In-Situ Ion Milling in the Transmission Electron Microscope (TEM) Outlook to a New Preparation Technique

2001 ◽  
Vol 7 (S2) ◽  
pp. 932-933
Author(s):  
Peter Gnauck ◽  
Claus Burkhardt ◽  
Erich Plies ◽  
Wilfried Nisch

Recent developments in transmission electron microscopy put high demands on specimen preparation. in general the imaging quality is not limited by the performance of the microscope but by the quality of the specimen. in order to achieve a spatial resolution of 0.1 nm in HRTEM undamaged samples with a thickness below 10 nm are required. in energy filtering analytical electron microscopy (EFTEM), a constant specimen thickness over large areas and very low contamination is needed.Conventional ion-milling techniques for TEM specimen preparation are essentially blind. Thus, it is left to chance whether the specimen detail of interest is suitable for TEM-imaging (many specimen areas are too thick). Another problem is the reaction of the specimen with the atmosphere during the transfer from the preparation stage to the microscope, which makes it very difficult to obtain the clean specimen surfaces that are needed in analytical EFTEM. Especially in high-resolution electron microscopy and electron holography the formation of amorphous oxidation and contamination layers on otherwise crystalline materials may seriously reduce the quality of high resolution images of the crystal structure.

1998 ◽  
Vol 523 ◽  
Author(s):  
John Mardinly ◽  
David W. Susnitzky

AbstractThe demand for increasingly higher performance semiconductor products has stimulated the semiconductor industry to respond by producing devices with increasingly complex circuitry, more transistors in less space, more layers of metal, dielectric and interconnects, more interfaces, and a manufacturing process with nearly 1,000 steps. As all device features are shrunk in the quest for higher performance, the role of Transmission Electron Microscopy as a characterization tool takes on a continually increasing importance over older, lower-resolution characterization tools, such as SEM. The Ångstrom scale imaging resolution and nanometer scale chemical analysis and diffraction resolution provided by modem TEM's are particularly well suited for solving materials problems encountered during research, development, production engineering, reliability testing, and failure analysis. A critical enabling technology for the application of TEM to semiconductor based products as the feature size shrinks below a quarter micron is advances in specimen preparation. The traditional 1,000Å thick specimen will be unsatisfactory in a growing number of applications. It can be shown using a simple geometrical model, that the thickness of TEM specimens must shrink as the square root of the feature size reduction. Moreover, the center-targeting of these specimens must improve so that the centertargeting error shrinks linearly with the feature size reduction. To meet these challenges, control of the specimen preparation process will require a new generation of polishing and ion milling tools that make use of high resolution imaging to control the ion milling process. In addition, as the TEM specimen thickness shrinks, the thickness of surface amorphization produced must also be reduced. Gallium focused ion beam systems can produce hundreds of Ångstroms of amorphised surface silicon, an amount which can consume an entire thin specimen. This limitation to FIB milling requires a method of removal of amorphised material that leaves no artifact in the remaining material.


2017 ◽  
Vol 46 (1) ◽  
pp. 47-61 ◽  
Author(s):  
Uschi M. Graham ◽  
Robert A. Yokel ◽  
Alan K. Dozier ◽  
Lawrence Drummy ◽  
Krishnamurthy Mahalingam ◽  
...  

This is the first utilization of advanced analytical electron microscopy methods, including high-resolution transmission electron microscopy, high-angle annular dark field scanning transmission electron microscopy, electron energy loss spectroscopy, and energy-dispersive X-ray spectroscopy mapping to characterize the organ-specific bioprocessing of a relatively inert nanomaterial (nanoceria). Liver and spleen samples from rats given a single intravenous infusion of nanoceria were obtained after prolonged (90 days) in vivo exposure. These advanced analytical electron microscopy methods were applied to elucidate the organ-specific cellular and subcellular fate of nanoceria after its uptake. Nanoceria is bioprocessed differently in the spleen than in the liver.


1999 ◽  
Vol 571 ◽  
Author(s):  
N. D. Zakharov ◽  
P. Werner ◽  
V. M. Ustinov ◽  
A.R. Kovsh ◽  
G. E. Cirlin ◽  
...  

