TEM diffraction investigations of amorphous materials

Author(s):  
A. R. Pelton

Transmission electron microscopy has proven invaluable for studies of amorphous materials. The combination of imaging, diffraction and chemical analysis is particularily important for investigations of small volumes of mixed crystalline and amorphous alloys. Several articles have been published recently that describe imaging and EDS of metastable alloys [1-3]. The purpose of this paper is to outline the use of electron diffraction techniques to obtain both qualitative and quantitative structural information from non-crystalline materials.The SADPs in Fig.1 were taken from a study of rapidly-solidified Ti-Zr-Be metallic glasses [4,5]. Initial investigations of these alloys reported apparent evidence from calorimetry and TEM for amorphous phase separation [4]. The images from that study were characteristic of crystalline alloys that undergo spinodal decomposition. However, more recent investigations of the same alloys were able to show conclusively that the “amorphous spinodal” microstructures were actually due to thin-foil artifacts [5].

Author(s):  
D. C. Joy ◽  
D. M. Maher

An accurate knowledge of the specimen foil thickness often is required in quantitative transmission electron microscopy. The methods used for thickness determinations of thin crystalline materials (e.g. the trace method, thickness fringe counts and stereoscopic measurements) generally are selected according to the history of the specimen and nature of the microstructure. For amorphous materials a measurement of the relative transmission of electrons I/I0, where I is the transmitted and I0 the incident electron intensity, affords an accurate estimate of the specimen thickness. In this case, for a sufficiently large specimen thickness, I/I0 varies exponentially according to the mass thickness relationship e-μt, where μ is the mass absorption coefficient and t is the specimen thickness. The purpose of this paper is to demonstrate that the thickness of a crystalline specimen also may be determined accurately from a measurement of I/I0, provided that well defined diffracting conditions are used. The results presented here are for silicon.


2005 ◽  
Vol 11 (5) ◽  
pp. 378-400 ◽  
Author(s):  
Christian Kübel ◽  
Andreas Voigt ◽  
Remco Schoenmakers ◽  
Max Otten ◽  
David Su ◽  
...  

Electron tomography is a well-established technique for three-dimensional structure determination of (almost) amorphous specimens in life sciences applications. With the recent advances in nanotechnology and the semiconductor industry, there is also an increasing need for high-resolution three-dimensional (3D) structural information in physical sciences. In this article, we evaluate the capabilities and limitations of transmission electron microscopy (TEM) and high-angle-annular-dark-field scanning transmission electron microscopy (HAADF-STEM) tomography for the 3D structural characterization of partially crystalline to highly crystalline materials. Our analysis of catalysts, a hydrogen storage material, and different semiconductor devices shows that features with a diameter as small as 1–2 nm can be resolved in three dimensions by electron tomography. For partially crystalline materials with small single crystalline domains, bright-field TEM tomography provides reliable 3D structural information. HAADF-STEM tomography is more versatile and can also be used for high-resolution 3D imaging of highly crystalline materials such as semiconductor devices.


1986 ◽  
Vol 82 ◽  
Author(s):  
D.W. Susnitzky ◽  
C.B. Carter

ABSTRACTSurfaces of crystalline materials generally facet and form steps and ledges on low-index planes to reduce their total energy. A conventional wedge-shaped transmission electron microscope (TEM) thin foil, prepared slightly misoriented with respect to a low-index plane, provides a suitable geometry for the study of surface ledges, steps and facets. This TEM study characterizes the surface features of annealed thin foils prepared from various oxides with a range of nominally low-index orientations. Observations from single-crystal α-A12O3 and MgAl2O4 (spinel) will be included.The steps and facets typically form along energetically favorable, low-index planes and bound terraces of low-index orientation. The structure of these features are discussed. In addition, surface step movement has been observed and monitored through a series of reannealing experiments on the same foil.


1993 ◽  
Vol 8 (7) ◽  
pp. 1728-1735
Author(s):  
H. Maghsoudlou ◽  
L. Salamanca-Riba ◽  
E. Haro-Poniatowski

GeSe2 can exist in both amorphous and crystalline phases. Although most semiconductor devices are constructed from crystalline materials, the use of amorphous materials in devices has high potential. The study of GeSe2 is especially interesting since it has been established that an amorphous-to-crystalline transition can be induced by laser irradiation. In order to better understand this phenomenon, it is necessary to study the microstructure of GeSe2 glass. Therefore, transmission electron microscopy studies were undertaken to investigate the degree of crystallinity of GeSe2 glass. It was found that small microcrystallites with diameters in the range of 100–300 Å were embedded in a glass matrix. These microcrystallites formed larger clusters in some areas.


