scholarly journals Low-Voltage Electron-Probe Microanalysis of Uranium

2021 ◽  
pp. 1-18
Author(s):  
Mike B. Matthews ◽  
Stuart L. Kearns ◽  
Ben Buse

Abstract

2013 ◽  
Vol 19 (6) ◽  
pp. 1698-1708 ◽  
Author(s):  
Phillip Gopon ◽  
John Fournelle ◽  
Peter E. Sobol ◽  
Xavier Llovet

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.


2019 ◽  
Vol 25 (05) ◽  
pp. 1112-1129 ◽  
Author(s):  
Mike B. Matthews ◽  
Ben Buse ◽  
Stuart L. Kearns

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.


2017 ◽  
Vol 59 (10) ◽  
pp. 1061-1064 ◽  
Author(s):  
A. Yu. Kuzin ◽  
M. A. Stepovich ◽  
V. B. Mityukhlyaev ◽  
P. A. Todua ◽  
M. N. Filippov

2017 ◽  
Vol 59 (11) ◽  
pp. 1234-1237
Author(s):  
A. Yu. Kuzin ◽  
V. B. Mityukhlyaev ◽  
P. A. Todua ◽  
M. N. Filippov

Author(s):  
E. Heikinheimo ◽  
P.T. Pinard ◽  
S. Richter ◽  
X. Llovet ◽  
S. Louhenkilpi

2014 ◽  
Vol 78 (9) ◽  
pp. 821-825 ◽  
Author(s):  
V. V. Kazmiruk ◽  
I. G. Kurganov ◽  
T. N. Savitskaya

Author(s):  
Claude Lechene

Electron probe microanalysis of frozen hydrated kidneysThe goal of the method is to measure on the same preparation the chemical elemental content of the renal luminal tubular fluid and of the surrounding renal tubular cells. The following method has been developed. Rat kidneys are quenched in solid nitrogen. They are trimmed under liquid nitrogen and mounted in a copper holder using a conductive medium. Under liquid nitrogen, a flat surface is exposed by sawing with a diamond saw blade at constant speed and constant pressure using a custom-built cryosaw. Transfer into the electron probe column (Cameca, MBX) is made using a simple transfer device maintaining the sample under liquid nitrogen in an interlock chamber mounted on the electron probe column. After the liquid nitrogen is evaporated by creating a vacuum, the sample is pushed into the special stage of the instrument. The sample is maintained at close to liquid nitrogen temperature by circulation of liquid nitrogen in the special stage.


Author(s):  
Huang Min ◽  
P.S. Flora ◽  
C.J. Harland ◽  
J.A. Venables

A cylindrical mirror analyser (CMA) has been built with a parallel recording detection system. It is being used for angular resolved electron spectroscopy (ARES) within a SEM. The CMA has been optimised for imaging applications; the inner cylinder contains a magnetically focused and scanned, 30kV, SEM electron-optical column. The CMA has a large inner radius (50.8mm) and a large collection solid angle (Ω > 1sterad). An energy resolution (ΔE/E) of 1-2% has been achieved. The design and performance of the combination SEM/CMA instrument has been described previously and the CMA and detector system has been used for low voltage electron spectroscopy. Here we discuss the use of the CMA for ARES and present some preliminary results.The CMA has been designed for an axis-to-ring focus and uses an annular type detector. This detector consists of a channel-plate/YAG/mirror assembly which is optically coupled to either a photomultiplier for spectroscopy or a TV camera for parallel detection.


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