Instrumentation and Computation

Author(s):  
P.B. Hirsch

The benefit to society arising from developments in instrumentation and computation can be judged primarily by the advances in knowledge and understanding generated by their application in different branches of science, covered in the other papers in this symposium. Without advances in instrumentation none of these advances is possible; developments in instrumentation and in image interpretation are therefore fundamental to and precede scientific advances in fields in which knowledge of structure is important. There is little doubt that the revolutionary first step was the development of the transmission electron microscope (TEM) in 1931 by Ernst Ruska; a second was the development of the scanning electron microscope (SEM); and the third the introduction of the scanning tunnelling microscope (STM) for high resolution surface imaging, by Binnig and Rohrer.The TEM and SEM have undergone continuous developments over the last 50 years or so, and have had a far-reaching impact in a wide range of disciplines; the STM is a relative newcomer but no doubt it too will have an increasing impact in furthering our understanding of solids and surfaces in particular. Once the basic instruments became available subsequent developments have been driven by the demands of the scientific disciplines in which these instruments have been applied. Many of the new developments in instrumentation and interpretation have been pioneered by the users themselves, and these in turn have led to modifications in commercial instruments to make such advances in technique available to the user community as a whole. Other developments have been initiated directly by the manufacturers as a result of a perceived need. There has been and continues to be a close interaction between the developers of hardware (not only of electron microscopes but also of ancillary equipment, e.g. microanalysis attachments, image processing equipment, specialist specimen stages, and specimen preparation facilities) and the users, leading to extensions in the range of applications and the types of information which can be obtained by electron microscopy. The following examples from the developments of electron microscopy in Materials Science illustrate these interactions and the particular advances arising from specific developments:

Author(s):  
M.A. O’Keefe ◽  
J. Taylor ◽  
D. Owen ◽  
B. Crowley ◽  
K.H. Westmacott ◽  
...  

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.


2001 ◽  
Vol 7 (S2) ◽  
pp. 776-777
Author(s):  
John F. Mansfield

The environmental scanning electron microscope (ESEM™) and variable pressure electron microscope (VPSEM) have become accepted tools in the contemporary electron microscopy facility. Their flexibility and their ability to image almost any sample with little, and often no, specimen preparation has proved so attractive that each manufacturer of scanning electron microscopes now markets a low vacuum model.The University of Michigan Electron Microbeam Analysis Laboratory (EMAL) operates two variable pressure instruments, an ElectroScan E3 ESEM and a Hitachi S3200N VPSEM. The E3 ESEM was acquired in the early 1990s with funding from the Amoco Foundation and it has been used to examine an extremely wide variety of different materials. Since EMAL serves the entire university community, and offers support to neighboring institutions and local industry, the types of materials examined span a wide range. There are users from Materials Science & Engineering, Chemical Engineering, Nuclear Engineering, Electrical Engineering, Physics, Chemistry, Geology, Biology, Biophysics, Pharmacy and Pharmacology.


Author(s):  
Edward A. Kenik ◽  
Karren L. More

The Shared Research Equipment (SHaRE) Program provides access to the wide range of advanced equipment and techniques available in the Metals and Ceramics Division of ORNL to researchers from universities, industry, and other national laboratories. All SHaRE projects are collaborative in nature and address materials science problems in areas of mutual interest to the internal and external collaborators. While all facilities in the Metals and Ceramics Division are available under SHaRE, there is a strong emphasis on analytical electron microscopy (AEM), based on state-of-the-art facilities, techniques, and recognized expertise in the Division. The microscopy facilities include four analytical electron microscopes (one 300 kV, one 200 kV, and two 120 kV instruments), a conventional transmission electron microscope with a low field polepiece for examination of ferromagnetic materials, a high voltage (1 MV) electron microscope with a number of in situ capabilities, and a variety of EM support facilities. An atom probe field-ion microscope provides microstructural and elemental characterization at atomic resolution.


MRS Bulletin ◽  
1994 ◽  
Vol 19 (6) ◽  
pp. 17-21 ◽  
Author(s):  
Frances M. Ross

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.


1998 ◽  
Vol 4 (S2) ◽  
pp. 856-857
Author(s):  
David M. Longo ◽  
James M. Howe ◽  
William C. Johnson

The focused ion beam (FIB) has become an indispensable tool for a variety of applications in materials science, including that of specimen preparation for the transmission electron microscope (TEM). Several FIB specimen preparation techniques have been developed, but some problems result when FIB specimens are analyzed in the TEM. One of these is X-ray fluorescence from bulk material surrounding the thin membrane in FIB-prepared samples. This paper reports on a new FIB specimen preparation method which was devised for the reduction of X-ray fluorescence during energy dispersive X-ray spectroscopy (EDS) in the TEM.Figure 1 shows three membrane geometries that were investigated in this study on a single-crystal Si substrate with a RF sputter-deposited 50 nm Ni film. Membrane 1 is the most commonly reported geometry in the literature, with an approximately 20 urn wide trench and a membrane having a single wedge with a 1.5° incline.


