scholarly journals True Colour SEM Imaging for Phase Recognition AMD X-Ray Microanalysis

1997 ◽  
Vol 5 (3) ◽  
pp. 8-18
Author(s):  
Peter J. Statham

Secondary (SE) and backscattered electron (BSE) signals in the SEM provide high resolution monochrome images. BSE signal strength is modulated by mean atomic number and ‘false” colour can be introduced to enhance material contrast. Colour can also be introduced using multiple SE detectors, each with a different sensitivity to topographic and compositional information: by controlling signal mixtures and colours, the operator effectively has access to a powerful “studio” to generate aesthetically pleasing colour images. In both these examples, the correspondence between local elemental content and colour is entirely arbitrary and under subjective control of the operator, Elemental x-ray maps can be acquired and combinations colour coded to reveal phase distributions. For large numbers of maps and images, chemometric techniques such as PCA may be used to discover common relationships and assist the process of colour coding. Images derived from x-ray maps are usually low resolution and the analyst has to decide which elements to include and do a fair amount of data manipulation before any conclusions can be drawn.

Author(s):  
Peter J. Statham

Secondary (SE) and backscattered electron (BSE) signals in the SEM provide high resolution monochrome images. BSE signal strength is modulated by mean atomic number and “false” colour can be introduced to enhance material contrast. Colour can also be introduced using multiple SE detectors, each with a different sensitivity to topographic and compositional information: by controlling signal mixtures and colours, the operator effectively has access to a powerful “studio” to generate aesthetically pleasing colour images. In both these examples, the correspondence between local elemental content and colour is entirely arbitrary and under subjective control of the operator. Elemental x-ray maps can be acquired and combinations colour coded to reveal phase distributions. For large numbers of maps and images, chemometric techniques such as PCA may be used to discover common relationships and assist the process of colour coding. Images derived from x-ray maps are usually low resolution and the analyst has to decide which elements to include and do a fair amount of data manipulation before any conclusions can be drawn. Furthermore, local topography effects perturb any multivariate statistical analysis. This paper presents a novel imaging technique which addresses these limitations.


Author(s):  
I. Noell ◽  
D. Morris

Proton microprobe and electron probe X-ray microanalysis (EPXMA) simultaneously measure and map elemental content, and hence are excellent tools for investigating the distribution and function of elevated Ni levels in hyperaccumulating plants (Ni concentration >1000 μg g−1 dry weight). Five major hypotheses have been proposed for the function of Ni hyperaccumulation. Our research focuses on the hypothesis that Ni defends against herbivore or pathogen attack and examines the movement of Ni from soil through plant to herbivore in Stackhousia tryonii, the only known hyperaccumulator in eastern Australia. Using a JEOL JXA-840-A electron probe microanalyzer with Moran Scientific Analysis software, we located features of high mean atomic number in whole leaves and cross-sections through backscattered-electron imaging (BEI), then we used EPXMA to identify the elements present and to prepare semi-quantitative x-ray maps of seven key elements.


Author(s):  
J. L. Abraham ◽  
K. Miyai

The scanning electron microscope (SEM) offers several signal modes, each of which may contain unique information about the specimen. In this paper we demonstrate and compare the merits of the familiar secondary electron (SE) mode, the backscattered electron (BSE) mode, and x-ray distribution mapping.Lungs of hamsters treated intratracheally with the radiographic contrast medium tantalum suspended in carboxymethyl cellulose were fixed with intratracheal buffered 2% glutaraldehyde. Blocks were razor cut to a few mm, dehydrated and critical point dried. The dried blocks were mounted on aluminum SEM studs and coated with carbon,, followed in some instances by gold/palladium (60/40). Examination at 20 kv and 45° specimen tilt was done in an Etec SEM with a solid state BSE detector and a Cambridge S4 SEM with an ORTEC energy dispersive x-ray analysis system.


Author(s):  
J.M. Titchmarsh

The advances in recent years in the microanalytical capabilities of conventional TEM's fitted with probe forming lenses allow much more detailed investigations to be made of the microstructures of complex alloys, such as ferritic steels, than have been possible previously. In particular, the identification of individual precipitate particles with dimensions of a few tens of nanometers in alloys containing high densities of several chemically and crystallographically different precipitate types is feasible. The aim of the investigation described in this paper was to establish a method which allowed individual particle identification to be made in a few seconds so that large numbers of particles could be examined in a few hours.A Philips EM400 microscope, fitted with the scanning transmission (STEM) objective lens pole-pieces and an EDAX energy dispersive X-ray analyser, was used at 120 kV with a thermal W hairpin filament. The precipitates examined were extracted using a standard C replica technique from specimens of a 2¼Cr-lMo ferritic steel in a quenched and tempered condition.


