Low-Voltage Electron-Probe Microanalysis of Fe–Si Compounds Using Soft X-Rays

2013 ◽  
Vol 19 (6) ◽  
pp. 1698-1708 ◽  
Author(s):  
Phillip Gopon ◽  
John Fournelle ◽  
Peter E. Sobol ◽  
Xavier Llovet
Keyword(s):  
Electron Probe Microanalysis ◽  
Electron Probe ◽  
Low Voltage ◽  
Mass Attenuation Coefficient ◽  
X Rays ◽  
X Ray ◽  
Voltage Electron ◽  
Increased Sensitivity ◽  
Quantitative Analyses ◽  
Areas Of Interest

AbstractConventional electron-probe microanalysis has an X-ray analytical spatial resolution on the order of 1–4 μm width/depth. Many of the naturally occurring Fe–Si compounds analyzed in this study are smaller than 1 μm in size, requiring the use of lower accelerating potentials and nonstandard X-ray lines for analysis. Problems with the use of low-energy X-ray lines (soft X-rays) of iron for quantitative analyses are discussed and a review is given of the alternative X-ray lines that may be used for iron at or below 5 keV (i.e., accelerating voltage that allows analysis of areas of interest <1 μm). Problems include increased sensitivity to surface effects for soft X-rays, peak shifts (induced by chemical bonding, differential self-absorption, and/or buildup of carbon contamination), uncertainties in the mass attenuation coefficient for X-ray lines near absorption edges, and issues with spectral resolution and count rates from the available Bragg diffractors. In addition to the results from the traditionally used Fe Lα line, alternative approaches, utilizing Fe Lβ, and Fe Ll-η lines, are discussed.

Thermal Effects During Low-Voltage Electron-Probe X-Ray Spectral Microanalysis with Nanometer Localization

2017 ◽  
Vol 59 (10) ◽  
pp. 1061-1064 ◽  
Author(s):  
A. Yu. Kuzin ◽  
M. A. Stepovich ◽  
V. B. Mityukhlyaev ◽  
P. A. Todua ◽  
M. N. Filippov
Keyword(s):  
Thermal Effects ◽  
Electron Probe ◽  
Low Voltage ◽  
X Ray ◽  
Voltage Electron

Monte Carlo Simulation of Characteristic Secondary Fluorescence in Electron Probe Microanalysis of Homogeneous Samples Using the Splitting Technique

2015 ◽  
Vol 21 (3) ◽  
pp. 753-758 ◽  
Author(s):  
Mauricio Petaccia ◽  
Silvina Segui ◽  
Gustavo Castellano
Keyword(s):  
Monte Carlo Simulation ◽  
Monte Carlo ◽  
Electron Probe Microanalysis ◽  
Electron Probe ◽  
Variance Reduction ◽  
Fluorescence Enhancement ◽  
Radiation Transport ◽  
X Rays ◽  
X Ray ◽  
Secondary Fluorescence

AbstractElectron probe microanalysis (EPMA) is based on the comparison of characteristic intensities induced by monoenergetic electrons. When the electron beam ionizes inner atomic shells and these ionizations cause the emission of characteristic X-rays, secondary fluorescence can occur, originating from ionizations induced by X-ray photons produced by the primary electron interactions. As detectors are unable to distinguish the origin of these characteristic X-rays, Monte Carlo simulation of radiation transport becomes a determinant tool in the study of this fluorescence enhancement. In this work, characteristic secondary fluorescence enhancement in EPMA has been studied by using the splitting routines offered by PENELOPE 2008 as a variance reduction alternative. This approach is controlled by a single parameter NSPLIT, which represents the desired number of X-ray photon replicas. The dependence of the uncertainties associated with secondary intensities on NSPLIT was studied as a function of the accelerating voltage and the sample composition in a simple binary alloy in which this effect becomes relevant. The achieved efficiencies for the simulated secondary intensities bear a remarkable improvement when increasing the NSPLIT parameter; although in most cases an NSPLIT value of 100 is sufficient, some less likely enhancements may require stronger splitting in order to increase the efficiency associated with the simulation of secondary intensities.

Absorption Correction Curves Obtained from Measurements of the Production of X-Rays as a Function of Depth

1972 ◽  
Vol 16 ◽  
pp. 198-205
Author(s):  
J.D. Brown ◽  
L. Parobek
Keyword(s):  
Electron Probe Microanalysis ◽  
Electron Probe ◽  
X Rays ◽  
Matrix Elements ◽  
X Ray ◽  
Absorption Correction ◽  
Correction Equations

AbstractMeasurements of x-ray production as a function of depth in a sample (ϕ(ρz) curves) are fundamental to the determination of the quantitative equations for relating x-ray intensity to composition in electron probe microanalysis. These ϕ(ρz) curves have been measured for four different voltages and a number of different tracers in aluminum, copper, silver arid gold as matrix elements. From these ϕ(ρz) curves the absorption correction curves (f(x) curves) can be calculated. Such curves have been obtained and comparison is made with the absorption correction equations of Philibert. The effect of a tilted sample on the absorption correction is also discussed.