ABSTRACTQuantum dot structures containing 2 and 7 layers of small coherent InAs clusters embedded into a Si single crystal matrix were grown by MBE. The structure of these clusters was investigated by high resolution transmission electron microscopy. The crystallographic quality of the structure severely depends on the substrate temperature, growth sequence, and the geometrical parameters of the sample. The investigation demonstrates that Si can incorporate a limited volume of InAs in a form of small coherent clusters about 3 nm in diameter. If the deposited InAs layer exceeds a critical thickness, large dislocated InAs precipitates are formed during Si overgrowth accumulating the excess of InAs.


Author(s):  
K. Fortunati ◽  
M. Fendorf ◽  
M. Powers ◽  
C.P. Burmester ◽  
R. Gronsky

Transmission electron microscopy, in particular high-resolution TEM, is proving to be a valuable tool in the continuing effort to characterize and understand the “high-Tc” superconducting oxides. Since specimen quality is of critical importance in high-resolution studies, care must be taken to choose the most appropriate specimen preparation technique for the material under study. The BiCaSrCuO material investigated here was in the form of small, sintered pellets with a porous microstructure which consists of small, randomly oriented, poorly connected, plate-like grains (see Figure 1). We have found that this morphology can significantly effect the production of suitable TEM specimens.The simplest and most rapid specimen preparation method employed consists of crushing a small amount of the starting material to a fine powder in an agate mortar and suspending the powder in pure ethanol or propanol. An eye dropper or syringe is then used to transfer 4-6 drops of the suspension onto a holey carbon film supported on a mesh grid, thus effectively dispersing the powder across the grid. A strong tendency for the crystal to cleave along (001) planes, due to the weak bonding between BiO layers, results in flake-like particles which exhibit a preferred [001] orientation on the grid. A high-resolution image of a specimen prepared using this method is shown in Figure 2. We have observed that some specimens produced in this manner are unstable under a 200kV beam (with LaB6 filament), with heavy damage occurring within the time that a through-focus series of micrographs can be exposed. It is also important to note that since separation along grain boundaries occurs during crushing, this method is not an appropriate choice for imaging grain boundary structures.


2013 ◽  
Vol 774-776 ◽  
pp. 799-802
Author(s):  
Zhong Yuan Liu ◽  
J. Tan ◽  
G. Wang

In this paper, high resolution transmission electron microscopy (HRTEM) has been used to observe a Zr41.25Ti13.75Ni10Cu12.5Be22.5 (at. %) bulk metallic glass (BMG) prepared from different methods, i.e. ion milling and electropolishing. The ion thinning brings out the white bulb pattern on the specimen surface and induces localized temperature increasing. The electropolishing does not influence microstructure of the amorphous phase. A new preparation technique of grinding method is introduced. For BMG, the electropolishing and grinding are the better method for TEM specimen preparation as compared with the ion thinning.


Author(s):  
K. J. Morrissey

Grain boundaries and interfaces play an important role in determining both physical and mechanical properties of polycrystalline materials. To understand how the structure of interfaces can be controlled to optimize properties, it is necessary to understand and be able to predict their crystal chemistry. Transmission electron microscopy (TEM), analytical electron microscopy (AEM,), and high resolution electron microscopy (HREM) are essential tools for the characterization of the different types of interfaces which exist in ceramic systems. The purpose of this paper is to illustrate some specific areas in which understanding interface structure is important. Interfaces in sintered bodies, materials produced through phase transformation and electronic packaging are discussed.


Author(s):  
Jan-Olle Malm ◽  
Jan-Olov Bovin

Understanding of catalytic processes requires detailed knowledge of the catalyst. As heterogeneous catalysis is a surface phenomena the understanding of the atomic surface structure of both the active material and the support material is of utmost importance. This work is a high resolution electron microscopy (HREM) study of different phases found in a used automobile catalytic converter.The high resolution micrographs were obtained with a JEM-4000EX working with a structural resolution better than 0.17 nm and equipped with a Gatan 622 TV-camera with an image intensifier. Some work (e.g. EDS-analysis and diffraction) was done with a JEM-2000FX equipped with a Link AN10000 EDX spectrometer. The catalytic converter in this study has been used under normal driving conditions for several years and has also been poisoned by using leaded fuel. To prepare the sample, parts of the monolith were crushed, dispersed in methanol and a drop of the dispersion was placed on the holey carbon grid.


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