The measurement and calculation of the X-ray spatial resolution obtained in the analytical electron microscope

1990 ◽  
Vol 160 (1) ◽  
pp. 41-53 ◽  
Author(s):  
J. R. Michael ◽  
D. B. Williams ◽  
C. F. Klein ◽  
R. Ayer
2001 ◽  
Vol 7 (S2) ◽  
pp. 694-695
Author(s):  
Eric Lifshin ◽  
Raynald Gauvin ◽  
Di Wu

In Castaing’s classic Ph.D. dissertation he described how the limiting value of x-ray spatial resolution for x-ray microanalysis, of about 1 μm, was not imposed by the diameter of the electron beam, but by the size of the region excited inside the specimen. Fifty years later this limit still applies to the majority of measurement made in EMAs and SEMs, even though there is often a need to analyze much finer structures. When high resolution chemical analysis is required, it is generally necessary to prepare thin sections and examine them in an analytical electron microscope where the maximum diameter of the excited volume may be as small as a few nanometers. Since it is not always possible or practical, it is important to determine just what is the best spatial resolution attainable for the examination of polished or “as received” samples with an EMA or SEM and how to achieve it experimentally.


Author(s):  
C. E. Lyman ◽  
J. I. Goldstein ◽  
D.B. Williams ◽  
D.W. Ackland ◽  
S. von Harrach ◽  
...  

A major goal of analytical electron micrsocopy (AEM) is to detect small amounts of an element in a given matrix at high spatial resolution. While there is a tradeoff between low detection limit and high spatial resolution, a field emission electron gun allows detection of small amounts of an element at sub-lOnm spatial resolution. The minimum mass fraction of one element measured in another is proportional to [(P/B)·P]-1/2 where the peak-to-background ratio P/B and the peak intensity P both must be high to detect the smallest amount of an element. Thus, the x-ray detection performance of an analytical electron microscope may be characterized in terms of standardized measurements of peak-to-background, x-ray intensity, the level of spurious x-rays (hole count), and x-ray detector performance in terms of energy resolution and peak shape.This paper provides measurements of these parameters from Lehigh’s VG Microscopes HB-603 field emission AEM. This AEM was designed to provide the best x-ray detection possible.


Author(s):  
A. D. Romig ◽  
J. R. Michael

High spatial resolution x-ray microanalysis in the analytical electron microscope (AEM) describes a technique by which chemical composition can be determined on spatial scales of less than 50 nm. Dependent upon the size of the incident probe, the energy (voltage) of the beam, the average atomic number of the material being analyzed, and the thickness of the specimen at the point of analysis it is possible to measure uniquely the composition of a region 2-20 nm in diameter. Conventional thermionic (tungsten or LaB6) AEMs can attain direct spatial resolutions as small as 20 nm, while field emission (PEG) AEM's can attain direct spatial resolutions approaching 2 nm. Recently, efforts have been underway to extract compositional information on a finer spatial scale by using massively parallel Monte Carlo electron trajectory simulations coupled with AEM measurements. By deconvolving the measured concentration profile with the calculated x-ray generation profile it is possible to extract compositional information at near atomic resolution.


Author(s):  
Zenji Horita ◽  
Ryuzo Nishimachi ◽  
Takeshi Sano ◽  
Minoru Nemoto

Absorption correction is often required in quantitative x-ray microanalysis of thin specimens using the analytical electron microscope. For such correction, it is convenient to use the extrapolation method[l] because the thickness, density and mass absorption coefficient are not necessary in the method. The characteristic x-ray intensities measured for the analysis are only requirement for the absorption correction. However, to achieve extrapolation, it is imperative to obtain data points more than two at different thicknesses in the identical composition. Thus, the method encounters difficulty in analyzing a region equivalent to beam size or the specimen with uniform thickness. The purpose of this study is to modify the method so that extrapolation becomes feasible in such limited conditions. Applicability of the new form is examined by using a standard sample and then it is applied to quantification of phases in a Ni-Al-W ternary alloy.The earlier equation for the extrapolation method was formulated based on the facts that the magnitude of x-ray absorption increases with increasing thickness and that the intensity of a characteristic x-ray exhibiting negligible absorption in the specimen is used as a measure of thickness.


Author(s):  
S. M. Zemyan ◽  
D. B. Williams

As has been reported elsewhere, a thin evaporated Cr film can be used to monitor the x-ray peak to background ratio (P/B) in an analytical electron microscope. Presented here are the results of P/B measurements for the Cr Ka line on a Philips EM430 TEM/STEM, with Link Si(Li) and intrinsic Ge (IG) x-ray detectors. The goal of the study was to determine the best conditions for x-ray microanalysis.We used the Fiori P/B definition, in which P/B is the ratio of the total peak integral to the average background in a 10 eV channel beneath the peak. Peak and background integrals were determined by the window method, using a peak window from 5.0 to 5.7 keV about Cr Kα, and background windows from 4.1 to 4.8 keV and 6.3 to 7.0 keV.


2014 ◽  
Vol 20 (4) ◽  
pp. 1318-1326 ◽  
Author(s):  
Nestor J. Zaluzec

AbstractClosed form analytical equations used to calculate the collection solid angle of six common geometries of solid-state X-ray detectors in scanning and scanning/transmission analytical electron microscopy are presented. Using these formulae one can make realistic comparisons of the merits of the different detector geometries in modern electron column instruments. This work updates earlier formulations and adds new detector configurations.


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