Influence of X-Ray Induced Fluorescence on Energy Dispersive X-Ray Analysis of Thin Foils

Author(s):  
E. A. Kenik ◽  
J. Bentley

Cliff and Lorimer (1) have proposed a simple approach to thin foil x-ray analy sis based on the ratio of x-ray peak intensities. However, there are several experimental pitfalls which must be recognized in obtaining the desired x-ray intensities. Undesirable x-ray induced fluorescence of the specimen can result from various mechanisms and leads to x-ray intensities not characteristic of electron excitation and further results in incorrect intensity ratios.In measuring the x-ray intensity ratio for NiAl as a function of foil thickness, Zaluzec and Fraser (2) found the ratio was not constant for thicknesses where absorption could be neglected. They demonstrated that this effect originated from x-ray induced fluorescence by blocking the beam with lead foil. The primary x-rays arise in the illumination system and result in varying intensity ratios and a finite x-ray spectrum even when the specimen is not intercepting the electron beam, an ‘in-hole’ spectrum. We have developed a second technique for detecting x-ray induced fluorescence based on the magnitude of the ‘in-hole’ spectrum with different filament emission currents and condenser apertures.

Author(s):  
C. E. Lyman ◽  
D. W. Ackland

Analytical electron microscopy (AEM) was well served by the original hole count test that prompted microscope manufacturers to reduce, by an order of magnitude, spurious x-ray generation in the specimen. This spurious x-ray signal is caused by hard x-rays or uncollimated electrons from the illumination system and is typically generated over the entire specimen regardless of where the electron probe is placed for analysis. The original test was performed on an ion-milled thin foil disk specimen of Ag or Mo, but the absolute value of hole count was dependent upon both specimen and operator. To make progress in die reduction of spurious xrays at intermediate voltages (if the problem is present), a hole-count test on a standard specimen that does not require operator judgement would be useful. The ultimate goal would be to reduce spurious x-rays to a level that would not affect any experiment on any specimen.


2014 ◽  
Vol 92 (11) ◽  
pp. 1489-1493 ◽  
Author(s):  
P.V. Sreevidya ◽  
S.B. Gudennavar ◽  
Daisy Joseph ◽  
S.G. Bubbly

K shell X-rays of barium and thallium following internal conversion decay in Cs137 and Hg203, respectively, were detected using a Si(Li) X-ray detector coupled to PC-based 8k multichannel analyser employing the method suggested earlier by our group. The K shell X-ray intensity ratios and vacancy transfer probabilities for thallium and barium were calculated. The obtained results are compared with theoretical, semiempirical, and others’ experimental results obtained via photoionization as well as decay processes. The effects of beta decay and internal conversion on X-ray emission probabilities are discussed.


1989 ◽  
Vol 33 ◽  
pp. 521-529
Author(s):  
Tomoya Arai ◽  
Takashi Shoji

In the spectroscopic analysis of composite elements by x-ray fluorescence (XRF), it is the fundamental feature of this method that the background x-ray intensity is lower than that with electron excitation. However, the background x-rays of this method, which consist of Thomson (Rayleigh) and Compton scattered x-rays from the primary radiation, impair the analytical performance at the ppm level. In order toinvestigate the intensity of the background x-rays precisely,the study was conducted in two parts. The first part compared the measured and theoretically calculated x-ray intensities for Rh Kα and Rh Kβ peaks from various materials. The second part examined the determination of low concentrations of lead,arsenic and colonium in steel samples. The variation in the background x-ray intensities of the analyzed elements was found to be caused by the variation of the major elements and a correction equation for it is derived.


1969 ◽  
Vol 13 ◽  
pp. 26-48
Author(s):  
A. K. Baird

Qualitative and quantitative analyses of elements below atomic number 20, and extending to atomic number 4, have been made practical and reasonably routine only in the past five to ten years by advances in: 1) excitation sources; 2) dispersive spectrometers; 3) detection devices; and 4) reductions of optic path absorption. At present agreement is lacking on the best combination of parameters for light element analysis. The principal contrasts in opinion concern excitation.Direct electron excitation, particularly as employed in microprobe analysis (but not limited to such instruments), provides relatively high emission intensities of all soft X-rays, but also generates a high continuum, requires the sample to be at essentially electron gun vacuum, and introduces practical calibration problems (“matrix effects“). X-ray excitation of soft X-rays overcomes some of the latter three disadvantages, and has its own limitations. Sealed X-ray sources of conventional or semi-conventional design can provide useful (if not optimum) light element emission intensities down to atomic number 9, hut with serious loss of efficiency in many applications below atomic number 15 largely because of window-thinness limitations under electron bombardment.