Change in the Chemical Composition of an Analyzed Object During Low-Voltage Electron Probe X-Ray Spectral Microanalysis

2017 ◽  
Vol 59 (11) ◽  
pp. 1234-1237
Author(s):  
A. Yu. Kuzin ◽  
V. B. Mityukhlyaev ◽  
P. A. Todua ◽  
M. N. Filippov
Keyword(s):  
Chemical Composition ◽  
Electron Probe ◽  
Low Voltage ◽  
X Ray ◽  
Voltage Electron

scholarly journals A Model for Characteristic X-Ray Emission in Electron Probe Microanalysis based on the Spherical Harmonic (PN) Method for Electron Transport

2021 ◽  
Author(s):  
Jonas Buenger ◽  
Silvia Richter ◽  
Manuel Torrilhon
Keyword(s):  
Monte Carlo ◽  
Electron Transport ◽  
Electron Probe Microanalysis ◽  
Spherical Harmonic ◽  
Electron Probe ◽  
Material Structure ◽  
X Rays ◽  
Minimum Entropy ◽  
Promising Alternative ◽  
X Ray

Classical k-ratio models, e.g. ZAF and phi(rho z), used in electron probe microanalysis (EPMA) assume a homogeneous or multi-layered material structure, which essentially limits the spatial resolution of EPMA to the size of the interaction volume where characteristic x-rays are produced. We present a new model for characteristic x-ray emission that avoids assumptions on the material structure to not restrict the resolution of EPMA a-priori. Our model bases on the spherical harmonic (PN) approximation of the Boltzmann equation for electron transport in continuous slowing down approximation. PN models have a simple structure, are hierarchical in accuracy and well-suited for efficient adjoint-based gradient computation, which makes our model a promising alternative to classical models in terms of improving the resolution of EPMA in the future. We present results of various test cases including a comparison of the PN model to a minimum entropy moment model as well as Monte-Carlo (MC) trajectory sampling, a comparison of PN-based k-ratios to k-ratios obtained with MC, a comparison with experimental data of electron backscattering yields as well as a comparison of PN and Monte-Carlo based on characteristic X-ray generation in a three-dimensional material probe with fine structures.

Quantitative Electron Probe Microanalysis of Nonconducting Specimens: Science or Art?

2004 ◽  
Vol 10 (6) ◽  
pp. 733-738 ◽  
Author(s):  
Guillaume F. Bastin ◽  
Hans J.M. Heijligers
Keyword(s):  
Electrical Conductivity ◽  
Electron Probe Microanalysis ◽  
Electron Probe ◽  
Light Element ◽  
X Ray ◽  
Surface Charging ◽  
Quantitative Electron Probe Microanalysis ◽  
Quantitative Analyses ◽  
Intensity Ratios ◽  
Effect Of Surface

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.

Electron Probe Microanalysis Through Coated Oxidized Surfaces

2019 ◽  
Vol 25 (05) ◽  
pp. 1112-1129 ◽  
Author(s):  
Mike B. Matthews ◽  
Ben Buse ◽  
Stuart L. Kearns
Keyword(s):  
Electron Probe Microanalysis ◽  
Electron Probe ◽  
Low Voltage ◽  
Layer Structure ◽  
Oxide Thickness ◽  
Linear Functions ◽  
Voltage Electron ◽  
Before And After ◽  
20 Nm ◽  
Good Agreement

AbstractLow voltage electron probe microanalysis (EPMA) of metals can be complicated by the presence of a surface oxide. If a conductive coating is applied, analysis becomes one of a three-layer structure. A method is presented which allows for the coating and oxide thicknesses and the substrate intensities to be determined. By restricting the range of coating and oxide thicknesses, tc and to respectively, x-ray intensities can be parameterized using a combination of linear functions of tc and to. tc can be determined from the coating element k-ratio independently of the oxide thickness. to can then be derived from the O k-ratio and tc. From tc and to the intensity components of the k-ratios from the oxide layer and substrate can each be derived. Modeled results are presented for an Ag on Bi2O3 on Bi system, with tc and to each ranging from 5 to 20 nm, for voltages of 5–20 kV. The method is tested against experimental measurements of Ag- or C-coated samples of polished Bi samples which have been allowed to naturally oxidize. Oxide thicknesses determined both before and after coating with Ag or C are consistent. Predicted Bi Mα k-ratios also show good agreement with EPMA-measured values.

