Measurements of absolute K -shell ionization cross sections and L -shell x-ray production cross sections of Ge by electron impact

Results from measurements of absolute K -shell ionization cross sections and L α x-ray production cross sections of Ge by impact of electrons with kinetic energies ranging from the ionization threshold up to 40 keV are presented. The cross sections were obtained by measuring K α and L α x-ray intensities emitted from ultrathin Ge films deposited onto self-supporting carbon backing films. Recorded x-ray intensities were converted to absolute cross sections by using estimated values of the sample thicknesses, the number of incident electrons, and the detector efficiency. Experimental data are compared with the results of widely used simple analytical formulas, with calculated cross sections obtained from the plane-wave and distorted-wave Born approximations and with experimental data from the literature

Use of the Bethe equation for inner-shell ionization by electron impact

We analyzed calculated cross sections for K-, L-, and M-shell ionization by electron impact to determine the energy ranges over which these cross sections are consistent with the Bethe equation for inner-shell ionization. Our analysis was performed with K-shell ionization cross sections for 26 elements, with L-shell ionization cross sections for seven elements, L-3-subshell ionization cross sections for Xe, and M-shell ionization cross sections for three elements. The validity (or otherwise) of the Bethe equation could be checked with Fano plots based on a linearized form of the Bethe equation. Our Fano plots, which display theoretical cross sections and available measured cross sections, reveal two linear regions as predicted by de Heer and Inokuti [in Electron Impact Ionization, edited by T. D. Mark and G. H. Dunn, (Springer-Verlag, Vienna, 1985), Chap. 7, pp. 232-276]. For each region, we made linear fits and determined values of the two element-specific Bethe parameters. We found systematic variations of these parameters with atomic number for both the low-and the high-energy linear regions of the Fano plots. We also determined the energy ranges over which the Bethe equation can be used

A track record of Au-Ag nanomelt generation during fuid‑mineral interactions

Recent studies have reported the signifcant role of Au-bearing nanoparticles in the formation of hydrothermal gold deposits. Despite the ever-increasing understanding of the genesis and stability of Au-bearing nanoparticles, it is still unknown how they behave when exposed to hydrothermal fuids. Here, we study the nanostructural evolution of Au–Ag nanoparticles hosted within Co-rich diarsenides and sulfarsenides of a natural hydrothermal deposit. We use high-resolution transmission electron microscopy to provide a singular glimpse of the complete melting sequence of Au–Ag nanoparticles exposed to the hydrothermal fuid during coupled dissolution–precipitation reactions of their host minerals. The interaction of Au–Ag nanoparticles with hydrothermal fuids at temperatures (400– 500 ºC) common to most hydrothermal gold deposits may promote melting and generation of Au–Ag nanomelts. This process has important implications in noble metal remobilization and accumulation during the formation of these deposits

Abellaite, NaPb2(CO3)2(OH), a new supergene mineral from the Eureka mine, Lleida province, Catalonia, Spain

