Operating Conditions For Quantitative X-Ray Analysis In The Environmental SEM

1998 ◽  
Vol 4 (S2) ◽  
pp. 294-295
Author(s):  
R. A. Carlton ◽  
C. E. Lyman ◽  
J. E. Roberts
Keyword(s):  
Electron Beam ◽  
Target Location ◽  
Primary Electron ◽  
Operating Conditions ◽  
Environmental Scanning ◽  
X Rays ◽  
X Ray ◽  
Sample Chamber ◽  
Low Pressures ◽  
Environmental Sem

Standard Reference Material (SRM) 482 of the National Institute of Standards and Technology is a set of 6 gold/copper wires, ranging in concentration from 0 to 100% Cu in 20% steps, intended for calibration studies of electron beam microanalyzers. This is an appropriate standard to test the accuracy of energy dispersive x-ray spectrometry (EDS) in the Environmental Scanning Electron Microscope (ESEM). While the presence of the gas in the sample chamber gives the ESEM its unique capabilities, it also is the source of complications to x-ray spectrometry. The gas can spread the primary electron beam into a wide skirt of electrons with the consequent production of x-rays many micrometers from the target location of the beam. In spite of the difficulties, at least two methods have been proposed to correct high pressure data to that expected at low pressures.

Factors Affecting Quantitative Analysis Error in ESEM-EDS

2000 ◽  
Vol 6 (S2) ◽  
pp. 790-791
Author(s):  
R. A. Carlton ◽  
C. E. Lyman ◽  
J. E. Roberts
Keyword(s):  
Electron Beam ◽  
Target Location ◽  
Primary Electron ◽  
Environmental Scanning ◽  
X Rays ◽  
Factors Affecting ◽  
X Ray ◽  
Carbon Coated ◽  
Sample Chamber ◽  
Analysis Error

Standard Reference Material (SRM) 482 of the National Institute of Standards and Technology is a set of 6 gold/copper wires, ranging in concentration from 0 to 100% Cu in 20% steps, intended for calibration studies of electron beam microanalyzers. This is an appropriate standard to test the accuracy of energy dispersive x-ray spectrometry (EDS) in the Environmental Scanning Electron Microscope (ESEM). While the presence of the gas in the sample chamber gives the ESEM its unique capabilities, it also is the source of complications to x-ray spectrometry. The gas can spread the primary electron beam into a wide skirt of electrons with the consequent production of x-rays many micrometers from the target location of the beam.The six wires (∼ 500 jam in diameter) were embedded and polished in one epoxy mount. The mount was carbon coated in one set of experiments. The coating was removed and the sample retested.

X-Ray Energy Dispersive Spectroscopy in the Environmental Scanning Electron Microscope

1998 ◽  
Vol 4 (S2) ◽  
pp. 182-183
Author(s):  
John F. Mansfield ◽  
Brett L. Pennington
Keyword(s):  
Electron Beam ◽  
Electron Microscope ◽  
Scanning Electron Microscope ◽  
Energy Dispersive Spectroscopy ◽  
Primary Electron ◽  
Environmental Scanning ◽  
Primary Electron Beam ◽  
X Ray ◽  
Environmental Sem ◽  
Scanning Electron

The environmental scanning electron microscope (Environmental SEM) has proved to be a powerful tool in both materials science and the life sciences. Full characterization of materials in the environmental SEM often requires chemical analysis by X-ray energy dispersive spectroscopy (XEDS). However, the spatial resolution of the XEDS signal can be severely degraded by the gaseous environment in the sample chamber. At an operating pressure of 5Torr a significant fraction of the primary electron beam is scattered after it passes through the final pressure limiting aperture and before it strikes the sample. Bolon and Griffin have both published data that illustrates this effect very well. Bolon revealed that 45% of the primary electron beam was scattered by more than 25 μm in an Environmental SEM operating at an accelerating voltage of 30kV, with a water vapor pressure of 3Torr and a working distance of 15mm.

scholarly journals X-ray Analysis in the Low Vacuum SEM (Part 3 of 3)

1998 ◽  
Vol 6 (10) ◽  
pp. 10-13
Author(s):  
Don Chernoff
Keyword(s):  
Electron Beam ◽  
Path Length ◽  
Experimental Methods ◽  
Gas Pressure ◽  
Operating Conditions ◽  
X Rays ◽  
X Ray ◽  
Software Models ◽  
Working Distance ◽  
Low Vacuum Sem

In this third and final installment on x-ray analysis in the environmental and low vacuum SEM, I will present experimental methods for measuring beam scatter. In my previous two articles I discussed how operating conditions detemine beam scatter. It was shown that the type of gas used, the gas pressure in the chamber, the working distance or beam gas path length, and the accelerating voltage all have an effect on how much the electron beam scatters. I also discussed how the beam scatter influences x-ray results by producing x-rays beyond the area of the primary beam. Furthermore, I showed how software models could be used to determine the amount of beam scatter based on different combinations of the four variables (pressure, gas, working distance, and kV).

