scholarly journals Automated mapping of the crystallographic sample orientation from diffraction patterns in momentum-resolved STEM

2021 ◽  
Vol 27 (S1) ◽  
pp. 1444-1445
Author(s):  
Mauricio Cattaneo ◽  
Knut Müller-Caspary ◽  
Juri Barthel ◽  
Katherine MacArthur ◽  
Marta Lipinska-Chwalek
Keyword(s):  
Automated Mapping ◽  
Sample Orientation ◽  
Diffraction Patterns

Imogolite: a unique aluminosilicate

Clay Minerals ◽  
1969 ◽  
Vol 8 (1) ◽  
pp. 87-99 ◽  
Author(s):  
J. D. Russell ◽  
W. J. McHardy ◽  
A. R. Fraser
Keyword(s):  
Electron Diffraction ◽  
Infrared Absorption ◽  
Chain Structure ◽  
Absorption Bands ◽  
Repeat Units ◽  
Sample Orientation ◽  
Different Types ◽  
Stretching Vibrations ◽  
Diffraction Patterns ◽  
Silicate Chain

The fibrous aluminosilicate imogolite has been studied by electronoptical and infrared absorption methods. Electron diffraction patterns are interpreted in terms of repeat units of 8·4 Å parallel and 23 Å perpendicular to the fibre axis. These spacings can not be reconciled with a continuous silicate chain structure and this conclusion is supported by an Si-O vibration near 930 cm−1. A structure is postulated in which distorted chains of Al-O octahedra are cross-linked through isolated Si2O7 groups.Multiple OH stretching vibrations indicate different types of OH group in the imogolite structure. Absorption bands near 1000, 700 and 600 cm−1 are sensitive to sample orientation. This is attributed to the morphology and dimensions of the imogolite fibres.

scholarly journals Dictionary Indexing of Electron Channeling Patterns

2017 ◽  
Vol 23 (1) ◽  
pp. 1-10 ◽  
Author(s):  
Saransh Singh ◽  
Marc De Graef
Keyword(s):  
Electron Channeling ◽  
Orientation Space ◽  
Derivative Free Optimization ◽  
Indexing Method ◽  
Derivative Free ◽  
Sample Orientation ◽  
Master Pattern ◽  
Diffraction Patterns ◽  
Detector Model ◽  
Bound Optimization

AbstractThe dictionary-based approach to the indexing of diffraction patterns is applied to electron channeling patterns (ECPs). The main ingredients of the dictionary method are introduced, including the generalized forward projector (GFP), the relevant detector model, and a scheme to uniformly sample orientation space using the “cubochoric” representation. The GFP is used to compute an ECP “master” pattern. Derivative free optimization algorithms, including the Nelder–Mead simplex and the bound optimization by quadratic approximation are used to determine the correct detector parameters and to refine the orientation obtained from the dictionary approach. The indexing method is applied to poly-silicon and shows excellent agreement with the calibrated values. Finally, it is shown that the method results in a mean disorientation error of 1.0° with 0.5° SD for a range of detector parameters.

Light Optical Diffraction Studies of Macromolecular Ultrastructure

1970 ◽  
Vol 28 ◽  
pp. 258-259
Author(s):  
Glen B. Haydon
Keyword(s):  
High Resolution ◽  
Diffraction Analysis ◽  
Diffraction Pattern ◽  
Electron Micrographs ◽  
Optical Diffraction ◽  
Electron Micrograph ◽  
Its Analysis ◽  
Resolution Electron ◽  
Diffraction Patterns

Analysis of light optical diffraction patterns produced by electron micrographs can easily lead to much nonsense. Such diffraction patterns are referred to as optical transforms and are compared with transforms produced by a variety of mathematical manipulations. In the use of light optical diffraction patterns to study periodicities in macromolecular ultrastructures, a number of potential pitfalls have been rediscovered. The limitations apply to the formation of the electron micrograph as well as its analysis.(1) The high resolution electron micrograph is itself a complex diffraction pattern resulting from the specimen, its stain, and its supporting substrate. Cowley and Moodie (Proc. Phys. Soc. B, LXX 497, 1957) demonstrated changing image patterns with changes in focus. Similar defocus images have been subjected to further light optical diffraction analysis.