The new mineral abellaite (IMA 2014-111), ideally NaPb2 (CO3)2 (OH), is a supergene mineral that was found in one of the galleries of the long-disused Eureka mine, in the southern Pyrenees (Lleida province), Catalonia, Spain. Abellaite is found as sparse coatings on the surface of the primary mineralization, it forms subhedral crystals not larger than 10μm as well as larger pseudohexagonal platelets up to ~ 30μm. Individual crystals commonly have a tabular to lamellar habit and form fairly disordered aggregates. The mineral is associated with a large number of primary minerals (roscoelite, pyrite, uraninite, coffinite, 'carbon', galena, sphalerite, nickeloan cobaltite, covellite, tennantite and chalcopyrite) and supergene minerals (hydrozincite, aragonite, gordaite, As-rich vanadinite andersonite, čejkaite, malachite and devilline). Abellaite is colourless to white, with a vitreous to nacreous lustre. The mineral is translucent, has a white streak and is non-fluorescent. The aggregates of microcrystals are highly friable. The calculated density using the ideal formula is 5.93 g/cm3. The chemical composition of the mineral (the mean of 10 electron microprobe analyses) is Na 3.88, Ca 0.29, Pb 72.03, C 4.17, O 19.47 and H 0.17, total 100.00 wt% (H, C and O by stoichiometry assuming the ideal formula). On the basis of 7 O atoms, the empirical formula of abellaite is Na0.96 Ca0.04 Pb1.98 (CO3)2 (OH). The simplified formula of the mineral is NaPb2 (CO3)2 (OH). The mineral is hexagonal, space group P 63 mc, a = 5.254(2), c = 13.450(5) Å, V = 321.5(2) Å3 and Z = 2. The strongest powder-diffraction lines [d in Å (I) (h k l)] are: 3.193 (100) (0 1 3), 2.627 (84) (1 1 0), 2.275 (29) (0 2 0), 2.242 (65) (0 2 1, 0 0 6), 2.029(95) (0 2 3). Abellaite has a known synthetic analogue, and the crystal structure of the mineral was refined by using crystallographic data of the synthetic phase. The mineral is named in honour of the mineralogist and gemmologist Joan Abella i Creus (b. 1968), who has long studied the deposits of the Eureka mine and who collected the mineral

Técnicas de caracterización mineral y su aplicación en exploración minera

En este trabajo se presenta una síntesis de las técnicas analíticas más utilizadas en la caracterización mineral, y su aplicación a la exploración y explotación minera. Las técnicas han sido clasificadas en 2 grupos. El primer grupo incluye a las técnicas de mayor uso ("técnicas convencionales"): (i) difracción de polvo de rayos X y difracción cuantitativa de rayos X, (ii) Microscopio electrónico de barrido con analizador de energías (SEM-EDS), (iii) catodoluminiscencia, y iv) microsonda electrónica (EMPA). El segundo grupo abarca un grupo de técnicas menos accesible, y mucho más caras, ("técnicas no convencionales"): (i) Particle Induced X-Ray Emission(Micro-PIXE), (ii) Secondary Ion Mass Spectrometry (SIMS, (iii) Laser-Ablation-Inductively Coupled Plasma-Mass Spectrometry (LAICP-MS). La mayor parte de la compilación esta dedicada a las técnicas convencionales (DRX, SEM-EDS y EMP), las cuales pueden ser de mayor impacto en el campo de la pequeña minerí

Electron probe microanalysis: principles and applications

Podeu consultar el llibre complet a: http://hdl.handle.net/2445/32166This article summarizes the basic principles of electron probe microanalysis, with examples of applications in materials science and geology that illustrate the capabilities of the technique