Review of Techniques for Overcoming XEDS Problems in the Environmental Scanning Electron Microscope

1997 ◽  
Vol 3 (S2) ◽  
pp. 1207-1208
Author(s):  
John Mansfield
Keyword(s):  
Electron Beam ◽  
Electron Microscope ◽  
Scanning Electron Microscope ◽  
Primary Electron ◽  
Environmental Scanning Electron Microscope ◽  
Significant Fraction ◽  
Environmental Scanning ◽  
Primary Electron Beam ◽  
Environmental Sem ◽  
Scanning Electron

Full characterization of materials in the environmental scanning electron microscope (Environmental SEM) often requires chemical analysis by X-ray energy dispersive spectroscopy (XEDS). However, a major problem arises because the spatial resolution of the XEDS signal is severely degraded by the gaseous environment in the sample chamber. The significant fraction of the primary electron beam is scattered after it passes through the final pressure limiting aperture and before it strikes the sample. Bolon and Griffin have both published data that illustrates this effect very well. Bolon revealed that 45% of the primary electron beam was scattered by more than 25μm in an Environmental SEM operating at an accelerating voltage of 30kV, with a water vapor pressure of 3Torr and a working distance of 15mm. Griffin’s work demonstrated that even at higher voltages (30 kV), shorter working distances (<10mm) and lower chamber pressures (2Torr), there is a significant fraction of the electron beam scattered out to over 400 μm away from the point where the primary beam strikes the sample.

Effects of chamber pressure and accelerating voltage on X-RAY resolution in the ESEM

1992 ◽  
Vol 50 (2) ◽  
pp. 1324-1325 ◽  
Author(s):  
Brendon J. Griffin
Keyword(s):  
Electron Beam ◽  
Primary Electron ◽  
Chamber Pressure ◽  
X Rays ◽  
Viewing Angle ◽  
Primary Electron Beam ◽  
Specific Data ◽  
X Ray ◽  
Working Distance ◽  
Eds Microanalysis

Chamber pressure, accelerating voltage and working distance have been shown to control the relative diameter of the scattered skirt of the primary electron beam at the specimen surface in the ESEM. Inital x-ray studies indicate that at 3 torr, 30 kV and a WD=15mm, 45% of the beam comes from beyond 25 μm of the incidence point and 4% from beyond 1.5mm. At 5 torr 66% of the beam is scattered beyond 25 μm2. No specific data was available on the spatial resolution of x rays and this study aimed to improve that situation. The results also form the basis for establishing a mechanism for and defining the potential limits of quantitative EDS microanalysis in the ESEM.The negative viewing angle of the EDS x-ray detector in the current ESEM (model E-3) requires at least a 15 degree tilt on a flat sample for microanalysis. This geometry places a narrow limit on the working distance range that can be used, due to the collimation of the detector, thereby effectively eliminating working distance as a variable in x-ray microanalysis.

Charge-Related Problems Associated with X-Ray Microanalysis in the Variable Pressure Scanning Electron Microscope at Low Pressures

2003 ◽  
Vol 9 (2) ◽  
pp. 155-165 ◽  
Author(s):  
Brendan J. Griffin ◽  
Alexandra A. Suvorova
Keyword(s):  
Primary Electron ◽  
Current Data ◽  
Operating Conditions ◽  
Variable Pressure ◽  
Charge Effects ◽  
X Ray ◽  
Sample Characteristics ◽  
Low Pressures ◽  
Chamber Gas ◽  
Scanning Electron

In variable pressure scanning electron microscopy (VPSEM) the current data suggests that considerable caution is required in the interpretation of X-ray data from nonconductive samples, depending on the operating conditions. This article reviews some of the documented approaches and presents data that illustrate the nature and magnitude of the effects of charge above, on, and in the sample on the detected X-ray emissions from the sample and from elsewhere within the VPSEM specimen chamber. The collection of reliable and reproducible X-ray data has been found to require relatively high specimen chamber gas pressures, at the upper end of or beyond the available pressures for most VPSEMs. It is also shown that sample characteristics, including composition, strongly influence local charge effects, which can significantly affect the primary electron landing energy and consequently the resultant emitted X-ray signal under low pressure environments.