Author(s):  
M.D. Ball ◽  
H. Lagace ◽  
M.C. Thornton

The backscattered electron coefficient η for transmission electron microscope specimens depends on both the atomic number Z and the thickness t. Hence for specimens of known atomic number, the thickness can be determined from backscattered electron coefficient measurements. This work describes a simple and convenient method of estimating the thickness and the corrected composition of areas of uncertain atomic number by combining x-ray microanalysis and backscattered electron intensity measurements.The method is best described in terms of the flow chart shown In Figure 1. Having selected a feature of interest, x-ray microanalysis data is recorded and used to estimate the composition. At this stage thickness corrections for absorption and fluorescence are not performed.


Author(s):  
Allen Angel ◽  
Kathryn A. Jakes

Fabrics recovered from archaeological sites often are so badly degraded that fiber identification based on physical morphology is difficult. Although diagenetic changes may be viewed as destructive to factors necessary for the discernment of fiber information, changes occurring during any stage of a fiber's lifetime leave a record within the fiber's chemical and physical structure. These alterations may offer valuable clues to understanding the conditions of the fiber's growth, fiber preparation and fabric processing technology and conditions of burial or long term storage (1).Energy dispersive spectrometry has been reported to be suitable for determination of mordant treatment on historic fibers (2,3) and has been used to characterize metal wrapping of combination yarns (4,5). In this study, a technique is developed which provides fractured cross sections of fibers for x-ray analysis and elemental mapping. In addition, backscattered electron imaging (BSI) and energy dispersive x-ray microanalysis (EDS) are utilized to correlate elements to their distribution in fibers.


Author(s):  
R. J. Lee ◽  
A. J. Schwoeble ◽  
Yuan Jie

Water/Cement (W/C) ratio is a very important parameter affecting the strength and durability of concrete. At the present time, there are no ASTM methods for determining W/C ratio of concrete structures after the production period. Existing techniques involving thin section standard density comparative associations using light optical microscopy and rely on visual comparisons using standards and require highly trained personnel to produce reliable data. This has led to the exploration of other methods utilizing automated procedures which can offer a precise and rapid measurement of W/C ratio. This paper discusses methods of determining W/C ratio using a scanning electron microscope (SEM) backscattered electron image (BEI) intensity signal and x-ray computer tomography.


Author(s):  
M. D. Vaudin ◽  
J. P. Cline

The study of preferred crystallographic orientation (texture) in ceramics is assuming greater importance as their anisotropic crystal properties are being used to advantage in an increasing number of applications. The quantification of texture by a reliable and rapid method is required. Analysis of backscattered electron Kikuchi patterns (BEKPs) can be used to provide the crystallographic orientation of as many grains as time and resources allow. The technique is relatively slow, particularly for noncubic materials, but the data are more accurate than any comparable technique when a sufficient number of grains are analyzed. Thus, BEKP is well-suited as a verification method for data obtained in faster ways, such as x-ray or neutron diffraction. We have compared texture data obtained using BEKP, x-ray diffraction and neutron diffraction. Alumina specimens displaying differing levels of axisymmetric (0001) texture normal to the specimen surface were investigated.BEKP patterns were obtained from about a hundred grains selected at random in each specimen.


Author(s):  
N.K.R. Smith ◽  
K.E. Hunter ◽  
P. Mobley ◽  
L.P. Felpel

Electron probe energy dispersive x-ray microanalysis (XRMA) offers a powerful tool for the determination of intracellular elemental content of biological tissue. However, preparation of the tissue specimen , particularly excitable central nervous system (CNS) tissue , for XRMA is rather difficult, as dissection of a sample from the intact organism frequently results in artefacts in elemental distribution. To circumvent the problems inherent in the in vivo preparation, we turned to an in vitro preparation of astrocytes grown in tissue culture. However, preparations of in vitro samples offer a new and unique set of problems. Generally, cultured cells, growing in monolayer, must be harvested by either mechanical or enzymatic procedures, resulting in variable degrees of damage to the cells and compromised intracel1ular elemental distribution. The ultimate objective is to process and analyze unperturbed cells. With the objective of sparing others from some of the same efforts, we are reporting the considerable difficulties we have encountered in attempting to prepare astrocytes for XRMA.Tissue cultures of astrocytes from newborn C57 mice or Sprague Dawley rats were prepared and cultured by standard techniques, usually in T25 flasks, except as noted differently on Cytodex beads or on gelatin. After different preparative procedures, all samples were frozen on brass pins in liquid propane, stored in liquid nitrogen, cryosectioned (0.1 μm), freeze dried, and microanalyzed as previously reported.


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