Electron-induced x-ray emission from solids. Simulation and measurements

Theoretical methods to compute accurate x-ray spectra emitted from targets bombarded with kV electrons are required for quantification in Electron Probe Microanalysis (EPMA), especially for the analysis of non-homogeneous samples. Monte Carlo simulation has proved to be the most suitable theoretical tool for the computation of x-ray spectra; it can incorporate realistic interaction cross sections and can be applied to complex geometries. Moreover, it allows us to keep track of the evolution of all secondary particles (and their descendants) generated by primary electrons. A Monte Carlo program for the calculation of ionization depth distributions and x-ray spectra produced by kV electron irradiation has been developed. Inner-shell ionization by electron impact is described by means of total cross sections evaluated from an optical-data model. A double differential cross section is proposed for bremsstrahlung emission, which combines a modified Bethe-Heitler DCS with the Kirkpatrick WiedmannStatham angular distribution, and reproduces the radiative stopping powers derived from the partial wave calculations of Kissel, Quarles and Pratt [At. Data Nud. Data Tables 28, 381 (1983)]. These ionization and radiative cross sections have been introduced into the general-purpose subroutine package PENELOPE, which performs simulation of coupled electron and photon transport for arbitrary materials. The underlying electron scattering model combines elastic scattering cross sections calculated by the partial wave method with inelastic cross sections obtained from Liljequist's generalized oscillator strength model. The reliability of the electron trajectory generation algorithm has been verified through a comparison of simulation results with measured backscattering coefficients and spatial dose distributions. To improve the efficiency of the simulation, a variance reduction technique, interaction forcing, has been applied for both ionizing collisions and radiative events. A systematic method for the measurement of ionization cross sections by electron impact, using the electron microprobe, has been proposed and applied. Measurements of ionization cross sections for Ni, er and Cu have been performed, from threshold up to 40 keV, combining the use of wavelength and energy dispersive spectrometers. Our results provide the electron-energy dependence of the ionization cross section to an accuracy of about 3%. The transformation to absolute cross section values increases the global uncertainty to about 12%. These errors include the determination of the target thickness, detector efficiency, solid angle of collection, the number of incident electrons, the fluorescence yield and the line fraction. The comparison between experiment and various theoretical formulas confirms that the optical-data model yields a more reliable energy dependence of the ionization cross section in the energy range of interest in microanalysis. Further work to reduce errors in the determination of the target mass thickness is required to draw a definite conclusion about the accuracy of the theoretical model in absolute magnitude. Simulated depth-distribution of ionizations and surface ionization, for different homogeneous targets and energies, have been shown to be in satisfactory agreement with experimental data taken from the literature. Comparison of simulated data, using various ionization cross sections, confirms again the validity of the optical-data model used. In the case of non-homogeneous samples (e.g. thin layers on substrates or multilayered structures) or special geometries (e.g. oblique incidence) experimental measurements are very rare and there is a real need for experimental data to check the reliability of simulations and/or alternative approximate formulations. Thus, experimental measurements and Monte Carlo simulations of the surface ionization have been performed (for Ni KC(o) X-rays) on Cu films of various thickness (40.5, 67, 100 and 196 nm) deposited onto a variety of substrates and for accelerating voltages between 10 keY and 30 keY. Measurements have been performed using the wavelength-dispersive spectrometer. The main difficulties of the measurements have been i) to ensure that tracer films have the same thickness, ii) the large statistical uncertainties due to the smallness of the peak-to-background ratio of the tracer peak, iii) the contribution from the substrate and iv) the surface contamination. In spite of the uncertainties arising from sample preparation and from the smallness of the peak-to-background ratio, the results from the experiments and the Monte Carlo simulations are found to agree to within 5%. These measurements allow us to validate the developed code and to obtain information of interest for the analytical methods of microanalysis. In particular, we have derived a simple analytical formula, based in a new scaling rule, which gives the surface ionization in terms of the bulk values of the substrate and the overlayer. Finally, simulated ionization distributions for different layered targets have been presented, which allow us to study the influence of the substrate on the ionization of the film. The reliability of the simulation code has been globally assessed by comparison of measured x-ray spectra with simulation results. X-ray spectra have been measured using the energy-dispersive spectrometer and converted to absolute units. Measurements in absolute units serve as the most stringent test of the physical parameters used in the simulation algorithm, although they may contain systematic uncertainties. Measurements have been performed for different targets and irradiation conditions, including multilayered targets and oblique incidence. The result of the various experimental sources of error leads to an overall uncertainty of 5-7%. The agreement between simulation and experiment has been shown to be satisfactory in the "meaningful" region of the spectra (say, between 3-15 keY), where the detector efficiency is essentially constant. Comparison of simulated and measured x-ray spectra obtained with the wavelength-dispersive spectrometer allows us to derive the absolute efficiency of the latter as a function of the x-ray incident energy. This information is essential for standardless x-ray microanalysis using wavelength-dispersive spectrometers. In short, we have developed a realistic Monte Carlo code adequate for the simulation of x-ray generation by electron irradiation of samples with complex geometries. We have already demonstrated its usefulness for EPMA of layered specimens. Although further work is required to include L- and M-shell ionization, the code has an evident potentiality for quantitative EPMA of samples with complex geometries. A Monte Carlo program for the calculation of ionization depth distributions and x-ray spectra produced by kV electron irradiation has been developed. The code is based on the PENELOPE subroutine package, which has been suitably modified to extend its range of application to lower energies. It incorporates a new double differential cross section for bremsstrahlung emission, which combines a modified Bethe-Heitler DCS with the Kirkpatrick-Wiedmann-Statham angular distribution. Ionization of inner-shells by electron impact is described by means of an optical-data model proposed by Mayol and Salvat. Interaction forcing is systematically applied to both bremsstrahlung and impact ionization to improve the efficiency of the simulation. The simulation program is applicable to samples with arbitrary geometries (multilayers, particulate samples, etc.). The ionization cross section for Ni, Cr and Cu has been experimentally determined using the electron microprobe. Measurements confirm that the optical-data model yields a more reliable energy dependence of the ionization cross section. Simulated depth-distribution of ionizations and surface ionization, for different homogeneous targets and energies, has been shown to be in satisfactory agreement with experimental data taken from the literature. Systematic measurements of the surface ionization, for a Ni tracer, in Cu films of different thicknesses deposited on a wide variety of substrates have been performed. The results from the experiments and simulations have been found to agree to within 5%. A simple analytical formula is proposed, which gives the surface ionization in terms of the bulk values of the substrate and the overlayer. Simulated ionization distributions for layered targets have been presented. Absolute x-ray spectra have been measured using the energy-dispersive spectrometer, for different targets and irradiation conditions. The agreement between simulation and experiment has been found to be satisfactory in the photon energy region of aprox. 3-15 keY, where the detector efficiency is constant. The absolute efficiency of a wavelength dispersive spectrometer has been obtained

