"Standardless" Quantitative Electron Probe Microanalysis with Energy-Dispersive X-ray Spectrometry: Is It Worth the Risk?

1995 ◽  
Vol 67 (11) ◽  
pp. 1866-1871 ◽  
Author(s):  
Dale E. Newbury ◽  
Carol R. Swyt ◽  
Robert L. Myklebust
Author(s):  
J. D. Brown

The goal of correction methods for quantitative electron probe microanalysis is to convert k-ratios for any type of specimen, any x-ray line and all electron beam energies into accurate concentrations. Early attempts to approach this goal were hindered by sparse data on electron interactions with solids, limited knowledge of x-ray parameters such as mass absorption coefficients and limited computing power which made necessary mathematical simplifications in practical applications.In developing the early models for quantitative analysis, the argument was made that the absorption correction was insensitive to the shape of the ϕ(ρz) curve. For that reason, a number of very crude models which ranged from constant x-ray generation as a function of depth(l) to an exponential decrease from the surface(2) were used. In fact, these models worked quite well for the restricted conditions for which they were designed but of course lack accuracy when applied to more general situations. ϕ(ρz) measurements


2008 ◽  
Vol 14 (S2) ◽  
pp. 1152-1153
Author(s):  
K Keil ◽  
R Fitzgerald ◽  
KFJ Heinrich

Extended abstract of a paper presented at Microscopy and Microanalysis 2008 in Albuquerque, New Mexico, USA, August 3 – August 7, 2008


Author(s):  
Peter Willich

Materials containing ultralight elements (B, C, N, O) in combination with a metal are of considerable interest in thin film technology. Quantitative electron probe microanalysis of the coatings should be independent of the substrate and has to be carried out under the condition that the ultimate depth of x-ray emission (Rx) is within the provided film thickness of 0.2-0.8 μm. Rx, for an element (critical excitation energy Ec) in a specified matrix is controlled by the energy (E0) of the primary electrons. EPMA of high atomic number elements (Ec = 2-7 keV), under the condition of Rx < 1 μm, frequently requires operation at a low overvoltage of E0/Ec < 2. Consequendy, tne x-ray intensities are very low and the analytical sensitivity is drastically reduced. For the ultralight elements the strong effects oft x-ray absorption always lead to a shallow depth of x-ray emission, even at a high overvoltage.


2004 ◽  
Vol 10 (6) ◽  
pp. 733-738 ◽  
Author(s):  
Guillaume F. Bastin ◽  
Hans J.M. Heijligers

The influence of a lack of sufficient electrical conductivity on the results of quantitative electron probe microanalysis has been investigated on a number of oxides. The effect of surface charging and the way it alters the emitted X-ray signals has been studied. It is shown that the presence of conducting coatings, such as carbon or copper, will affect the interelement X-ray intensity ratios, whatever the thickness of the coating may be. Although the effects for heavier elements may be acceptable, they cannot be ignored for a light element such as oxygen, where strong variations with coating thickness were observed. Quantitative analyses of oxygen, on uncoated well-conducting oxide specimens, using uncoated well-conducting hematite (Fe2O3) as a standard yielded excellent results in the range between 4 and 40 kV with the φ(ρz) software used. As soon as coated nonconducting specimens were examined, using the same hematite standard, coated under exactly the same conditions, widely scattering and noncoherent results were obtained. These discrepancies can only be attributed to a lack of conductivity.


2001 ◽  
Vol 30 (6) ◽  
pp. 419-426 ◽  
Author(s):  
J. Osán ◽  
J. de Hoog ◽  
P. Van Espen ◽  
I. Szalóki ◽  
C.-U. Ro ◽  
...  

1998 ◽  
Vol 4 (S2) ◽  
pp. 222-223
Author(s):  
John J. Donovan

A number of problematic analytical situations are known to exist in electron probe microanalysis (EPMA) where characteristic x-ray spectral overlaps are not only severe, but are also of the “self-interfering” or “cascade” variety. The “self-interfering” variety is exemplified by the innocuous Ba Lα ↔ Ti Kα; to the fearsome Pb Lα↔As Kα binaries, while “cascade” interferences are often seen among the transition metal series as in Ti Kβ → V Kα - V Kα Cr Kα or as seen with a secondary fluorescence interference effect as in Ni K ⇒ Fe Kα - Fe Kβ → Co Kα. Unlike simple interferences of the type Mn Kβ → Fe Kα, both of these types of spectral interferences are often quite troublesome for the analyst to correct for, especially for Si(Li) and Ge energy dispersive spectrometers (EDS) where the analytical peaks are often so overlapped as to prevent graphical deconvolution, and even for the higher resolution wavelength dispersive spectrometers (WDS) along with the yet to come bolometric energy dispersive detectors (based on projected resolution), the task can still be formidable.


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