An Automated Jet Polishing Technique for Preparation of Transmission Electron Microscope Specimens for In-Situ Straining

1987 ◽  
Vol 115 ◽  
Author(s):  
W. A. T. Clark ◽  
B. Hardiman ◽  
R. H. Wagoner
Keyword(s):  
Video Recording ◽  
Recording Equipment ◽  
Specimen Holder ◽  
Transmission Electron ◽  
Gauge Section ◽  
Dynamic Experiments ◽  
Teflon Sheet ◽  
Specific Shape ◽  
Electron Microscopes

ABSTRACTThe increasing availability of intermediate and high voltage transmission electron microscopes, together with recent improvements in video recording equipment, have led to renewed interest in in situ dynamic experiments. To alleviate the problems encountered in preparing TEM specimens with the awkward geometries required for straining stages, a jet polishing technique has been developed which allows the use of a conventional twin-jet electropolishing unit, with all its attendant advantages. A pair of Teflon sheet inserts, with rectangular openings cut to a specific shape and size, are used in the conventional specimen holder. Specimens with elliptical holes close to the center of the gauge section, and with large electron transparent areas at both ends of the long axis, are produced routinely and rapidly. Samples of many annealed metals, such as brass, molybdenum, and aluminum, prepared by this method are stronger, and can be handled more easily, than those prepared by conventional methods.

Materials Science in the Electron Microscope

MRS Bulletin ◽  
1994 ◽  
Vol 19 (6) ◽  
pp. 17-21 ◽  
Author(s):  
Frances M. Ross
Keyword(s):  
Electron Microscopy ◽  
Electron Microscope ◽  
Real Time ◽  
Materials Science ◽  
Foil Thickness ◽  
Specimen Holder ◽  
Transmission Electron ◽  
Dynamic Experiments ◽  
Electron Microscopes

This issue of the MRS Bulletin aims to highlight the innovative and exciting materials science research now being done using in situ electron microscopy. Techniques which combine real-time image acquisition with high spatial resolution have contributed to our understanding of a remarkably diverse range of physical phenomena. The articles in this issue present recent advances in materials science which have been made using the techniques of transmission electron microscopy (TEM), including holography, scanning electron microscopy (SEM), low-energy electron microscopy (LEEM), and high-voltage electron microscopy (HVEM).The idea of carrying out dynamic experiments involving real-time observation of microscopic phenomena has always had an attraction for materials scientists. Ever since the first static images were obtained in the electron microscope, materials scientists have been interested in observing processes in real time: we feel that we obtain a true understanding of a microscopic phenomenon if we can actually watch it taking place. The idea behind “materials science in the electron microscope” is therefore to use the electron microscope—with its unique ability to image subtle changes in a material at or near the atomic level—as a laboratory in which a remarkable variety of experiments can be carried out. In this issue you will read about dynamic experiments in areas such as phase transformations, thin-film growth, and electromigration, which make use of innovative designs for the specimen, the specimen holder, or the microscope itself. These articles speak for themselves in demonstrating the power of real-time analysis in the quantitative exploration of reaction mechanisms.The first transmission electron microscopes operated at low accelerating voltages, up to about 100 kV. This placed a severe limitation on the thickness of foils that could be examined: Heavy elements, for example, had to be made into foils thinner than 0.1 μm. It was felt that any phenomenon whose “mean free path” was comparable to the foil thickness would be significantly affected by the foil surfaces, and therefore would be unsuitable for study in situ. However, technology quickly generated ever higher accelerating voltages, culminating in the giant 3 MeV electron microscopes. At these voltages, electrons can penetrate materials as thick as 6–9 μm for light elements such as Si and Al, and 1 μm for very heavy ones such as Au and U.

