to the hydroxide structure. To estimate the degree of orientation, a sample of brucite was treated in a similar way to the Ca(OH)2; a comparison shows that a high degree of orientation is preserved in the conversion of Ca(OH)2 to CaO. This observation is contrary to earlier reports.

The beam of an electron microscope has been used to dehydrate single crystals of magnesium hydroxide to magnesium oxide. Electron diffraction photographs and electron micrographs were taken at various stages to follow the crystallographic and morphological changes which accompany decomposition. The decomposition may be considered to occur in two stages. First, there is a small shrinkage in the basal plane, and the resulting strain causes a maze of cracks in the crystal. This change is followed by a collapse of the planes down the original [0001] of magnesium hydroxide. The collapse is controlled by the migration of water molecules from between the planes to a surface where they can escape. The product is a highly oriented aggregate of micro-crystallites of magnesium oxide. More intense irradiation in the electron beam occasionally causes bulk movement of the solid.


1996 ◽  
Vol 452 ◽  
Author(s):  
J. Taylor ◽  
M. Libera ◽  
E. Goldburt ◽  
R. Bhargava

AbstractThis paper presents the results of microstructural studies of terbium-doped yttria quantum nanocrystals by imaging and diffraction in a transmission electron microscope. The nanocrystals are typically found in clusters of varying size. Electron energy-loss spectroscopy confirms that the particles consist of yttrium and oxygen. Analysis of selected-area electron diffraction patterns shows that the nanocrystals largely have the cubic structure found in bulk yttria. These patterns furthermore suggest that within each cluster the nanocrystals align themselves with a preferred orientation relative to the incident electron beam as well as to each other.


1951 ◽  
Vol 29 (2) ◽  
pp. 122-128 ◽  
Author(s):  
D. E. McLennan

Electron bombardment experiments have been carried out on small crystals of the alkali halides within the electron microscope. Crystals of two size ranges were bombarded at high intensity, and evidence of a generalized photographic effect within the ionic group of solids is presented. The first group of crystal specimens ranged in size from 0.2 to 0.002 cm., the bombardment causing the formation of F-centers and entrapped metal colloids in the crystal lattice. Ionization pulses were observed to occur in the region of the specimen during bombardment. The second group ranged in size from 10 to 0.01 μ, observations on the effects of bombardment being carried out with electron diffraction techniques. A process has been suggested to explain the phenomenon of ionic crystals which appear to lose their centers under high electron beam intensity in the electron microscope.


Author(s):  
Carolyn Nohr ◽  
Ann Ayres

Texts on electron diffraction recommend that the camera constant of the electron microscope be determine d by calibration with a standard crystalline specimen, using the equation


Author(s):  
Chester J. Calbick ◽  
Richard E. Hartman

Quantitative studies of the phenomenon associated with reactions induced by the electron beam between specimens and gases present in the electron microscope require precise knowledge and control of the local environment experienced by the portion of the specimen in the electron beam. Because of outgassing phenomena, the environment at the irradiated portion of the specimen is very different from that in any place where gas pressures and compositions can be measured. We have found that differential pumping of the specimen chamber by a 4" Orb-Ion pump, following roughing by a zeolite sorption pump, can produce a specimen-chamber pressure 100- to 1000-fold less than that in the region below the objective lens.


Author(s):  
R. C. Moretz ◽  
D. F. Parsons

Short lifetime or total absence of electron diffraction of ordered biological specimens is an indication that the specimen undergoes extensive molecular structural damage in the electron microscope. The specimen damage is due to the interaction of the electron beam (40-100 kV) with the specimen and the total removal of water from the structure by vacuum drying. The lower percentage of inelastic scattering at 1 MeV makes it possible to minimize the beam damage to the specimen. The elimination of vacuum drying by modification of the electron microscope is expected to allow more meaningful investigations of biological specimens at 100 kV until 1 MeV electron microscopes become more readily available. One modification, two-film microchambers, has been explored for both biological and non-biological studies.


Author(s):  
R. Sinclair ◽  
B.E. Jacobson

INTRODUCTIONThe prospect of performing chemical analysis of thin specimens at any desired level of resolution is particularly appealing to the materials scientist. Commercial TEM-based systems are now available which virtually provide this capability. The purpose of this contribution is to illustrate its application to problems which would have been intractable until recently, pointing out some current limitations.X-RAY ANALYSISIn an attempt to fabricate superconducting materials with high critical currents and temperature, thin Nb3Sn films have been prepared by electron beam vapor deposition [1]. Fine-grain size material is desirable which may be achieved by codeposition with small amounts of Al2O3 . Figure 1 shows the STEM microstructure, with large (∽ 200 Å dia) voids present at the grain boundaries. Higher quality TEM micrographs (e.g. fig. 2) reveal the presence of small voids within the grains which are absent in pure Nb3Sn prepared under identical conditions. The X-ray spectrum from large (∽ lμ dia) or small (∽100 Ǻ dia) areas within the grains indicates only small amounts of A1 (fig.3).


Author(s):  
J. C. Ingram ◽  
P. R. Strutt ◽  
Wen-Shian Tzeng

The invisibility criterion which is the standard technique for determining the nature of dislocations seen in the electron microscope can at times lead to erroneous results or at best cause confusion in many cases since the dislocation can still show a residual image if the term is non-zero, or if the edge and screw displacements are anisotropically coupled, or if the dislocation has a mixed character. The symmetry criterion discussed below can be used in conjunction with and in some cases supersede the invisibility criterion for obtaining a valid determination of the nature of the dislocation.The symmetry criterion is based upon the well-known fact that a dislocation, because of the symmetric nature of its displacement field, can show a symmetric image when the dislocation is correctly oriented with respect to the electron beam.


Author(s):  
Willem H.J. Andersen

Electron microscope design, and particularly the design of the imaging system, has reached a high degree of perfection. Present objective lenses perform up to their theoretical limit, while the whole imaging system, consisting of three or four lenses, provides very wide ranges of magnification and diffraction camera length with virtually no distortion of the image. Evolution of the electron microscope in to a routine research tool in which objects of steadily increasing thickness are investigated, has made it necessary for the designer to pay special attention to the chromatic aberrations of the magnification system (as distinct from the chromatic aberration of the objective lens). These chromatic aberrations cause edge un-sharpness of the image due to electrons which have suffered energy losses in the object.There exist two kinds of chromatic aberration of the magnification system; the chromatic change of magnification, characterized by the coefficient Cm, and the chromatic change of rotation given by Cp.


Author(s):  
Robert M. Glaeser ◽  
Bing K. Jap

The dynamical scattering effect, which can be described as the failure of the first Born approximation, is perhaps the most important factor that has prevented the widespread use of electron diffraction intensities for crystallographic structure determination. It would seem to be quite certain that dynamical effects will also interfere with structure analysis based upon electron microscope image data, whenever the dynamical effect seriously perturbs the diffracted wave. While it is normally taken for granted that the dynamical effect must be taken into consideration in materials science applications of electron microscopy, very little attention has been given to this problem in the biological sciences.


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