Replica Extraction Method on Nanostructured Gold Coatings and Orientation Determination Combining SEM and TEM Techniques

2014 ◽  
Vol 20 (6) ◽  
pp. 1654-1661 ◽  
Author(s):  
Christian Bocker ◽  
Michael Kracker ◽  
Christian Rüssel

AbstractIn the field of electron microscopy the replica technique is known as an indirect method and also as an extraction method that is usually applied on metallurgical samples. This contribution describes a fast and simple transmission electron microscopic (TEM) sample preparation by complete removal of nanoparticles from a substrate surface that allows the study of growth mechanisms of nanostructured coatings. The comparison and combination of advanced diffraction techniques in the TEM and scanning electron microscopy (SEM) provide possibilities for operators with access to both facilities. The analysis of TEM-derived diffraction patterns (convergent beam electron diffraction) in the SEM/electron backscatter diffraction software simplifies the application, especially when the patterns are not aligned along a distinct zone axis. The study of the TEM sample directly by SEM and transmission Kikuchi diffraction allows cross-correlation with the TEM results.

1993 ◽  
Vol 8 (6) ◽  
pp. 1373-1378 ◽  
Author(s):  
A. Catana ◽  
J-P. Locquet

Dy2O3 layers have been grown on SrTiO3 by molecular beam epitaxy. X-ray and electron diffraction patterns clearly show that Dy2O3 grows epitaxially on SrTiO3 with {100} planes parallel to the substrate surface. Transmission electron microscopy reveals that the Dy2O3 film breaks up into small domains (10–40 nm). This leads to the formation of terraces which limits the structural perfection of thin overgrown DyBa2Cu3O7 by introducing steps and small misorientations (within 3°). The resulting surface corrugation does not preclude the growth of epitaxial c-axis DyBa2Cu3O7 films with a Tc0 of 86 K. Crystallographic analysis and image calculations show that the domain growth of Dy2O3 is associated with the formation of 90° rotation twins.


2014 ◽  
Vol 20 (6) ◽  
pp. 1805-1816 ◽  
Author(s):  
Bryan R. Bandli ◽  
Mickey E. Gunter

AbstractSince 1972, when the US Occupational Health and Safety Administration established the first limits on occupational exposure to asbestos fibers, numerous analytical methods employing several microscopy techniques have been developed to identify a group of minerals defined by legislation as asbestos. While transmission electron microscopy (TEM) is implemented in standardized analytical methods, these methods specify the use of selected area electron diffraction. Because of this constraint, the diffraction data a TEM can provide are often underutilized due to challenges associated with collecting and interpreting individual diffraction patterns. It has been shown that transmission electron backscatter diffraction (tEBSD) produces diffraction patterns nearly identical to electron backscatter diffraction, but from smaller crystal domains. This paper explores the utility of tEBSD for characterization of asbestiform particles from reference asbestos materials, a suite of amphibole minerals of varying morphologies to determine if there is a correlation between mineral habit (i.e., crystal form), microscopic particle shape preferred orientation, and mineral specimens from an industrial talc deposit to provide a case study of the utility and limitations of the technique.


Author(s):  
Loren Anderson ◽  
Pat Pizzo ◽  
Glen Haydon

Transmission electron microscopy of replicas has long been used to study the fracture surfaces of components which fail in service. Recently, the scanning electron microscope (SEM) has gained popularity because it allows direct examination of the fracture surface. However, the somewhat lower resolution of the SEM coupled with a restriction on the sample size has served to limit the use of this instrument in investigating in-service failures. It is the intent of this paper to show that scanning electron microscopic examination of conventional negative replicas can be a convenient and reliable technique for determining mode of failure.


Author(s):  
C. N. Gordon

Gordon and Kleinschmidt have described a new preparative technique for visualizing DNA by electron microscopy. This procedure, which is a modification of Hall's “mica substrate technique”, consists of the following steps: (a) K+ ions on the cleavage surface of native mica are exchanged for Al3+ ions by ion exchange. (b) The mica, with Al3+ in the exchange sites on the surface, is placed in a dilute aqueous salt solution of DNA for several minutes; during this period DNA becomes adsorbed on the surface. (c) The mica with adsorbed DNA is removed from the DNA solution, rinsed, dried and visualized for transmission electron microscopy by Hall's platinum pre-shadow replica technique.In previous studies of circular DNA by this technique, most of the molecules seen were either broken to linears or extensively tangled; in general, it was not possible to obtain suitably large samples of open extended molecules for contour length measurements.