Remote On-Line Control of a High-Voltage in situ Transmission Electron Microscope with A Rational User Interface

1996 ◽  
Vol 54 ◽  
pp. 384-385
Author(s):  
M.A. O’Keefe ◽  
J. Taylor ◽  
D. Owen ◽  
B. Crowley ◽  
K.H. Westmacott ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Electron Microscope ◽  
User Interface ◽  
Transmission Electron Microscope ◽  
High Voltage ◽  
Materials Science ◽  
Transmission Electron ◽  
On Line ◽  
Electron Microscopes

Remote on-line electron microscopy is rapidly becoming more available as improvements continue to be developed in the software and hardware of interfaces and networks. Scanning electron microscopes have been driven remotely across both wide and local area networks. Initial implementations with transmission electron microscopes have targeted unique facilities like an advanced analytical electron microscope, a biological 3-D IVEM and a HVEM capable of in situ materials science applications. As implementations of on-line transmission electron microscopy become more widespread, it is essential that suitable standards be developed and followed. Two such standards have been proposed for a high-level protocol language for on-line access, and we have proposed a rational graphical user interface. The user interface we present here is based on experience gained with a full-function materials science application providing users of the National Center for Electron Microscopy with remote on-line access to a 1.5MeV Kratos EM-1500 in situ high-voltage transmission electron microscope via existing wide area networks. We have developed and implemented, and are continuing to refine, a set of tools, protocols, and interfaces to run the Kratos EM-1500 on-line for collaborative research. Computer tools for capturing and manipulating real-time video signals are integrated into a standardized user interface that may be used for remote access to any transmission electron microscope equipped with a suitable control computer.

In-Situ Electrochemical Transmission Electron Microscopy for Battery Research

2014 ◽  
Vol 20 (2) ◽  
pp. 484-492 ◽  
Author(s):  
B. Layla Mehdi ◽  
Meng Gu ◽  
Lucas R. Parent ◽  
Wu Xu ◽  
Eduard N. Nasybulin ◽  
...  
Keyword(s):  
Electron Beam ◽  
Silicon Nanowires ◽  
Electrochemical Processes ◽  
Transmission Electron ◽  
Experimental Parameters ◽  
Scanning Transmission ◽  
Electrode Interface ◽  
Electron Microscopes

AbstractThe recent development of in-situ liquid stages for (scanning) transmission electron microscopes now makes it possible for us to study the details of electrochemical processes under operando conditions. As electrochemical processes are complex, care must be taken to calibrate the system before any in-situ/operando observations. In addition, as the electron beam can cause effects that look similar to electrochemical processes at the electrolyte/electrode interface, an understanding of the role of the electron beam in modifying the operando observations must also be understood. In this paper we describe the design, assembly, and operation of an in-situ electrochemical cell, paying particular attention to the method for controlling and quantifying the experimental parameters. The use of this system is then demonstrated for the lithiation/delithiation of silicon nanowires.

scholarly journals Computer-Controlled Polishing System For Preparing Multiple Pre-FIB TEM Specimens

2007 ◽  
Vol 15 (6) ◽  
pp. 38-39
Author(s):  
D. J. MacMahon ◽  
E. Raz-Moyal
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Product Yield ◽  
Interface Layer ◽  
Ex Situ ◽  
Advantages And Disadvantages ◽  
Transmission Electron ◽  
Invaluable Tool ◽  
Electron Microscopes

Semiconductor manufacturers are increasingly turning to Transmission Electron Microscopes (TEMs) to monitor product yield and process control, analyze defects, and investigate interface layer morphology. To prepare TEM specimens, Focused Ion Beam (FIB) technology is an invaluable tool, yielding a standard milled TEM lamella approximately 15 μm wide, 5 μm deep and ~100 nm thick. Several techniques have been developed to extract these tiny objects from a large wafer and view it in the TEM. These techniques, including ex-situ lift-out, H-bar, and in-situ lift-out, have different advantages and disadvantages, but all require painstaking preparation of one specimen at a time.

