A new method for quantitative analysis of EELS

Author(s):  
Suichu Luo ◽  
David C. Joy

Techniques to remove plural scattering from electron energy loss spectra (EELS) are important in bot hmicroanalysis and other quantitative applications of electron spectroscopy. The techniques used are either based on convolution, or Fourier transform deconvolution, methods, in which either the elastic scattering angular correction or both elastic and inelastic angular corrections are not included. In this work we propose a new method based on both angular and energy loss three-dimension Poisson statistics which includes elastic and inelastic mixed angular scattering correction in order to obtain more accurate quantitative analysis for EELS.The electron scattering distribution determined by angular and energy loss three-dimension Poissonstatistics is given by:where IT is the total incident electron intensity; t is the sample thickness; λi, λe and λT are inelastic , elastic and total scattering mean free paths; Si (θ) and Se(θ) are normalized single inelastic and elastic angular scattering distributions respectively, F(E) is the single scattering normalized energy loss distribution.

Author(s):  
Suichu Luo ◽  
John R. Dunlap ◽  
Richard W. Williams ◽  
David C. Joy

In analytical electron microscopy, it is often important to know the local thickness of a sample. The conventional method used for measuring specimen thickness by EELS is:where t is the specimen thickness, λi is the total inelastic mean free path, IT is the total intensity in an EEL spectrum, and I0 is the zero loss peak intensity. This is rigorouslycorrect only if the electrons are collected over all scattering angles and all energy losses. However, in most experiments only a fraction of the scattered electrons are collected due to a limited collection semi-angle. To overcome this problem we present a method based on three-dimension Poisson statistics, which takes into account both the inelastic and elastic mixed angular correction.The three-dimension Poisson formula is given by:where I is the unscattered electron intensity; t is the sample thickness; λi and λe are the inelastic and elastic scattering mean free paths; Si (θ) and Se(θ) are normalized single inelastic and elastic angular scattering distributions respectively ; F(E) is the single scattering normalized energy loss distribution; D(E,θ) is the plural scattering distribution,


Author(s):  
L. Reimer ◽  
R. Oelgeklaus

Quantitative electron energy-loss spectroscopy (EELS) needs a correction for the limited collection aperture α and a deconvolution of recorded spectra for eliminating the influence of multiple inelastic scattering. Reversely, it is of interest to calculate the influence of multiple scattering on EELS. The distribution f(w,θ,z) of scattered electrons as a function of energy loss w, scattering angle θ and reduced specimen thickness z=t/Λ (Λ=total mean-free-path) can either be recorded by angular-resolved EELS or calculated by a convolution of a normalized single-scattering function ϕ(w,θ). For rotational symmetry in angle (amorphous or polycrystalline specimens) this can be realised by the following sequence of operations :(1)where the two-dimensional distribution in angle is reduced to a one-dimensional function by a projection P, T is a two-dimensional Fourier transform in angle θ and energy loss w and the exponent -1 indicates a deprojection and inverse Fourier transform, respectively.


Author(s):  
M. Isaacson

In an earlier paper1 it was found that to a good approximation, the efficiency of collection of electrons that had lost energy due to an inner shell excitation could be written as where σE was the total excitation cross-section and σE(θ, Δ) was the integral cross-section for scattering within an angle θ and with an energy loss up to an energy Δ from the excitation edge, EE. We then obtained: where , with P being the momentum of the incident electron of velocity v. The parameter r was due to the assumption that d2σ/dEdΩ∞E−r for energy loss E. In reference 1 it was assumed that r was a constant.


Author(s):  
G. Zanchi ◽  
Y. Kihn ◽  
J. Sévely

The electron energy loss spectra can be considered as the result of the convolution of elementary inelastic scattering processes (1, 2). We have developed a procedure which allows to write the intensity of the spectrum as a function of the energy loss.These calculations take the electron angular scattering into account.The probability for an electron to suffer an energy loss E and to be deviated through an angle after a single electron-electron interaction of any kind is given by a normalized function D(E, ), which can be written with a good approximation as a product of two functions g(E) and f(), separately normalized. Assuming that the excitation probabilities of any interaction follows a Poisson distribution, for a collection angle θd the intensity of the spectrum can be written in the Fourier space :Gs(ω) is the Fourier transform of GS(E) which characterizes the transfer function of the experimental device.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Lihao Yang ◽  
Bo Da ◽  
Károly Tőkési ◽  
Z. J. Ding

AbstractWe present the first theoretical recipe for the clear and individual separation of surface, bulk and Begrenzungs effect components in surface electron energy spectra. The procedure ends up with the spectral contributions originated from surface and bulk-Begrenzungs excitations by using a simple method for dealing with the mixed scatterings. As an example, the model is applied to the reflection electron energy loss spectroscopy spectrum of Si. The electron spectroscopy techniques can directly use the present calculation schema to identify the origin of the electron signals from a sample. Our model provides the possibility for the detailed and accurate quantitative analysis of REELS spectra.