Characteristic and Continuum Fluorescence in Electron Beam X-ray Microanalysis

1999 ◽  
Vol 5 (S2) ◽  
pp. 562-563
Author(s):  
C.E. Nockolds
Keyword(s):  
Electron Beam ◽  
Electron Probe Microanalysis ◽  
Electron Probe ◽  
Mathematical Framework ◽  
X Rays ◽  
Correction Procedure ◽  
X Ray ◽  
Exponential Term ◽  
Accurate Expression ◽  
Original Formula

Of the different aspects of electron probe microanalysis(EPMA)which were studied by Castaing during his doctorate the work on characteristic x-ray fluorescence was the most definitive. In his thesis, which was completed in 1951, Castaing established the physical and mathematical framework for a correction procedure for fluorescence which is essentially still used in EPMA today. Much of the effort since then has been in refining and improving the accuracy of the correction and extending the scope of the correction to a wider range of specimen types. The Castaing formula was developed for the case of a K x-ray from element A being excited by a K xray from element B (K-K fluorescence) and in 1965 Reed extended the range of the correction by including the K-L, L-L and L-K interactions. In the same paper Reed also introduced the expression from Green and Cosslett for the calculation of K intensities, which was believed to be more accurate than the expression used by Castaing. The original formula included a somewhat unrealistic exponential term to allow for the depth of the production of the primary x-rays and a number of workers have tried replacing this term with a more accurate expression, however, in general this has led to only small changes in the final correction. Reed also simplified the formula in order to make the calculation easier in the days before fast computers; in particular he replaced the jump ratio variable by two constants, one for the K-shell and one for the L-shell. Much later Heinrich showed that this simplification was no longer necessary and that the jump ratio could in fact be calculated directly.

Improving the Analtical Accuracy in the Analysis of Particles by Employing Low Voltage Analysis:

2000 ◽  
Vol 6 (S2) ◽  
pp. 924-925
Author(s):  
JA Small ◽  
JT Armstrong
Keyword(s):  
Electron Beam ◽  
Electron Probe ◽  
Low Voltage ◽  
X Rays ◽  
Relative Uncertainty ◽  
Particle Volume ◽  
X Ray ◽  
Uncertainty Estimates ◽  
Corrected Data ◽  
Particle Geometry

The energy of the electron beam, in conventional electron probe microanalysis, is generally in the range of 15-25 keV which provides the necessary overvoltage to excite efficiently the K and L x-ray lines for elements with atomic numbers in the range of about 5-83. One of the primary microanalytical methods for obtaining compositional information on particles is X-ray analysis in the electron probe and these same voltage criteria have been applied to the procedures developed for this purpose. The main difference in analytical procedures for bulk samples and particles is that corrections have to be applied to the particle k-ratios or calculated compositions to compensate for: 1) the penetration or scattering of electrons out of the particle volume and 2) variations in the absorption due to particle geometry of x-rays less than about 3 keV. In general, particle corrections improve the accuracy and reduce the relative uncertainty estimates from several tens of percent for uncorrected data to about 10% for corrected data.

Celebrating 40 Years of Energy Dispersive X-Ray Spectrometry in Electron Probe Microanalysis: A Historic and Nostalgic Look Back into the Beginnings

2009 ◽  
Vol 15 (6) ◽  
pp. 476-483 ◽  
Author(s):  
Klaus Keil ◽  
Ray Fitzgerald ◽  
Kurt F.J. Heinrich
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Electron Probe Microanalysis ◽  
Electron Probe ◽  
Energy Dispersive Spectrometer ◽  
Fluorescence Analysis ◽  
Energy Dispersive ◽  
X Rays ◽  
New Era ◽  
X Ray

AbstractOn February 2, 1968, R. Fitzgerald, K. Keil, and K.F.J. Heinrich published a seminal paper in Science (159, 528–530) in which they described a solid-state Si(Li) energy dispersive spectrometer (EDS) for electron probe microanalysis (EPMA) with, initially, a resolution of 600 eV. This resolution was much improved over previous attempts to use either gas-filled proportional counters or solid-state devices for EDS to detect X-rays and was sufficient, for the first time, to make EDS a practically useful technique. It ushered in a new era not only in EPMA, but also in scanning electron microscopy, analytical transmission electron microscopy, X-ray fluorescence analysis, and X-ray diffraction. EDS offers many advantages over wavelength-dispersive crystal spectrometers, e.g., it has no moving parts, covers the entire X-ray energy range of interest to EPMA, there is no defocusing over relatively large distances across the sample, and, of particular interest to those who analyze complex minerals consisting of many elements, all X-ray lines are detected quickly and simultaneously.

Sign in / Sign up

Export Citation Format

Share Document