Electron microscopy and diffraction studies of polyimides

1983 ◽  
Vol 41 ◽  
pp. 28-29
Author(s):  
O.C. de Hodgins ◽  
K. R. Lawless ◽  
R. Anderson
Keyword(s):  
Electron Microscopy ◽  
Electron Microscope ◽  
Structural Features ◽  
Inert Atmosphere ◽  
Polyimide Films ◽  
Resolution Electron ◽  
The Matrix ◽  
High Resolution Electron Microscope ◽  
Diffraction Patterns ◽  
Polymeric Samples

Commercial polyimide films have shown to be homogeneous on a scale of 5 to 200 nm. The observation of Skybond (SKB) 705 and PI5878 was carried out by using a Philips 400, 120 KeV STEM. The objective was to elucidate the structural features of the polymeric samples. The specimens were spun and cured at stepped temperatures in an inert atmosphere and cooled slowly for eight hours. TEM micrographs showed heterogeneities (or nodular structures) generally on a scale of 100 nm for PI5878 and approximately 40 nm for SKB 705, present in large volume fractions of both specimens. See Figures 1 and 2. It is possible that the nodulus observed may be associated with surface effects and the structure of the polymers be regarded as random amorphous arrays. Diffraction patterns of the matrix and the nodular areas showed different amorphous ring patterns in both materials. The specimens were viewed in both bright and dark fields using a high resolution electron microscope which provided magnifications of 100,000X or more on the photographic plates if desired.

Two Investigations into Grain Boundary Structure

1977 ◽  
Vol 35 ◽  
pp. 688-691
Author(s):  
P. Humble
Keyword(s):  
Grain Boundary ◽  
Dark Field ◽  
Boundary Structure ◽  
Boundary Dislocation ◽  
Bright Field ◽  
Intrinsic Structure ◽  
Weak Beam ◽  
Grain Boundary Structure ◽  
Independent Information ◽  
Diffraction Patterns

There has been sustained interest over the last few years into both the intrinsic (primary and secondary) structure of grain boundaries and the extrinsic structure e.g. the interaction of matrix dislocations with the boundary. Most of the investigations carried out by electron microscopy have involved only the use of information contained in the transmitted image (bright field, dark field, weak beam etc.). Whilst these imaging modes are appropriate to the cases of relatively coarse intrinsic or extrinsic grain boundary dislocation structures, it is apparent that in principle (and indeed in practice, e.g. (1)-(3)) the diffraction patterns from the boundary can give extra independent information about the fine scale periodic intrinsic structure of the boundary.In this paper I shall describe one investigation into each type of structure using the appropriate method of obtaining the necessary information which has been carried out recently at Tribophysics.

Disappearance Voltage Determinations Using a Convergent Beam

1971 ◽  
Vol 29 ◽  
pp. 184-185
Author(s):  
W. L. Bell
Keyword(s):  
Second Order ◽  
Objective Method ◽  
Uniform Thickness ◽  
Rocking Curve ◽  
Crystal Perfection ◽  
Kikuchi Line ◽  
Central Maximum ◽  
Diffraction Patterns ◽  
Convergent Beam ◽  
Beam Technique

Disappearance voltages for second order reflections can be determined experimentally in a variety of ways. The more subjective methods, such as Kikuchi line disappearance and bend contour imaging, involve comparing a series of diffraction patterns or micrographs taken at intervals throughout the disappearance range and selecting that voltage which gives the strongest disappearance effect. The estimated accuracies of these methods are both to within 10 kV, or about 2-4%, of the true disappearance voltage, which is quite sufficient for using these voltages in further calculations. However, it is the necessity of determining this information by comparisons of exposed plates rather than while operating the microscope that detracts from the immediate usefulness of these methods if there is reason to perform experiments at an unknown disappearance voltage.The convergent beam technique for determining the disappearance voltage has been found to be a highly objective method when it is applicable, i.e. when reasonable crystal perfection exists and an area of uniform thickness can be found. The criterion for determining this voltage is that the central maximum disappear from the rocking curve for the second order spot.

