Electron microscopy materials

National Center for Electron Microscopy, Materials and Chemicals Sciences Division, Lawrence Berkeley Laboratory, Berkeley, CA 94720... 

LCenter for Advanced Materials, Materials and Chemical Sciences Division, Lawrence Berkeley Laboratory, and Materials Science and Mineral Engineering Department, University of California, Berkeley, CA 94720 2National Center for Electron Microscopy, Materials and Chemical Sciences Division, Lawrence Berkeley Laboratory, and Materials Science and Mineral Engineering Department, University of California, Berkeley, CA 94720... 

The specific surface area of a solid is one of the first things that must be determined if any detailed physical chemical interpretation of its behavior as an adsorbent is to be possible. Such a determination can be made through adsorption studies themselves, and this aspect is taken up in the next chapter there are a number of other methods, however, that are summarized in the following material. Space does not permit a full discussion, and, in particular, the methods that really amount to a particle or pore size determination, such as optical and electron microscopy, x-ray or neutron diffraction, and permeability studies are largely omitted. 

Thomas G and Goringe M J 1981 Transmission Electron Microscopy of Materials (New York Wiiey)... 

Williams D B and Carter C B 1996 Transmission Electron Microscopy, A Textbook for Material Science (New York Plenum)... 

A variety of experimental techniques have been employed to research the material of this chapter, many of which we shall not even mention. For example, pressure as well as temperature has been used as an experimental variable to study volume effects. Dielectric constants, indices of refraction, and nuclear magnetic resonsance (NMR) spectra are used, as well as mechanical relaxations, to monitor the onset of the glassy state. X-ray, electron, and neutron diffraction are used to elucidate structure along with electron microscopy. It would take us too far afield to trace all these different techniques and the results obtained from each, so we restrict ourselves to discussing only a few types of experimental data. Our failure to mention all sources of data does not imply that these other techniques have not been employed to good advantage in the study of the topics contained herein. 

Physical testing appHcations and methods for fibrous materials are reviewed in the Hterature (101—103) and are generally appHcable to polyester fibers. Microscopic analyses by optical or scanning electron microscopy are useful for evaluating fiber parameters including size, shape, uniformity, and surface characteristics. Computerized image analysis is often used to quantify and evaluate these parameters for quaUty control. 

Nylon-6. Nylon-6—clay nanometer composites using montmorillonite clay intercalated with 12-aminolauric acid have been produced (37,38). When mixed with S-caprolactam and polymerized at 100°C for 30 min, a nylon clay—hybrid (NCH) was produced. Transmission electron microscopy (tern) and x-ray diffraction of the NCH confirm both the intercalation and molecular level of mixing between the two phases. The benefits of such materials over ordinary nylon-6 or nonmolecularly mixed, clay-reinforced nylon-6 include increased heat distortion temperature, elastic modulus, tensile strength, and dynamic elastic modulus throughout the —150 to 250°C temperature range. 

Transmission electron microscopy (tern) is used to analyze the stmcture of crystals, such as distinguishing between amorphous siUcon dioxide and crystalline quartz. The technique is based on the phenomenon that crystalline materials are ordered arrays that scatter waves coherently. A crystalline material diffracts a beam in such a way that discrete spots can be detected on a photographic plate, whereas an amorphous substrate produces diffuse rings. Tern is also used in an imaging mode to produce images of substrate grain stmctures. Tern requires samples that are very thin (10—50 nm) sections, and is a destmctive as well as time-consuming method of analysis. 

Transmission electron microscopy is very widely used by biologists as well as materials scientists. The advantage of being able to resolve 0.2 nm outweighs the disadvantages of TEM. The disadvantages include the inabiUty of the common 100-kV electron beam to penetrate more than a few tenths of a micrometer (a 1000-kV beam, rarely used, penetrates specimens about 10 times thicker). Specimen preparation for the TEM is difficult because of the... 

In order to define the extent of emissions from automotive brakes and clutches, a study was carried out in which specially designed wear debris collectors were built for the dmm brake, the disk brake, and the clutch of a popular U.S. vehicle (1). The vehicle was driven through various test cycles to determine the extent and type of brake emissions generated under all driving conditions. Typical original equipment and aftermarket friction materials were evaluated. Brake relines were made to simulate consumer practices. The wear debris was analyzed by a combination of optical and electron microscopy to ascertain the asbestos content and its particle size distribution. It was found that more than 99.7% of the asbestos was converted to a nonfibrous form and... 

