Energy dispersive compositional analysis

Current methods used to image MCM-41 include (1) analytical transmission electron microscopy (TEM) to determine structure, size, morphology, and local chemical composition (2) energy-dispersive X-ray spectroscopy (EDXS) in a scanning electron microscope (SEM) to determine chemical composition 5 and (3) electron energy loss spectroscopy (EELS) for elemental analysis.6... 

Figure 12.17 (a) Scanning electron micrograph of a cross-section of a carbon/carbon composite (b) energy-dispersive spectroscopy analysis showing location of silicon. 

Chemical analysis of the metal can serve various purposes. For the determination of the metal-alloy composition, a variety of techniques has been used. In the past, wet-chemical analysis was often employed, but the significant size of the sample needed was a primary drawback. Nondestmctive, energy-dispersive x-ray fluorescence spectrometry is often used when no high precision is needed. However, this technique only allows a surface analysis, and significant surface phenomena such as preferential enrichments and depletions, which often occur in objects having a burial history, can cause serious errors. For more precise quantitative analyses samples have to be removed from below the surface to be analyzed by means of atomic absorption (82), spectrographic techniques (78,83), etc. 

Tubercle compositions were measured using energy dispersive x-ray analysis) ... 

Close examination of the weld under a low-power stereoscopic microscope revealed small openings (Fig. 15.6). Probing these sites with a pin revealed a large pit that had been covered by a thin skin of weld metal. These sites contained fibrous, metallic remnants (Fig. 15.7). Examination under a scanning electron microscope further revealed the fibrous character of the material (Fig. 15.2) and also the convoluted shapes of the individual fibers (Fig. 15.21). Energy-dispersive spectrographic analysis of this material revealed the compositions in Table 15.1. 

We have already discussed a number of applications of the SEM to materials characterization topographical (SE) imaging, Energy-Dispersive X-Ray analysis (EDS) and the use of backscattering measurements to determine the composition of binary alloy systems. We now shall briefly discuss applications that are, in part, spe-... 

As illustrated by Eig. 4.13, an electron microscope offers additional possibilities for analyzing the sample. Diffraction patterns (spots from a single-crystal particle and rings from a collection of randomly oriented particles) enable one to identify crystallographic phases as in XRD. Emitted X-rays are characteristic for an element and allow for a determination of the chemical composition of a selected part of the sample. This technique is referred to as energy-dispersive X-ray analysis (EDX). 

SEM studies of composites were carried out using a JEOL JSM-T300 scanning electron microscope. Energy dispersive X-ray (EDX) analysis was performed by energy dispersive device LINK 860-500 attached to the SEM unit. JEOL-JEM-200 transmission electron microscope was used for TEM investigations. 

As indicated in Fig. 7.2, X-rays are among the by-products in an electron microscope. Already at the beginning of this century, people knew that matter emits X-rays when it is bombarded with electrons. The explanation of the phenomenon came with the development of quantum mechanics. Nowadays, it is the basis for determining composition on the submicron scale and, with still increasing spatial resolution, is used in the technique referred to as Electron Microprobe Analysis (EMA), Electron Probe Microanalysis (EPMA) or Energy Dispersive Analysis of X-rays (EDAX, EDX) [21]. 

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