Electronic Cone Illumination with the Conventional Transmission Electron Microscope

1977 ◽  
Vol 35 ◽  
pp. 72-73
Author(s):  
William Krakow
Keyword(s):  
Electronic Device ◽  
Chromatic Aberration ◽  
Objective Lens ◽  
Hollow Cone ◽  
Transmission Electron ◽  
Lissajous Figures ◽  
High Resolution Images ◽  
Imaging Mode ◽  
Diffraction Patterns ◽  
Transmission Microscope

An electronic device has been constructed which manipulates the primary beam in the conventional transmission microscope to illuminate a specimen under a variety of virtual condenser aperture conditions. The device uses the existing tilt coils of the microscope, and modulates the D.C. signals to both x and y tilt directions simultaneously with various waveforms to produce Lissajous figures in the back-focal plane of the objective lens. Electron diffraction patterns can be recorded which reflect the manner in which the direct beam is tilted during exposure of a micrograph. The device has been utilized mainly for the hollow cone imaging mode where the device provides a microscope transfer function without zeros in all spatial directions and has produced high resolution images which are also free from the effect of chromatic aberration. A standard second condenser aperture is employed and the width of the cone annulus is readily controlled by defocusing the second condenser lens.

Computer Indexing of Electron Diffraction Patterns Including the Effects of Lattice Symmetry

1977 ◽  
Vol 35 ◽  
pp. 22-23
Author(s):  
J. S. Lally ◽  
R. J. Lee
Keyword(s):  
Electron Diffraction ◽  
Zone Axis ◽  
Crystal Thickness ◽  
Double Diffraction ◽  
Automated Method ◽  
Lattice Symmetry ◽  
Intensity Calculations ◽  
Unknown Structure ◽  
Diffraction Patterns ◽  
Orientation Parameters

In the 50 year period since the discovery of electron diffraction from crystals there has been much theoretical effort devoted to the calculation of diffracted intensities as a function of crystal thickness, orientation, and structure. However, in many applications of electron diffraction what is required is a simple identification of an unknown structure when some of the shape and orientation parameters required for intensity calculations are not known. In these circumstances an automated method is needed to solve diffraction patterns obtained near crystal zone axis directions that includes the effects of systematic absences of reflections due to lattice symmetry effects and additional reflections due to double diffraction processes.Two programs have been developed to enable relatively inexperienced microscopists to identify unknown crystals from diffraction patterns. Before indexing any given electron diffraction pattern, a set of possible crystal structures must be selected for comparison against the unknown.

Evaluation of Freezing Methods by Low Temperature X-Ray Diffraction

1977 ◽  
Vol 35 ◽  
pp. 330-333
Author(s):  
T. Gulik-Krzywicki ◽  
M.J. Costello
Keyword(s):  
Biological Materials ◽  
Molecular Organization ◽  
X Ray Diffraction ◽  
Glass Capillary ◽  
X Ray ◽  
Rate Dependent ◽  
Before And After ◽  
Freeze Etching ◽  
Diffraction Patterns ◽  
Set Up

Freeze-etching electron microscopy is currently one of the best methods for studying molecular organization of biological materials. Its application, however, is still limited by our imprecise knowledge about the perturbations of the original organization which may occur during quenching and fracturing of the samples and during the replication of fractured surfaces. Although it is well known that the preservation of the molecular organization of biological materials is critically dependent on the rate of freezing of the samples, little information is presently available concerning the nature and the extent of freezing-rate dependent perturbations of the original organizations. In order to obtain this information, we have developed a method based on the comparison of x-ray diffraction patterns of samples before and after freezing, prior to fracturing and replication.Our experimental set-up is shown in Fig. 1. The sample to be quenched is placed on its holder which is then mounted on a small metal holder (O) fixed on a glass capillary (p), whose position is controlled by a micromanipulator.

Electron-diffraction studies in synthetic polymer materials

1983 ◽  
Vol 41 ◽  
pp. 362-365
Author(s):  
D.T. Grubb
Keyword(s):  
Electron Diffraction ◽  
Synthetic Polymer ◽  
Polymer Materials ◽  
Crystallographic Structure ◽  
High Dose ◽  
Electron Dose ◽  
Dose Rates ◽  
First Case ◽  
Diffraction Patterns ◽  
The Many

Diffraction studies in polymeric and other beam sensitive materials may bring to mind the many experiments where diffracted intensity has been used as a measure of the electron dose required to destroy fine structure in the TEM. But this paper is concerned with a range of cases where the diffraction pattern itself contains the important information.In the first case, electron diffraction from paraffins, degraded polyethylene and polyethylene single crystals, all the samples are highly ordered, and their crystallographic structure is well known. The diffraction patterns fade on irradiation and may also change considerably in a-spacing, increasing the unit cell volume on irradiation. The effect is large and continuous far C94H190 paraffin and for PE, while for shorter chains to C 28H58 the change is less, levelling off at high dose, Fig.l. It is also found that the change in a-spacing increases at higher dose rates and at higher irradiation temperatures.

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