Structural studies of small amorphous volumes by electron diffraction

Author(s):  
Pierre Moine

Qualitatively, amorphous structures can be easily revealed and differentiated from crystalline phases by their Transmission Electron Microscopy (TEM) images and their diffraction patterns (fig.1 and 2) but, for quantitative structural information, electron diffraction pattern intensity analyses are necessary. The parameters describing the structure of an amorphous specimen have been introduced in the context of scattering experiments which have been, so far, the most used techniques to obtain structural information in the form of statistical averages. When only small amorphous volumes (< 1/μm in size or thickness) are available, the much higher scattering of electrons (compared to neutrons or x rays) makes, despite its drawbacks, electron diffraction extremely valuable and often the only feasible technique.In a diffraction experiment, the intensity IN (Q) of a radiation, elastically scattered by N atoms of a sample, is measured and related to the atomic structure, using the fundamental relation (Born approximation) : IN(Q) = |FT[U(r)]|.

Author(s):  
R.P. Goehner ◽  
W.T. Hatfield ◽  
Prakash Rao

Computer programs are now available in various laboratories for the indexing and simulation of transmission electron diffraction patterns. Although these programs address themselves to the solution of various aspects of the indexing and simulation process, the ultimate goal is to perform real time diffraction pattern analysis directly off of the imaging screen of the transmission electron microscope. The program to be described in this paper represents one step prior to real time analysis. It involves the combination of two programs, described in an earlier paper(l), into a single program for use on an interactive basis with a minicomputer. In our case, the minicomputer is an INTERDATA 70 equipped with a Tektronix 4010-1 graphical display terminal and hard copy unit.A simplified flow diagram of the combined program, written in Fortran IV, is shown in Figure 1. It consists of two programs INDEX and TEDP which index and simulate electron diffraction patterns respectively. The user has the option of choosing either the indexing or simulating aspects of the combined program.


Author(s):  
John F. Mansfield

One of the most important advancements of the transmission electron microscopy (TEM) in recent years has been the development of the analytical electron microscope (AEM). The microanalytical capabilities of AEMs are based on the three major techniques that have been refined in the last decade or so, namely, Convergent Beam Electron Diffraction (CBED), X-ray Energy Dispersive Spectroscopy (XEDS) and Electron Energy Loss Spectroscopy (EELS). Each of these techniques can yield information on the specimen under study that is not obtainable by any other means. However, it is when they are used in concert that they are most powerful. The application of CBED in materials science is not restricted to microanalysis. However, this is the area where it is most frequently employed. It is used specifically to the identification of the lattice-type, point and space group of phases present within a sample. The addition of chemical/elemental information from XEDS or EELS spectra to the diffraction data usually allows unique identification of a phase.


Author(s):  
Weiping Liu ◽  
Jennifer Fung ◽  
W.J. de Ruijter ◽  
Hans Chen ◽  
John W. Sedat ◽  
...  

Electron tomography is a technique where many projections of an object are collected from the transmission electron microscope (TEM), and are then used to reconstruct the object in its entirety, allowing internal structure to be viewed. As vital as is the 3-D structural information and with no other 3-D imaging technique to compete in its resolution range, electron tomography of amorphous structures has been exercised only sporadically over the last ten years. Its general lack of popularity can be attributed to the tediousness of the entire process starting from the data collection, image processing for reconstruction, and extending to the 3-D image analysis. We have been investing effort to automate all aspects of electron tomography. Our systems of data collection and tomographic image processing will be briefly described.To date, we have developed a second generation automated data collection system based on an SGI workstation (Fig. 1) (The previous version used a micro VAX). The computer takes full control of the microscope operations with its graphical menu driven environment. This is made possible by the direct digital recording of images using the CCD camera.


Author(s):  
Jan-Olov Bovin ◽  
Osamu Terasaki ◽  
Jan-Olle Malm ◽  
Sven Lidin ◽  
Sten Andersson

High resolution transmission electron microscopy (HRTEM) is playing an important role in identifying the new icosahedral phases. The selected area diffraction patterns of quasi crystals, recorded with an aperture of the radius of many thousands of Ångströms, consist of dense arrays of well defined sharp spots with five fold dilatation symmetry which makes the interpretation of the diffraction process and the resulting images different from those invoked for usual crystals. The atomic structure of the quasi crystals is not established even if several models are proposed. The correct structure model must of course explain the electron diffraction patterns with 5-, 3- and 2-fold symmetry for the phases but it is also important that the HRTEM images of the alloys match the computer simulated images from the model. We have studied quasi crystals of the alloy Al65Cu20Fe15. The electron microscopes used to obtain high resolution electro micrographs and electron diffraction patterns (EDP) were a (S)TEM JEM-2000FX equipped with EDS and PEELS showing a structural resolution of 2.7 Å and a IVEM JEM-4000EX with a UHP40 high resolution pole piece operated at 400 kV and with a structural resolution of 1.6 Å. This microscope is used with a Gatan 622 TV system with an image intensifier, coupled to a YAG screen. It was found that the crystals of the quasi crystalline materials here investigated were more sensitive to beam damage using 400 kV as electron accelerating voltage than when using 200 kV. Low dose techniques were therefore applied to avoid damage of the structure.


