Polytype identification in trioctahedral 1:1 layer silicates using electron diffraction with application to a chronstedtite that was synthesized using metallic iron-clay interactions

2018 ◽  
Vol 66 (4) ◽  
pp. 379-402 ◽  
Author(s):  
Jiří Hybler ◽  
Mariana Klementová ◽  
Markéta Jarošová ◽  
Isabella Pignatelli ◽  
Régine Mosser-Ruck ◽  
...  
Author(s):  
Douglas L. Dorset

Recently the direct 3D determination of an aluminosilicate structure was reported based on high-voltage, high resolution electron microscopy of thin slices representing several projections of the crystal. It was particularly interesting that the relatively light oxygen atom positions could be visualized along with those of heavier components (Al, Si, Fe) in the staurolite structure.Although this direct visualization of a crystal structure in the electron microscope certainly is a tour de force, representing a significant advance in microscopic instrumentation and technique, the electron crystallography of silicate structures at atomic resolution is, in itself, not particularly a new field of investigation. For example, in his book, B. B. Zvyagin outlines how he was able to use texture electron diffraction intensity data from several layer silicates in order to determine their crystal structures via interpretation of the Patterson function or construction of reasonable layer models suggested by the atomic stoichiometry.It is unfortunate that many of the early Russian electron diffraction structure analyses have been overlooked or even ignored by the crystallographic community.


Author(s):  
S.W. Hui ◽  
D.F. Parsons

The development of the hydration stages for electron microscopes has opened up the application of electron diffraction in the study of biological membranes. Membrane specimen can now be observed without the artifacts introduced during drying, fixation and staining. The advantages of the electron diffraction technique, such as the abilities to observe small areas and thin specimens, to image and to screen impurities, to vary the camera length, and to reduce data collection time are fully utilized. Here we report our pioneering work in this area.


Author(s):  
J. B. Warren

Electron diffraction intensity profiles have been used extensively in studies of polycrystalline and amorphous thin films. In previous work, diffraction intensity profiles were quantitized either by mechanically scanning the photographic emulsion with a densitometer or by using deflection coils to scan the diffraction pattern over a stationary detector. Such methods tend to be slow, and the intensities must still be converted from analog to digital form for quantitative analysis. The Instrumentation Division at Brookhaven has designed and constructed a electron diffractometer, based on a silicon photodiode array, that overcomes these disadvantages. The instrument is compact (Fig. 1), can be used with any unmodified electron microscope, and acquires the data in a form immediately accessible by microcomputer.Major components include a RETICON 1024 element photodiode array for the de tector, an Analog Devices MAS-1202 analog digital converter and a Digital Equipment LSI 11/2 microcomputer. The photodiode array cannot detect high energy electrons without damage so an f/1.4 lens is used to focus the phosphor screen image of the diffraction pattern on to the photodiode array.


Author(s):  
P. Ling ◽  
R. Gronsky ◽  
J. Washburn

The defect microstructures of Si arising from ion implantation and subsequent regrowth for a (111) substrate have been found to be dominated by microtwins. Figure 1(a) is a typical diffraction pattern of annealed ion-implanted (111) Si showing two groups of extra diffraction spots; one at positions (m, n integers), the other at adjacent positions between <000> and <220>. The object of the present paper is to show that these extra reflections are a direct consequence of the microtwins in the material.


Author(s):  
R. E. Ferrell ◽  
G. G. Paulson ◽  
C. W. Walker

Selected area electron diffraction (SAD) has been used successfully to determine crystal structures, identify traces of minerals in rocks, and characterize the phases formed during thermal treatment of micron-sized particles. There is an increased interest in the method because it has the potential capability of identifying micron-sized pollutants in air and water samples. This paper is a short review of the theory behind SAD and a discussion of the sample preparation employed for the analysis of multiple component environmental samples.


Author(s):  
G. Lehmpfuhl

Introduction In electron microscopic investigations of crystalline specimens the direct observation of the electron diffraction pattern gives additional information about the specimen. The quality of this information depends on the quality of the crystals or the crystal area contributing to the diffraction pattern. By selected area diffraction in a conventional electron microscope, specimen areas as small as 1 µ in diameter can be investigated. It is well known that crystal areas of that size which must be thin enough (in the order of 1000 Å) for electron microscopic investigations are normally somewhat distorted by bending, or they are not homogeneous. Furthermore, the crystal surface is not well defined over such a large area. These are facts which cause reduction of information in the diffraction pattern. The intensity of a diffraction spot, for example, depends on the crystal thickness. If the thickness is not uniform over the investigated area, one observes an averaged intensity, so that the intensity distribution in the diffraction pattern cannot be used for an analysis unless additional information is available.


Author(s):  
R.A. Ploc ◽  
G.H. Keech

An unambiguous analysis of transmission electron diffraction effects requires two samplings of the reciprocal lattice (RL). However, extracting definitive information from the patterns is difficult even for a general orthorhombic case. The usual procedure has been to deduce the approximate variables controlling the formation of the patterns from qualitative observations. Our present purpose is to illustrate two applications of a computer programme written for the analysis of transmission, selected area diffraction (SAD) patterns; the studies of RL spot shapes and epitaxy.When a specimen contains fine structure the RL spots become complex shapes with extensions in one or more directions. If the number and directions of these extensions can be estimated from an SAD pattern the exact spot shape can be determined by a series of refinements of the computer input data.


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

Electron microscopy and diffraction of biological materials in the hydrated state requires the construction of a chamber in which the water vapor pressure can be maintained at saturation for a given specimen temperature, while minimally affecting the normal vacuum of the remainder of the microscope column. Initial studies with chambers closed by thin membrane windows showed that at the film thicknesses required for electron diffraction at 100 KV the window failure rate was too high to give a reliable system. A single stage, differentially pumped specimen hydration chamber was constructed, consisting of two apertures (70-100μ), which eliminated the necessity of thin membrane windows. This system was used to obtain electron diffraction and electron microscopy of water droplets and thin water films. However, a period of dehydration occurred during initial pumping of the microscope column. Although rehydration occurred within five minutes, biological materials were irreversibly damaged. Another limitation of this system was that the specimen grid was clamped between the apertures, thus limiting the yield of view to the aperture opening.


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):  
Douglas L. Dorset ◽  
Anthony J. Hancock

Lipids containing long polymethylene chains were among the first compounds subjected to electron diffraction structure analysis. It was only recently realized, however, that various distortions of thin lipid microcrystal plates, e.g. bends, polar group and methyl end plane disorders, etc. (1-3), restrict coherent scattering to the methylene subcell alone, particularly if undistorted molecular layers have well-defined end planes. Thus, ab initio crystal structure determination on a given single uncharacterized natural lipid using electron diffraction data can only hope to identify the subcell packing and the chain axis orientation with respect to the crystal surface. In lipids based on glycerol, for example, conformations of long chains and polar groups about the C-C bonds of this moiety still would remain unknown.One possible means of surmounting this difficulty is to investigate structural analogs of the material of interest in conjunction with the natural compound itself. Suitable analogs to the glycerol lipids are compounds based on the three configurational isomers of cyclopentane-1,2,3-triol shown in Fig. 1, in which three rotameric forms of the natural glycerol derivatives are fixed by the ring structure (4-7).


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