Transmission electron microscopy materials

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)... 

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... 

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. 

Processes that occur at a size scale larger than the individual chain have been studied using microscopy, mainly transmission electron microscopy (TEM), but optical microscopy has been useful to examine craze shapes. The knowledge of the crazing process obtained by TEM has been ably summarised by Kramer and will not be repeated here [2,3]. At an interface between two polymers a craze often forms within one of the materials, typically the one with lower crazing stress. 

High-resolution transmission electron microscopy (HREM) is the technique best suited for the structural characterization of nanometer-sized graphitic particles. In-situ processing of fullerene-related structures may be performed, and it has been shown that carbonaceous materials transform themselves into quasi-spherical onion-like graphitic particles under the effect of intense electron irradiation[l 1],... 

Four different material probes were used to characterize the shock-treated and shock-synthesized products. Of these, magnetization provided the most sensitive measure of yield, while x-ray diffraction provided the most explicit structural data. Mossbauer spectroscopy provided direct critical atomic level data, whereas transmission electron microscopy provided key information on shock-modified, but unreacted reactant mixtures. The results of determinations of product yield and identification of product are summarized in Fig. 8.2. What is shown in the figure is the location of pressure, mean-bulk temperature locations at which synthesis experiments were carried out. Beside each point are the measures of product yield as determined from the three probes. The yields vary from 1% to 75 % depending on the shock conditions. From a structural point of view a surprising result is that the product composition is apparently not changed with various shock conditions. The same product is apparently obtained under all conditions only the yield is changed. 

Multi-walled CNTs (MWCNTs) are produced by arc discharge between graphite electrodes but other carbonaceous materials are always formed simultaneously. The main by-product, nanoparticles, can be removed utilizing the difference in oxidation reaction rates between CNTs and nanoparticles [9]. Then, it was reported that CNTs can be aligned by dispersion in a polymer resin matrix [10]. However, the parameters of CNTs are uncontrollable, such as the diameter, length, chirality and so on, at present. Furthermore, although the CNTs are observed like cylinders by transmission electron microscopy (TEM), some reports have pointed out the possibility of non-cylindrical structures and the existence of defects [11-14]. 

Alloys were prepared by arc melting high purity starting materials followed by homogenisation. Transmission electron microscopy specimens were prepared by... 

Usually, the molecular strands are coiled in the glassy polymer. They become stretched when a crack arrives and starts to build up the deformation zone. Presumably, strain softened polymer molecules from the bulk material are drawn into the deformation zone. This microscopic surface drawing mechanism may be considered to be analogous to that observed in lateral craze growth or in necking of thermoplastics. Chan, Donald and Kramer [87] observed by transmission electron microscopy how polymer chains were drawn into the fibrils at the craze-matrix-interface in PS films [92]. One explanation, the hypothesis of devitrification by Gent and Thomas [89] was set forth as early as 1972. 

Recent demands for polymeric materials request them to be multifunctional and high performance. Therefore, the research and development of composite materials have become more important because single-polymeric materials can never satisfy such requests. Especially, nanocomposite materials where nanoscale fillers are incorporated with polymeric materials draw much more attention, which accelerates the development of evaluation techniques that have nanometer-scale resolution." To date, transmission electron microscopy (TEM) has been widely used for this purpose, while the technique never catches mechanical information of such materials in general. The realization of much-higher-performance materials requires the evaluation technique that enables us to investigate morphological and mechanical properties at the same time. AFM must be an appropriate candidate because it has almost comparable resolution with TEM. Furthermore, mechanical properties can be readily obtained by AFM due to the fact that the sharp probe tip attached to soft cantilever directly touches the surface of materials in question. Therefore, many of polymer researchers have started to use this novel technique." In this section, we introduce the results using the method described in Section 21.3.3 on CB-reinforced NR. 

Many years have passed since the early days of AFM, when adhesion was seen as a hindrance, and it is now regarded as a useful parameter for identification of material as well as a key to understanding many important processes in biological function. In this area, the ability of AFM to map spatial variations of adhesion has not yet been fully exploited but in future could prove to be particularly useful. At present, the chemical nature and interaction area of the AFM probe are still rarely characterized to a desirable level. This may be improved dramatically by the use of nanotubes, carbon or otherwise, with functionalized end groups. However, reliance on other measurement techniques, such as transmission electron microscopy and field ion microscopy, will probably be essential in order to fully evaluate the tip-sample systems under investigation. 

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