Phosphor Imaging Plate Measurement of Electron Scattering in the Environmental Scanning Electron Micrsoscope

2000 ◽  
Vol 6 (S2) ◽  
pp. 798-799
Author(s):  
S.A. Wight ◽  
C.J. Zeissler
Keyword(s):  
Electron Beam ◽  
Direct Measurement ◽  
Electron Scattering ◽  
Measurement Data ◽  
Primary Electron ◽  
Environmental Scanning ◽  
Imaging Plate ◽  
X Rays ◽  
Primary Electron Beam ◽  
Scanning Electron

In this work, phosphor imaging plate technology is applied to measure electron scattering directly in the environmental scanning electron microscope (ESEM) specimen chamber. The scattering of electrons from the primary electron beam, under relatively high-pressure conditions (266 Pa) in the ESEM sample chamber, degrades the analytical accuracy of elemental analysis. The degree of this degradation is poorly known. To date, attempts to measure experimentally the spatial distribution of the scattered electrons have been limited to observing secondary effects such as the intensity of x-rays produced from copper targets positioned at various distances from the primary electron beam interaction point. A more accurate distribution of the scattered electron intensity can be obtained from a direct measurement of both the scattered and unscattered electrons over a large area with single electron sensitivity. Improvements to the accuracy of Monte Carlo models of the scattering process will be made possible by the direct measurement data.

The measurement of the fluorescence of Si K x-rays by Au M x-rays

1990 ◽  
Vol 48 (2) ◽  
pp. 198-199
Author(s):  
John A. Small ◽  
Scott A. Wight ◽  
Robert L. Myklebust ◽  
Dale E. Newbury
Keyword(s):  
Electron Beam ◽  
Electron Probe ◽  
Primary Electron ◽  
Characteristic Line ◽  
X Rays ◽  
Limited Information ◽  
Primary Electron Beam ◽  
X Ray ◽  
Image Position ◽  
Critical Excitation

The characteristic fluorescence correction is used in electron probe microanalysis to account for the x-ray intensity excited in element “a” by the x-rays from the characteristic line of another element, “b”, in the sample. Since the excited intensity is not generated by the primary electron beam, it is necessary to apply the fluorescence correction for quantitative elemental analysis. This correction can be significant particularly when element “b” is a major component of the sample and the characteristic line for element “b” is slightly higher in energy than the critical excitation energy for the excited line of element “a”.The fluorescence correction, which is used in the various analytical programs, is described in equation 1.where I'*fa/I'*pa is the ratio of the emitted “a” intensity excited by “b” x-rays to the emitted intensity excited by the primary electron beam. The various parameters in this equation are accurately known for the K x-ray lines, but only very limited information is available for the M x-ray lines.

scholarly journals FORMATION AND MONITORING OF SECONDARY X-RAY RADIATION UNDER PRODUCT PROCESSING WITH ELECTRON BEAM

2021 ◽  
pp. 201-205
Author(s):  
R.I. Pomatsalyuk ◽  
V.A. Shevchenko ◽  
D.V. Titov ◽  
A.Eh. Tenishev ◽  
V.L. Uvarov ◽  
...  
Keyword(s):  
Electron Beam ◽  
Primary Electron ◽  
X Rays ◽  
Bremsstrahlung Radiation ◽  
X Ray ◽  
Free Air ◽  
Industrial Radiation ◽  
Radiation Processes ◽  
Cultural Heritage Objects ◽  
Electron And Photon

When conducting an industrial radiation processes at an electron accelerator, a part of the beam energy is trans-formed into bremsstrahlung radiation. In such a way, the mixed e,X-radiation is formed in the area behind an irra-diated object. The intensity of the electron and photon components in the radiation is determined by the energy and power of the primary electron beam, as well as by the parameters of the object and devices located behind it. In paper, the characteristics of the e,X-radiation accompanying the product processing by a scanning electron beam with energy 8…12 MeV at a LU-10 Linac of NSC KIPT are studied. The conditions for obtaining a source of sec-ondary X-rays in the state of electronic equilibrium, as well as its monitoring using an extended free-air ionization chamber are explored. Such an extra-source of radiation can be used for carrying out various non-commercial pro-grams like radiation tests, sanitization of archival materials and cultural heritage objects, etc.

X-ray micro tomography in the scanning electron microscope

1978 ◽  
Vol 36 (1) ◽  
pp. 106-107 ◽  
Author(s):  
W. Brünger
Keyword(s):  
Electron Beam ◽  
Electron Microscope ◽  
Scanning Electron Microscope ◽  
Target Surface ◽  
The Body ◽  
X Rays ◽  
Cross Sectional ◽  
X Ray ◽  
Micro Tomography ◽  
Scanning Electron

Reconstructive tomography is a new technique in diagnostic radiology for imaging cross-sectional planes of the human body /1/. A collimated beam of X-rays is scanned through a thin slice of the body and the transmitted intensity is recorded by a detector giving a linear shadow graph or projection (see fig. 1). Many of these projections at different angles are used to reconstruct the body-layer, usually with the aid of a computer. The picture element size of present tomographic scanners is approximately 1.1 mm2.Micro tomography can be realized using the very fine X-ray source generated by the focused electron beam of a scanning electron microscope (see fig. 2). The translation of the X-ray source is done by a line scan of the electron beam on a polished target surface /2/. Projections at different angles are produced by rotating the object.During the registration of a single scan the electron beam is deflected in one direction only, while both deflections are operating in the display tube.

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