Handbook of instrumental techniques for materials, chemical and biosciences research

This Handbook contains a collection of articles describing instrumental techniques used for Materials, Chemical and Biosciences research that are available at the Scientific and Technological Centers of the University of Barcelona (CCiTUB). The CCiTUB are a group of facilities of the UB that provide both the research community and industry with ready access to a wide range of major instrumentation. Together with the latest equipment and technology, the CCiTUB provide expertise in addressing the methodological research needs of the user community and they also collaborate in R+D+i Projects with industry. CCiTUB specialists include technical and Ph.D.-level professional staff members who are actively engaged in methodological research. Detailed information on the centers’ resources and activities can be found at the CCiTUB website www.ccit.ub.edu ..

Handbook of instrumental techniques for materials, chemical and biosciences research

This Handbook contains a collection of articles describing instrumental techniques used for Materials, Chemical and Biosciences research that are available at the Scientific and Technological Centers of the University of Barcelona (CCiTUB). The CCiTUB are a group of facilities of the UB that provide both the research community and industry with ready access to a wide range of major instrumentation. Together with the latest equipment and technology, the CCiTUB provide expertise in addressing the methodological research needs of the user community and they also collaborate in R+D+i Projects with industry. CCiTUB specialists include technical and Ph.D.-level professional staff members who are actively engaged in methodological research. Detailed information on the centers’ resources and activities can be found at the CCiTUB website www.ccit.ub.edu ..

Measurements of absolute K -shell ionization cross sections and L -shell x-ray production cross sections of Ge by electron impact

Results from measurements of absolute K -shell ionization cross sections and L α x-ray production cross sections of Ge by impact of electrons with kinetic energies ranging from the ionization threshold up to 40 keV are presented. The cross sections were obtained by measuring K α and L α x-ray intensities emitted from ultrathin Ge films deposited onto self-supporting carbon backing films. Recorded x-ray intensities were converted to absolute cross sections by using estimated values of the sample thicknesses, the number of incident electrons, and the detector efficiency. Experimental data are compared with the results of widely used simple analytical formulas, with calculated cross sections obtained from the plane-wave and distorted-wave Born approximations and with experimental data from the literature