Energy dispersive compositional

Several forensic laboratories in the United States and in other countries have SEM facilities, many of which are equipped for energy dispersive compositional analysis (EDA). This paper will describe selected actual recent applications of SEM-EDA techniques performed at the New York State Police Scientific Laboratory and Electron Microanalysis Laboratory at Rensselaer Polytechnic Institute. 

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. 

Asbestos fiber identification can also be achieved through transmission or scanning electron microscopy (tern, sem) techniques which are especially usefiil with very short fibers, or with extremely small samples (see Microscopy). With appropriate peripheral instmmentation, these techniques can yield the elemental composition of the fibers using energy dispersive x-ray fluorescence, or the crystal stmcture from electron diffraction, selected area electron diffraction (saed). 

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-... 

Film-forming chemical reactions and the chemical composition of the film formed on lithium in nonaqueous aprotic liquid electrolytes are reviewed by Dominey [7], SEI formation on carbon and graphite anodes in liquid electrolytes has been reviewed by Dahn et al. [8], In addition to the evolution of new systems, new techniques have recently been adapted to the study of the electrode surface and the chemical and physical properties of the SEI. The most important of these are X-ray photoelectron spectroscopy (XPS), SEM, X-ray diffraction (XRD), Raman spectroscopy, scanning tunneling microscopy (STM), energy-dispersive X-ray spectroscopy (EDS), FTIR, NMR, EPR, calorimetry, DSC, TGA, use of quartz-crystal microbalance (QCMB) and atomic force microscopy (AFM). 

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). 

Energy-dispersive X-ray analyses were carried out by using the ratio technique (equation 1) to relate compositions to the intensities of the CoKa and WL characteristic X-ray peaks. The value of the kw Co factor was experimentally determined using single-phase eCo samples. A series of EDX analyses was performed from the edge to the interior of the foil and the results plotted in the form of the relationship ... 

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. 

The pH, EC and Fe3+ were used as control parameters. The first two were measured with an Orion probe combined pH/ATC electrode Triode and a conductivity cell DuraProbe ref. 0133030. Fe3+ was determined by molecular absorption (thiocyanate method). Mineralogical composition of the precipitates was determined by X-ray powder diffraction (XRD). Scanning electron microscopy, combined with an energy dispersive system (SEM-EDS), allowed the observation of morphological and compositional aspects of the precipitates. 

In HRTEM, very thin samples can be treated as weak-phase objects (WPOs) whereby the image intensity can be correlated with the projected electrostatic potential of crystals, leading to atomic structural information. Furthermore, the detection of electron-stimulated XRE in the electron microscope (energy dispersive X-ray spectroscopy, or EDX, discussed in the following sections) permits simultaneous determination of chemical compositions of catalysts to the sub-nanometer level. Both the surface and bulk structures of catalysts can be investigated. 

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]. 

Local composition is very useful supplementary information that can be obtained in many of the transmission electron microscopes (TEM). The two main methods to measure local composition are electron energy loss spectrometry (EELS), which is a topic of a separate paper in this volume (Mayer 2004) and x-ray emission spectrometry, which is named EDS or EDX after the energy dispersive spectrometer, because this type of x-ray detection became ubiquitous in the TEM. Present paper introduces this latter method, which measures the X-rays produced by the fast electrons of the TEM, bombarding the sample, to determine the local composition. As an independent topic, information content and usage of the popular X-ray powder dififaction database is also introduced here. Combination of information from these two sources results in an efficient phase identification. Identification of known phases is contrasted to solving unknown stmctures, the latter being the topic of the largest fiaction of this school. 

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