Scanning electron microscopy and energy dispersive analysis using X-rays

14 Scanning Electron Microscopy and Energy Dispersive Analysis using X-rays 

The earliest paper identified on this technique was published in 1996, in which ED AX was used for elemental analysis in order to map the non-crystalline regions in semicrystalline PET [393]. 

Dilsiz and co-workers used SEM and ED AX to examine silver coatings of spindle- and filament-type particles for conductive adhesive properties [394]. The same technique was used by Lambert and co-workers [395] to examine the silicate structure deep in PET comonomer/silicate hybrid materials. 

Start and Mauritz [396] used environmental SEM-EDAX, and also AFM and transmission electron microscopy, to study the formation of organic-inorganic nanocomposites within surlyn(PE-co-methacrylate-cation forms) random copolymers. SEM-EDAX has also been used to study of thin films of Prussian blue and N-substituted polypyrroles [397], epoxy resins [399], and the cause of failure in acetal plumbing fittings caused by exposure to chlorine [400]. 

Mazzanti, A. Valvassori and A. Pajaro, Chimica e L Industria (Milan), 1957,29, 773. 

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Pseudomorphs on a bronze Shang Dynasty halberd (ca. 1300 b.c.) were subjected to mineralogical analysis to determine their structure and composition. X-Ray diffraction, scanning electron microscopy, and energy dispersive analysis of x-rays were used in these analyses. Photomicrographs of pseudomorphs also were studied for fiber, yam, and fabric formations that give evidence of textiles. A model describing the process of silk pseudomorph formation was proposed. 

The role of silica-only systems on adhesion has been studied using model compounds with squalene [59]. It was shown that the mechanism for increased adhesion to brass-coated wire-to-rubber was not just a simple improvement of the physical properties of the rubber, but that silica moderated the thickness and composition of the interfacial layer by a chemical interaction. SEM-EDX (scanning electron microscopy with energy dispersive analysis of X-rays), XPS, AES and PIXE (proton induced X-ray emission spectroscopy) revealed that silica affected the relative concentrations of compounds present in the interfacial layer, promoting zinc oxide formation in particular. 

The composites as well as the nanowires were characterized by several techniques. Scanning electron microscopy (SEM) images and energy dispersive analysis of x-rays (EDAX) were obtained with a Leica S-440I microscope fitted with a Link ISIS spectrometer. Infrared (IR) spectra were recorded on small pieces of the samples embedded in KBr pellets using a Broker FT-IR spectrometer. DSC was carried out on the samples ( 7 mg) with a scanning rate of 20 K min-1 between 120 and 260 °C using a Mettler-Toledo DSC. 

Sakai W. S. and Sanford W. G. (1984) A developmental study of silicification in the abaxial epidermal cells of sugarcane leaf blades using scanning electron microscopy and energy dispersive X-ray analysis. Am. J. Bot. 71, 1315-1322. 

Automated image analysis used in conjunction with scanning electron microscopy and energy-dispersive x-ray analysis has been shown to be an effective tool to characterize in-situ the mineral matter in raw... 

THERMAL STUDIES OF MATERIALS USING HEATING AND COOLING STAGE SCANNING ELECTRON MICROSCOPY AND ENERGY DISPERSIVE X-RAY ANALYSIS... 

The amount of K which may be extracted by H2O has been reported to increase [67, 68] or to decrease [66] by the addition of Si the amount of K which may be extracted by H2O is decreased [66] by the addition of Ca, and decreases [67, 68] or increases [66] by heating the unreduced catalyst. By scanning electron microscopy and energy dispersive X-ray analysis it was found that K segregates to the outer part of the catalyst particles with storage and prolonged use [69]. 

In an article published in Analytical Chemistry in 2004, Keune and Boon [2004a] present the application of ToF-SIMS analysis to a paint cross-section. The sample used was from the panel painting The Descent from the Cross (Museo del Prado, Madrid) by the early Flemish painter Rogier van der Weyden (1399/1400 1464). Scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX) and infrared microscopy were also used to complete and confirm the results. 

Another technique we used to observe these distributions is scanning electron microscopy with energy dispersive x-ray analysis (EDAX). Concentrations of Cyasorb UV 1084, [2-2 -thiobis(4-ter -octylphenolato)-n-butylamine nickel], a nickel-containing UV absorber, were point counted to obtain nickel concentrations along a spherulite diameter. Figure 3 shows results for 1 and 4 wt % additive. This shows a uniform melt concentration, a boundary peak, a lower concentration within the spherulite, and a central dip. The resolution and sensitivity with this technique are poorer than with the optical microscopy. With every method, thin film crystallized samples and microtomed sections of bulk samples gave similar results. 

Scanning electron microscopy with energy dispersive X-ray spectrometry has found extensive applications in the analysis of glass, paint, fibers, and especially in the identification of gunshot residues (where it is the method of choice). This technique offers high resolution, great depth of field, and qualitative and quantitative information on small samples. However, although this technique has much to offer, its use in crime detection is often overrated. 

Among the variety of micro-analytical techniques used, electron probe X-ray micro-analysis (EPXMA) and computer controlled scanning electron microscopy with energy-dispersive X-ray detection (CC-SEM/EDX) are most commonly used. Both can be used in fully automated mode, and in combination with cluster analysis and/or multivariate techniques. They are ideally suited for the analysis of representative numbers (300-1000... 

CAR can be observed microscopically on double-sided PWBs using back lighting (Rig. 12). Subsequent scanning electron microscopy with energy dispersive x-ray spectroscopy (SEM/EDS) analysis shows that it contains copper and chloride (Fig. 13). A CAR sample was extracted and transmission electron microscopy (TEM) analysis was used to obtain electron diffraction data. Analysis of these results identify CAR as atacamite, Cu2(OH)3Cl (Ref 24). The Pourbaix diagram (Ref 25) (Fig. 14) of the cop-... 

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