2020 ◽  
Vol 108 (5) ◽  
pp. 415-423
Author(s):  
Esra Cinan ◽  
Bünyamin Aygün ◽  
M. I. Sayyed ◽  
Yüksel Özdemir

AbstractL X-ray intensity ratios for CeO2, Sm2(SO4)3, Ho2O3, and Yb2O3 compounds were experimentally investigated. The measurements were gauged following excitation by 59.54 keV γ-rays from a 100 mCi 241Am radioactive annular source at different temperatures in situ. Temperature change occurred between 50 °C and 400 °C. L X-ray emission spectra were obtained by using a solid-state Si(Li) X-ray detector. L X-ray production cross sections, intensity ratios, and full-width half maximum (FWHM) values for the compounds were determined by evaluating the emission spectra varying with the temperature. According to the results obtained, it was observed that Lβ1 X-rays were less influenced in comparison with Lα X-rays while Lα X-rays were also less influenced in comparison with Lβ2 X-rays.


1968 ◽  
Vol 46 (10) ◽  
pp. S409-S413 ◽  
Author(s):  
Walter H. G. Lewin ◽  
George W. Clark ◽  
William B. Smith

A complete X-ray survey of the northern sky has been made in the energy range 20–100 keV. Spectra are given for Cyg X-1 and Tau X-1. Intensity ratios (Cyg X-1/Tau X-1) of 0.84 ± 0.10 and 1.30 ± 0.25 were derived in the 20–70 keV range from data obtained on July 19, 1966 and February 13, 1967, respectively. Observations on Sco X-1 and the Coma cluster show upper limits which are quite different from results reported by other groups.


1968 ◽  
Vol 22 (5) ◽  
pp. 434-437 ◽  
Author(s):  
E. A. Hakkila ◽  
R. G. Hurley ◽  
G. R. Waterbury

Two methods were evaluated for determining rare earths in plutonium: (1) For the lighter rare earths ( Z≦66), or low concentrations of the heavier rare earths, an adjacent rare earth was added as a carrier and also as an internal standard, the rare earths were separated from plutonium by fluoride precipitation, and the measured intensity ratios for the sample and for solutions having known concentrations were compared. The Lβ1 x-rays were measured for the lighter rare earths and the Lα1 x rays for the remaining lanthanides. (2) For the heavier rare earths ( Z>66), the Lα1 x-ray intensities were measured from a nitric acid solution of the sample and compared to intensities obtained for solutions having known concentrations. The minimum concentrations that could be measured with a relative standard deviation no greater than 4% by the separation internal standard method varied from approximately 0.5% for lanthanum to 0.01% for lutetium. The direct measurement of x-ray intensity was much less sensitive. Applicability of the methods was shown by successful analyses of plutonium alloys containing dysprosium, thulium, or lutetium.


Author(s):  
J.M. Brown ◽  
H.L. Fraser

Quantitative X-ray microanalysis of thin foils may be achieved either by calculation or by making use of standards. This paper, although advocating the use of pure elemental standards for accurate quantification, points out some of the problems involved in the choice of good standards. Specifically, the presence of surface films on as-prepared thin foil standards must be removed or accounted for during data analysis.


Author(s):  
D. B. Williams ◽  
J. R. Michael ◽  
J. I. Goldstein ◽  
A. D. Romig

The spatial resolution of x-ray microanalysis in a thin foil is determined by the size of the beam-specimen interaction volume. This volume is a combination of the incident electron beam diameter (d) and the beam broadening (b) due to elastic scatter within the specimen. Definitions of spatial resolution have already been proposed on this basis but all present a worst case value for the resolution based on the dimensions of the beam emerging from the exit face of the foil.


2016 ◽  
Vol 61 (2) ◽  
pp. 791-796 ◽  
Author(s):  
S. Lesz ◽  
S. Griner ◽  
R. Nowosielski

Abstract The cracking of materials and fracture surface is of great practical and academic importance. Over the last few years the development of the fractography of crystalline alloys resulted in a useful tool for the prediction or failure analysis. Many attempts have been made to observe cracks using optical microscopy, X-ray topography and transmission electron microscopy (TEM). Of these techniques, the resolution of optical microscopy and X-ray topography is too poor. By contrast, the resolution of TEM is high enough for detailed information to be obtained. However, in order to apply TEM observations, a thin foil specimen must be prepared, and it is usually extremely difficult to prepare such a specimen from a pre-selected region containing a crack. In the present work, deformation mechanisms fracture surfaces of Ni-based metallic glass samples have been studied by specially designed experiments. In order to study the deformation mechanisms and fracture the Ni-based metallic glasses have been investigated in the tensile test. The structure and fracture surfaces after the decohesion process in tensile tests were observed using transmission electron microscope (TEM) and scanning electron microscope (SEM), respectively. The studies of structure were performed on thin foils. Moreover the investigated tape was subjected to a banding test. Then, the tape was straightened and the thin foil from the area of maximum strain was prepared. This thin foil sample was deformed before the TEM investigation to obtain local tears.


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