2020 ◽  
Vol 68 (6) ◽  
pp. 389-402
Author(s):  
Lars Möller ◽  
Gudrun Holland ◽  
Michael Laue

Diagnostic electron microscopy is a useful technique for the identification of viruses associated with human, animal, or plant diseases. The size of virus structures requires a high optical resolution (i.e., about 1 nm), which, for a long time, was only provided by transmission electron microscopes operated at 60 kV and above. During the last decade, low-voltage electron microscopy has been improved and potentially provides an alternative to the use of high-voltage electron microscopy for diagnostic electron microscopy of viruses. Therefore, we have compared the imaging capabilities of three low-voltage electron microscopes, a scanning electron microscope equipped with a scanning transmission detector and two low-voltage transmission electron microscopes, operated at 25 kV, with the imaging capabilities of a high-voltage transmission electron microscope using different viruses in samples prepared by negative staining and ultrathin sectioning. All of the microscopes provided sufficient optical resolution for a recognition of the viruses tested. In ultrathin sections, ultrastructural details of virus genesis could be revealed. Speed of imaging was fast enough to allow rapid screening of diagnostic samples at a reasonable throughput. In summary, the results suggest that low-voltage microscopes are a suitable alternative to high-voltage transmission electron microscopes for diagnostic electron microscopy of viruses.


1997 ◽  
Vol 5 (1) ◽  
pp. 14-15
Author(s):  
Vivian Robinson

Ever since electron microscopes were developed, it has been the goal of microscopists to observe specimens in their natural state, free from artefacts which can often be introduced through specimen preparation. For most biological specimens, that includes the presence of water. With a pressure of 10-4 torr or lower required to operate a scanning electron microscope (SEM), liquid water, which required a pressure of above 5 torr, was clearly a problem.Although several attempts had been made to examine hydrated specimens in a SEM, the first published results of water imaged in a stable and reproducible manner in the SEM, were presented at the Eighth International Congress on Electron Microscopy in Canberra in 1974 (Robinson, 1974).


Author(s):  
J. Bentley

The characterization of ceramic surfaces plays an important role in understanding a wide variety of properties such as fracture, wear, crack initiation, oxidation, sintering, and thin film growth on substrates. Three major microscopies are employed to obtain nanometer-scale resolution of ceramic surfaces: scanning electron microscopy (SEM), (scanning) transmission electron microscopy (STEM or TEM) especially in the glancing-incidence reflection modes, and scanning tip microscopies - most notably atomic force microscopy (AFM). Each technique has its own set of characteristics, advantages, and disadvantages and is usually complementary to the others.Conventional SEM is quick and easy to implement. As a mature technique, the contrast mechanisms, although sometimes complex, are largely well understood; computer programs for image simulation are available. The technique is applicable to a wide range of materials and specimen sizes; usually, little specimen preparation is involved. Charging of electrically insulating ceramics has traditionally been overcome by coating but, at high resolution, the faithful representation of the structure then becomes of some concern.


Author(s):  
Raynald Gauvin ◽  
Dominique Drouin ◽  
Pierre Hovington

In modern materials science, it is important to improve the resolution of the Scanning Electron Microscope (SEM) because small phases play a crutial role in the properties of materials. The Transmission Electron Microscope (TEM) is the tool of choice for imaging small phases embedded in a given matrix. However, this technique is expensive and also is slow owing to specimen preparation. In this context, it is important to improve spatial resolution of the SEM.In electron backscattering images, it is well know that the backscattered electrons have an energetic distribution when they escape the specimen.The electrons having loss less energy are those which have travelled less in the specimen and thus escape closer to the electron beam. So, in filtering the energy of the backscattering electron and keeping those which have loss only a small amount of energy to create the image, a significant improvement of the resolution of such images is expected. New detectors are now under development to take advantage of this technique of imaging.


2002 ◽  
Vol 8 (6) ◽  
pp. 447-466 ◽  
Author(s):  
Michael Lehmann ◽  
Hannes Lichte

Through recent years, off-axis electron holography has helped us to understand and to overcome some experimental restrictions in transmission electron microscopy. With development of powerful electron microscopes, slow-scan CCD cameras, and computers, holography is not an academic technique anymore used by specialized laboratories. Holography has proven its wide range of applications in solving real-world problems in materials science and biology. At medium resolution, that is, on nanometer scale, holography allows access to large area phase contrast produced by magnetic fields and electric potentials. In the high-resolution domain, holography unveils its power by unscrambling amplitude and phase of the electron wave, resulting in an improved lateral resolution up to the information limit. Holography is a thoroughly quantitative method, and, in combination with the perfect zero-loss filtering inherent to this method, the interpretation of the reconstructed data is strongly simplified. After outlining the basics of holography, in this tutorial we focus on development of a step-by-step procedure for recording and reconstruction of holograms. At the end, some recent applications are discussed.


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