A variety of instmmental techniques may be used to determine mineral content. Typically the coal sample is prepared by low temperature ashing to remove the organic material. Then one or more of the techniques of x-ray diffraction, infrared spectroscopy, differential thermal analysis, electron microscopy, and petrographic analysis may be employed (7). 

M. von Heimendahl. Electron Microscopy of Materials An Introduction. Materials Science and Technology Series (A S. Nowick, ed.) Academic, New York, 1980, Chapter l.This is an excellent introductory guide to the principles of TEM. 

J. W. Edington. Practical Electron Microscopy in Materials, van Nostrand Reinhold, New York, 1976. This is an excellent general reference and laboratory handbook for the TEM user. 

K. C. Thompson-Russell and J. W. Edington. Electron Microscope Specimen Preparation Techniques in Materials Science. Monographs in Practical Electron Microscopy, No. 5- Philips Technical Library, Eindhoven Delaware, 1977. 

D. B. Williams. Practical Analytical Electron Microscopy in Materials Science. Verlag Chemie International, Weinheim, 1984. A good monograph discussing the use and applications of AEM, especially at intermediate voltages. The discussion on EDS is an excellent primer for using X-ray analysis on a TEM. 

Cathodoluminescence (CL), i.e., the emission of light as the result of electron-beam bombardment, was first reported in the middle of the nineteenth century in experiments in evacuated glass tubes. The tubes were found to emit light when an electron beam (cathode ray) struck the glass, and subsequendy this phenomenon led to the discovery of the electron. Currendy, cathodoluminescence is widely used in cathode-ray tube-based (CRT) instruments (e.g., oscilloscopes, television and computer terminals) and in electron microscope fluorescent screens. With the developments of electron microscopy techniques (see the articles on SEM, STEM and TEM) in the last several decades, CL microscopy and spectroscopy have emerged as powerfirl tools for the microcharacterization of the electronic propenies of luminescent materials, attaining spatial resolutions on the order of 1 pm and less. Major applications of CL analysis techniques include ... 

High Resolution Transmission Electron Microscopy and Associated Techniques. (P. R. Buseck, J. M. Cowley, and L. Eyring, eds.) Oxford University Press, New York, 1988. A review covering these techniques in detail (except X-ray microanalysis) including extensive material on high-resolution TEM. 

Speciman Preparation for Transmission Electron Microscopy of Materials (J. C. Brauman, R. M. Anderson, and M. L. McDonald, eds.) MRS Symp. Proc vol. 115, Materials Research Society, Pittsburg, 1988. This conference proceedings contains many up-to-date methods as well as references to books on various aspects of specimen preparation. 

Alternatives to XRD include transmission electron microscopy (TEM) and diffraction, Low-Energy and Reflection High-Energy Electron Diffraction (LEED and RHEED), extended X-ray Absorption Fine Structure (EXAFS), and neutron diffraction. LEED and RHEED are limited to surfaces and do not probe the bulk of thin films. The elemental sensitivity in neutron diffraction is quite different from XRD, but neutron sources are much weaker than X-ray sources. Neutrons are, however, sensitive to magnetic moments. If adequately large specimens are available, neutron diffraction is a good alternative for low-Z materials and for materials where the magnetic structure is of interest. 

D. B. Williams, C. B. Carter Transmission Electron Microscopy - A Textbook for Materials Science, Plenum Press, New York and London 1996. 

S. Amelincks, D. van Dyck, J. van Landuyt, G. van Tendeloo (eds.) Electron Microscopy Principles and Fundamentals,VCH Verlagsgesellschaft mbH, Weinheim 1997. 2-178 R. M. Anderson, S. D. Walck (eds.) Specimen Preparation for Transmission Electron Microscopy of Materials IV, Materials Research Society, Pittsbrrrgh 1997. 

J. Heydenreich, W. Neumann (eds.) Proc. Analytical Transmission electron Microscopy in Materials Science - Fundamentals andTechni-ques, Elbe Druckerei, Wittenberg, 1993. 

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