Author(s):  
V. V. Damiano ◽  
R. P. Daniele ◽  
H. T. Tucker ◽  
J. H. Dauber

An important example of intracellular particles is encountered in silicosis where alveolar macrophages ingest inspired silica particles. The quantitation of the silica uptake by these cells may be a potentially useful method for monitoring silica exposure. Accurate quantitative analysis of ingested silica by phagocytic cells is difficult because the particles are frequently small, irregularly shaped and cannot be visualized within the cells. Semiquantitative methods which make use of particles of known size, shape and composition as calibration standards may be the most direct and simplest approach to undertake. The present paper describes an empirical method in which glass microspheres were used as a model to show how the ratio of the silicon Kα peak X-ray intensity from the microspheres to that of a bulk sample of the same composition correlated to the mass of the microsphere contained within the cell. Irregular shaped silica particles were also analyzed and a calibration curve was generated from these data.


Author(s):  
C P Scott ◽  
A J Craven ◽  
C J Gilmore ◽  
A W Bowen

The normal method of background subtraction in quantitative EELS analysis involves fitting an expression of the form I=AE-r to an energy window preceding the edge of interest; E is energy loss, A and r are fitting parameters. The calculated fit is then extrapolated under the edge, allowing the required signal to be extracted. In the case where the characteristic energy loss is small (E < 100eV), the background does not approximate to this simple form. One cause of this is multiple scattering. Even if the effects of multiple scattering are removed by deconvolution, it is not clear that the background from the recovered single scattering distribution follows this simple form, and, in any case, deconvolution can introduce artefacts.The above difficulties are particularly severe in the case of Al-Li alloys, where the Li K edge at ~52eV overlaps the Al L2,3 edge at ~72eV, and sharp plasmon peaks occur at intervals of ~15eV in the low loss region. An alternative background fitting technique, based on the work of Zanchi et al, has been tested on spectra taken from pure Al films, with a view to extending the analysis to Al-Li alloys.


Author(s):  
John C. Russ

Monte-Carlo programs are well recognized for their ability to model electron beam interactions with samples, and to incorporate boundary conditions such as compositional or surface variations which are difficult to handle analytically. This success has been especially powerful for modelling X-ray emission and the backscattering of high energy electrons. Secondary electron emission has proven to be somewhat more difficult, since the diffusion of the generated secondaries to the surface is strongly geometry dependent, and requires analytical calculations as well as material parameters. Modelling of secondary electron yield within a Monte-Carlo framework has been done using multiple scattering programs, but is not readily adapted to the moderately complex geometries associated with samples such as microelectronic devices, etc.This paper reports results using a different approach in which simplifying assumptions are made to permit direct and easy estimation of the secondary electron signal from samples of arbitrary complexity. The single-scattering program which performs the basic Monte-Carlo simulation (and is also used for backscattered electron and EBIC simulation) allows multiple regions to be defined within the sample, each with boundaries formed by a polygon of any number of sides. Each region may be given any elemental composition in atomic percent. In addition to the regions comprising the primary structure of the sample, a series of thin regions are defined along the surface(s) in which the total energy loss of the primary electrons is summed. This energy loss is assumed to be proportional to the generated secondary electron signal which would be emitted from the sample. The only adjustable variable is the thickness of the region, which plays the same role as the mean free path of the secondary electrons in an analytical calculation. This is treated as an empirical factor, similar in many respects to the λ and ε parameters in the Joy model.


Author(s):  
Nestor J. Zaluzec

The application of electron energy loss spectroscopy (EELS) to light element analysis is rapidly becoming an important aspect of the microcharacterization of solids in materials science, however relatively stringent requirements exist on the specimen thickness under which one can obtain EELS data due to the adverse effects of multiple inelastic scattering.1,2 This study was initiated to determine the limitations on quantitative analysis of EELS data due to specimen thickness.


Author(s):  
Fox T. R. ◽  
R. Levi-Setti

At an earlier meeting [1], we discussed information retrieval in the scanning transmission ion microscope (STIM) compared with the electron microscope at the same energy. We treated elastic scattering contrast, using total elastic cross sections; relative damage was estimated from energy loss data. This treatment is valid for “thin” specimens, where the incident particles suffer only single scattering. Since proton cross sections exceed electron cross sections, a given specimen (e.g., 1 μg/cm2 of carbon at 25 keV) may be thin for electrons but “thick” for protons. Therefore, we now extend our previous analysis to include multiple scattering. Our proton results are based on the calculations of Sigmund and Winterbon [2], for 25 keV protons on carbon, using a Thomas-Fermi screened potential with a screening length of 0.0226 nm. The electron results are from Crewe and Groves [3] at 30 keV.


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