In-Situ High Resolution Transmission Electron Microscopy of Dynamic Events During the Amorphous to Crystalline Phase Transformation in Silicon

1985 ◽  
Vol 62 ◽  
Author(s):  
M. A. Parker ◽  
T. W. Sigmon ◽  
R. Sinclair
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Phase Transformation ◽  
Solid State ◽  
High Resolution ◽  
Elevated Temperatures ◽  
Video Recording ◽  
Dynamic Events ◽  
Transmission Electron

ABSTRACTA technique has been developed which employs high resolution transmission electron microscopy (HRTEM) for the observation of the atomic mechanisms associated with solid state phase transformation as they occur at elevated temperatures. It consists of the annealing in-situ of cross-section transmission electron microscopy (TEM) specimens that have been favorably oriented for lattice fringe imaging and the video-recording of dynamic events as they occur in real-time. By means of this technique, we report the first video-recorded lattice images of crystallographic defect motion in silicon, viz. the motion of dislocations and stacking faults, as well as the first such images of the atomic mechanisms responsible for the amorphous to crystalline (a-c) phase transformation, viz. heterogeneous nucleation of crystal nuclei, coalescence of crystal nuclei by co-operative atomic processes, ledge motion at the growth interface, and normal growth in silicon. This technique holds great potential for the elucidation of the atomic mechanisms involved in reaction kinetics in the solid state.

Scanning Electron Microscope Facility for in situ Observations of Ion Implanted Surfaces

1975 ◽  
Vol 33 ◽  
pp. 262-263
Author(s):  
G. J. Thomas ◽  
W. Bauer
Keyword(s):  
Surface Deformation ◽  
Video Recording ◽  
Dose Dependence ◽  
Quantitative Information ◽  
High Dose ◽  
Recording Equipment ◽  
Cold Worked ◽  
Dose Levels ◽  
Scanning Electron

In previous studies of high dose He implantation of metals, observations of the resulting surface deformation were made after specific dose levels were attained. The present work describes a recently constructed system which allows scanning electron microscopy observation during implantation. A number of advantages can be gained by this approach. First, considerably more data can be obtained on a given sample so that, for example, the precise dose dependence of surface deformation can be determined. The technique also allows direct observation of deformation either above or below room temperature andin addition, quantitative information on the rates of blister formation and growth can be obtained. The rapidity with which surface features develop during implantation requires continuous and rapid storage of the sample image. Commercially available video recording equipment, with appropriate modification, has been used for this purpose.In preliminary studies, a comparison has been made of surface deformation due to He implantation of a hydride (TiH2), annealed Ti metal, and cold worked Ti.

In situ high-resolution Transmission electron microscopy of interphase boundary motion in metallic alloys

1991 ◽  
Vol 49 ◽  
pp. 450-451
Author(s):  
James M. Howe
Keyword(s):  
High Resolution ◽  
Interphase Boundary ◽  
Image Intensifier ◽  
Metallic Alloys ◽  
Video Cassette Recorder ◽  
Cold Stage ◽  
Transmission Electron ◽  
Electron Microscopes ◽  
Initial Results

Information provided by in situ studies is often essential for understanding microstructural evolution in solids. The recent development of intermediate-voltage high-resolution transmission electron microscopes (HRTEM) with in situ heating capabilities now provides the opportunity to perform in situ high-resolution studies of interphase boundary (IPB) motion. This paper presents initial results on in situ HRTEM studies of IPB motion in metallic alloys, in particular, during growth of Q precipitates in an Al-Cu-Mg-Ag alloy and Pd3Si crystals in an amorphous Pd-Si alloy.Samples of an Al-4Cu-0.5Mg-0.5Ag (wt.%) alloy were aged for 24 hr at 250°C and electropolished in a HNO3/methanol solution; samples of an amorphous Pd80Si20 (at.%) ribbon were ion milled in a liquid-nitrogen cold-stage at 6 kV, 0.3 mA and 15° tilt. The samples were examined at 400 kV in a JEOL 4000EX microscope equipped with a UHP40X hot-stage pole piece and double-tilt holder at temperatures of 200-400°C. Images were recorded on a Sony BetaCam video cassette recorder connected to a Gatan fiber-optically coupled TV camera with an image intensifier. A 35 mm camera was used to obtain photographs directly from the TV monitor during playback of the video cassettes.

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