Author(s):  
A.R. Pelton ◽  
A.F. Marshall ◽  
Y.S. Lee

Amorphous materials are of current interest due to their desirable mechanical, electrical and magnetic properties. Furthermore, crystallizing amorphous alloys provides an avenue for discerning sequential and competitive phases thus allowing access to otherwise inaccessible crystalline structures. Previous studies have shown the benefits of using AEM to determine crystal structures and compositions of partially crystallized alloys. The present paper will discuss the AEM characterization of crystallized Cu-Ti and Ni-Ti amorphous films.Cu60Ti40: The amorphous alloy Cu60Ti40, when continuously heated, forms a simple intermediate, macrocrystalline phase which then transforms to the ordered, equilibrium Cu3Ti2 phase. However, contrary to what one would expect from kinetic considerations, isothermal annealing below the isochronal crystallization temperature results in direct nucleation and growth of Cu3Ti2 from the amorphous matrix.


Author(s):  
T. E. Mitchell ◽  
R. B. Schwarz

Traditional oxide glasses occur naturally as obsidian and can be made easily by suitable cooling histories. In the past 30 years, a variety of techniques have been discovered which amorphize normally crystalline materials such as metals. These include [1-3]:Rapid quenching from the vapor phase.Rapid quenching from the liquid phase.Electrodeposition of certain alloys, e.g. Fe-P.Oxidation of crystals to produce amorphous surface oxide layers.Interdiffusion of two pure crystalline metals.Hydrogen-induced vitrification of an intermetal1ic.Mechanical alloying and ball-milling of intermetal lie compounds.Irradiation processes of all kinds using ions, electrons, neutrons, and fission products.We offer here some general comments on the use of TEM to study these materials and give some particular examples of such studies.Thin specimens can be prepared from bulk homogeneous materials in the usual way. Most often, however, amorphous materials are in the form of surface films or interfacial films with different chemistry from the substrates.


Author(s):  
A. Zangvil ◽  
L.J. Gauckler ◽  
G. Schneider ◽  
M. Rühle

The use of high temperature special ceramics which are usually complex materials based on oxides, nitrides, carbides and borides of silicon and aluminum, is critically dependent on their thermomechanical and other physical properties. The investigations of the phase diagrams, crystal structures and microstructural features are essential for better understanding of the macro-properties. Phase diagrams and crystal structures have been studied mainly by X-ray diffraction (XRD). Transmission electron microscopy (TEM) has contributed to this field to a very limited extent; it has been used more extensively in the study of microstructure, phase transformations and lattice defects. Often only TEM can give solutions to numerous problems in the above fields, since the various phases exist in extremely fine grains and subgrain structures; single crystals of appreciable size are often not available. Examples with some of our experimental results from two multicomponent systems are presented here. The standard ion thinning technique was used for the preparation of thin foil samples, which were then investigated with JEOL 200A and Siemens ELMISKOP 102 (for the lattice resolution work) electron microscopes.


Author(s):  
H. Koike ◽  
T. Matsuo ◽  
K. Ueno ◽  
M. Suzuki

Since the identification of single atoms was achieved by Crewe et al, scanning transmission microscopy has been put into pratical use. Recently they applied this method to the quantitative mass analysis of DNA.As pointed out previously the chromatic aberration which decreases the image contrast and quality, does not affect a scanning transmission image as it does a conventional transmission electron microscope image. Thus, the STEM method is advantageous for thick specimen. Further this method employs a high sensitive photomultiplier tube which also functions as an image intensifier. This detection method is effective for the observation of living specimens or easily damaged specimens. In this respect the scanning transmission microscope with high accelerating voltage is necessary.Since Uyeda's experiments of crystalline materials, many workers have been discussed how thick specimens can be observed by CTEM. With biological specimens, R. Szirmae reported on the decrease in the image contrast of rabbit psoas muscle sections at various accelerating voltages and specimen thicknesses.


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):  
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)]|.


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