Minerals ◽  
2019 ◽  
Vol 9 (4) ◽  
pp. 206 ◽  
Author(s):  
James Hower ◽  
Dali Qian ◽  
Nicolas Briot ◽  
Eduardo Santillan-Jimenez ◽  
Madison Hood ◽  
...  

Fly ash from the combustion of eastern Kentucky Fire Clay coal in a southeastern United States pulverized-coal power plant was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). TEM combined with elemental analysis via energy dispersive X-ray spectroscopy (EDS) showed that rare earth elements (REE; specifically, La, Ce, Nd, Pr, and Sm) were distributed within glassy particles. In certain cases, the REE were accompanied by phosphorous, suggesting a monazite or similar mineral form. However, the electron diffraction patterns of apparent phosphate minerals were not definitive, and P-lean regions of the glass consisted of amorphous phases. Therefore, the distribution of the REE in the fly ash seemed to be in the form of TEM-visible nano-scale crystalline minerals, with additional distributions corresponding to overlapping ultra-fine minerals and even true atomic dispersion within the fly ash glass.


1998 ◽  
Vol 4 (S2) ◽  
pp. 340-341
Author(s):  
Z.L. Wang ◽  
Chen Zhang

Quantitative analysis of structural information provided by transmission electron diffraction and imaging strongly relies on computer simulations. An important quantity in dynamic calculation is the “absorption” potential. The absorption here actually means that the electron is not absorbed by the specimen rather it is scattered out of the elastic state (or Bragg peaks) due to energy-loss and momentum transfer, resulting in a decrease in the intensity of the elastic wave. This is the effect of inelastic scattering (or diffuse scattering) on the Bragg reflected waves [1]. Almost all of the model calculations for the absorption potential have been based on the approximation o riginally introduced by Y o sh ioka, in which the Green's function is approximated by its form in free-space. Thus, the absorption potential is simplified into a non-local function that depends only on the nature of the inelastic scattering.


1989 ◽  
Vol 160 ◽  
Author(s):  
W. T. Pike

AbstractUsing the nanometer probe available in the dedicated scanning transmission electron microscope (STEM) local structural information can be obtained from individual layers in [100] grown Si-Si1-xGex multilayer structures. Furthermore the small probe size enables cleaved specimens with their very large wedge angles to be analyzed in cross-section. Diffraction patterns are shown from multilayers of varying periodicity. Analysis of the patterns concentrates on the higher order Laue zone (holz) reflections in the high angle excess ring . The behaviour of the excess holz reflections indicates the transition from a strained layer superiattice to a dislocated structure as the thickness of the layers increases for a given composition.


2009 ◽  
Vol 43 (1) ◽  
pp. 140-150 ◽  
Author(s):  
K. Z. Baba-Kishi ◽  
M. Pasciak

Incommensurate satellite reflections modulating along the 〈110〉* directions have been observed in the electron diffraction patterns of single crystals of the relaxor ferroelectric Pb2ScTaO6(PST) recordedviatransmission electron microscopy. The satellites occur characteristically within a specific temperature range and display differing or variable modulation vectors relative to their primary reflections. The satellites represent a weak frustrated antiferroelectric state in PST, termed the incommensurate antiferroelectric (IAFE) state. The observed IAFE state coexists with the ferroelectric and paraelectric states within a specific temperature regime and is dynamic in nature, meaning that the dispositions of the satellites can be altered by varying the temperature applied to the crystal,in-situin the transmission electron microscope. The observed satellites are associated with thin, needle-shaped, closely packed striated domains of about 5–15 nm in width. The satellites appear exclusively in crystals of PST with an advanced degree of 1:1 chemical long-range order, exceeding 90%. The satellites and their domains are interpreted as originating from a displacive, antiferroelectric coupling of the ions, driven in particular by the Pb ions. The Monte Carlo (MC) method was used exhaustively to evaluate the structural regimes that lead to the occurrence of the IAFE state. In the MC simulations, the displacements were correlated with the ferroelectric and antiferroelectric couplings, resulting in the IAFE domains and their associated satellites of differing dispositions or modulation vectors. The results of the MC simulations agree well with the electron diffraction observations, supporting the model of an antiferroelectric displacement with an incommensurate modulation of the Pb ions in the 〈110〉* directions.


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