Author(s):  
Joseph J. Comer ◽  
Charles Bergeron ◽  
Lester F. Lowe

Using a Van De Graaff Accelerator thinned specimens were subjected to bombardment by 3 MeV N+ ions to fluences ranging from 4x1013 to 2x1016 ions/cm2. They were then examined by transmission electron microscopy and reflection electron diffraction using a 100 KV electron beam.At the lowest fluence of 4x1013 ions/cm2 diffraction patterns of the specimens contained Kikuchi lines which appeared somewhat broader and more diffuse than those obtained on unirradiated material. No damage could be detected by transmission electron microscopy in unannealed specimens. However, Dauphiné twinning was particularly pronounced after heating to 665°C for one hour and cooling to room temperature. The twins, seen in Fig. 1, were often less than .25 μm in size, smaller than those formed in unirradiated material and present in greater number. The results are in agreement with earlier observations on the effect of electron beam damage on Dauphiné twinning.


Author(s):  
Peter K. Mueller ◽  
Glenn R. Smith ◽  
Leslie M Carpenter ◽  
Ronald L. Stanley

At the present time the primary objective of the electron microscopy group of the Air and Industrial Hygiene Laboratory is the development of a method suitable for use in establishing an air quality standard for asbestos in ambient air and for use in its surveillance. The main concept and thrust of our approach for the development of this method is to obtain a true picture of fiber occurrence as a function of particle size and asbestos type utilizing light and electron microscopy.We have now available an electron micrographic atlas of all asbestos types including selected area diffraction patterns and examples of fibers isolated from air samples. Several alternative approaches for measuring asbestos in ambient air have been developed and/or evaluated. Our experiences in this regard will be described. The most promising method involves: 1) taking air samples on cellulose ester membrane filters with a nominal pore size of 0.8 micron; 2) ashing in a low temperature oxygen plasma for several hours;


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):  
Veronika Burmeister ◽  
R. Swaminathan

Porphyria cutanea tarda (PCT) is a disorder of porphyrin metabolism which occurs most often during middle age. The disease is characterized by excessive production of uroporphyrin which causes photosensitivity and skin eruptions on hands and arms, due to minor trauma and exposure to sunlight. The pathology of the blister is well known, being subepidermal with epidermodermal separation, it is not always absolutely clear, whether the basal lamina is attached to the epidermis or the dermis. The purpose of our investigation was to study the attachment of the basement membrane in the blister by comparing scanning with transmission electron microscopy.


Author(s):  
Ryuichiro Oshima ◽  
Shoichiro Honda ◽  
Tetsuo Tanabe

In order to examine the origin of extra diffraction spots and streaks observed in selected area diffraction patterns of deuterium irradiated silicon, systematic diffraction experiments have been carried out by using parallel beam illumination.Disc specimens 3mm in diameter and 0.5mm thick were prepared from a float zone silicon single crystal(B doped, 7kΩm), and were chemically thinned in a mixed solution of nitric acid and hydrogen fluoride to make a small hole at the center for transmission electron microscopy. The pre-thinned samples were irradiated with deuterium ions at temperatures between 300-673K at 20keV to a dose of 1022ions/m2, and induced lattice defects were examined under a JEOL 200CX electron microscope operated at 160kV.No indication of formation of amorphous was obtained in the present experiments. Figure 1 shows an example of defects induced by irradiation at 300K with a dose of 2xl021ions/m2. A large number of defect clusters are seen in the micrograph.


Author(s):  
F. Shaapur

Non-uniform ion-thinning of heterogenous material structures has constituted a fundamental difficulty in preparation of specimens for transmission electron microscopy (TEM). A variety of corrective procedures have been developed and reported for reducing or eliminating the effect. Some of these techniques are applicable to any non-homogeneous material system and others only to unidirectionalfy heterogeneous samples. Recently, a procedure of the latter type has been developed which is mainly based on a new motion profile for the specimen rotation during ion-milling. This motion profile consists of reversing partial revolutions (RPR) within a fixed sector which is centered around a direction perpendicular to the specimen heterogeneity axis. The ion-milling results obtained through this technique, as studied on a number of thin film cross-sectional TEM (XTEM) specimens, have proved to be superior to those produced via other procedures.XTEM specimens from integrated circuit (IC) devices essentially form a complex unidirectional nonhomogeneous structure. The presence of a variety of mostly lateral features at different levels along the substrate surface (consisting of conductors, semiconductors, and insulators) generally cause non-uniform results if ion-thinned conventionally.


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