Quantitative EDS analysis in the SEM applying the XPP procedure

Author(s):  
Jean-Louis Pouchou ◽  
Françoise Pichoir

Extensive work has been done during the last decade to develop new models able to improve the performance of data reduction procedures 1n quantitative x-ray microanalysis. Some of them are now successfully used as routine tools in microprobe work, and allow to analyze accurately light and ultra-light elements and to characterize layered specimens.In the field of analytical scanning electron microscopy (SEM) using energy dispersive spectrometers (EDS), it seems that less attention has been paid to the effective improvement of the quantitation processes. Although EDS systems have unavoidable limitations due to their lower peak-to-background ratio and poorer resolution, the authors have the feeling that the quantitative results can be significantly improved by use of more reliable models taking properly into account the specific instrumental and experimental conditions.With this aim in view, our first contribution has been to implement our recently developed XPP model and associated routines (mass absorption coefficients, efficiency of the Quantum window) into the KEVEX Delta system.

Author(s):  
Jean-Louis pouchou ◽  
Françoise Pichoir

The ϕ(ρz) models developed during the recent years (Gaussian, PAP, XPP) have been shown by several authors to improve significantly the capability of quantitative x-ray microanalysis, mainly in the field of light elements, tilted specimens, and layered specimens. An increasing number of users is now able to take advantage of these models, since some of them have been implemented in EPMA or EDS commercial softwares.However, most of the reported successful applications are the result of analyses with standards, where the basic data are the relative x-ray intensities (also called k-ratios). Indeed, analyses with standards are well adapted to the electron microprobes, and permit to obtain very accurate results. But in the scanning electron microscopes (SEM), the operations of acquiring, processing and handling the EDS spectra of all the required standards are really time consuming. It is why an EDS standardless mode giving satisfactory quantitative results would be so useful, even for those laboratories which can also operate an electron microprobe for the applications requiring the highest degree of accuracy.


2020 ◽  
Vol 34 (7) ◽  
pp. 8848-8856
Author(s):  
Elena V. Fomenko ◽  
Vladimir V. Yumashev ◽  
Sergey V. Kukhtetskiy ◽  
Anatoliy M. Zhizhaev ◽  
Alexander G. Anshits

2011 ◽  
Vol 1307 ◽  
Author(s):  
M. Sajjad ◽  
H. X. Zhang ◽  
P. X. Feng

ABSTRACTThe synthesis of boron nitride nanowires on silicon (Si) and nanorods on molybdenum (Mo) substrates at the same experimental conditions was composed. Fine tip nanowires with diameters around 50 nm were produced on Si substrates, whereas, nanorods with diameter around 100 nm were formed on Mo substrates. The change in length from 5 μm to 100 μm for nanowires and 0.2 μm to 0.8μm for nanorods following variation of substrate temperature were studied systematically.Scanning Electron Microscopy was used to analyze the surface images of BN nanowires and nanorods. Energy Dispersive X-Ray spectroscopy (EDS) was used to analyze boron and nitrogen concentration in the samples. The crystal structures of BN samples were investigated using Raman spectroscopy and x-ray diffraction. The experimental results showed that the nanorods are hexagonal mixed with cubic, whereas the nanowires are hexagonal.


2014 ◽  
Vol 20 (5) ◽  
pp. 1565-1575 ◽  
Author(s):  
Abdelhalim Zoukel ◽  
Lahcen Khouchaf ◽  
Jean Di Martino ◽  
David Ruch

AbstractA procedure has been developed to follow degradation of energy-dispersive spectroscopy (EDS) X-ray lateral resolution in a variable pressure scanning electron microscope. This procedure is based on evaluation of the EDS profile shape change for different experimental conditions. Some parameters affecting the X-ray resolution in high-vacuum mode have been taken into account. Good agreement between the simulated and experimental EDS profiles shows the reliability of the proposed procedure. A significant improvement in measurement of the EDS profile interfacial distance (DINT) has been achieved.


2013 ◽  
Vol 1612 ◽  
Author(s):  
D. E. Ortega-Zavala ◽  
Alexander Gorokhovsky ◽  
J. I. Escalante-García

ABSTRACTPastes of waste glass (WG) and metakaolin (MK) were prepared by chemical activation with sodium silicate solutions of modulus Ms = 0.5, 0.75, 1 and 1.25 adjusted with sodium hydroxide. An experimental design was carried out using the Taguchi method. The compressive strength (CS) was followed for up to 120 days and then 4 selected formulations of the higher CS were further characterized by X-ray diffraction and scanning electron microscopy. The results showed that the CS depends on the experimental conditions of %WG, %Na2O and Ms and showed a maximum of 70 MPa after 120 days for the paste with 100%WG (%wt.), 8% Na2O and Ms=1.25; while a Portland cement specimen cured at 20°C reached 43MPa. The WG is more reactive than the MK under less alkaline conditions. The features of the microstructures varied notably with the %WG; however all showed relative dense matrices of reaction products, in agreement with the CS attained.


2011 ◽  
Vol 17 (5) ◽  
pp. 710-717 ◽  
Author(s):  
Luigi Paoletti ◽  
Biagio M. Bruni ◽  
Antonio Gianfagna ◽  
Simona Mazziotti-Tagliani ◽  
Alessandro Pacella

AbstractThe quantitative scanning electron microscope–energy dispersive X-ray (SEM-EDX) analysis of a horneblende and two augite prismatic samples reduced to submicrometric particles was performed, and error due to the particle effects (“absent mass” and the “reduced absorption” effect) was minimized. Correction factors as a function of fragment size were obtained for O, Na, Mg, Si, Ca, and Fe. In addition, the influence of chemical composition of the samples used as standards (the matrix effect) on correction factors was evaluated. The results indicate that the absent mass effect is dominant for all elements except for the light elements O and Na, for which the reduced absorption effect is dominant. No significant matrix effect has been observed. By using corrected SEM-EDX data, the error on quantification of the element concentration has been estimated to be 3% relative for light elements and below 2% relative for heavy elements (notably, about 1% relative for Fe).


2011 ◽  
Vol 493-494 ◽  
pp. 539-544
Author(s):  
Guler Ungan ◽  
F. Ak Azem ◽  
Ahmet Cakir

Ti6Al4V alloy commonly used in human body for load bearing prosthesis was coated by micro arc oxidation (MAO) with magnesium rich TiO2 oxide. Since the presence of magnesium in bone tissues is known to promote bone formation and proliferation in physiological environment, its integration with TiO2 on implant surface could bring about a bioactivity for a fast bone formation and proliferation. The formation of a composite layer consisting of Mg integrated TiO2 by MAO process was carried out in an electrolyte with different magnesium content. The characterization studies of these coatings were performed by using X-ray diffractometry (XRD), scanning electron microscopy (SEM) coupled with EDS analysis and XP2 surface profilometry.


2009 ◽  
Vol 24 (1) ◽  
pp. 58-65 ◽  
Author(s):  
Yange Zhang ◽  
Zhi Zheng ◽  
Ka Wai Wong ◽  
Fengling Yang ◽  
Zude Zhang

The α-, β-, and δ-MnO2 with various morphologies have been synthesized by a novel redox system of KMnO4 and CuCl with HCl added under a hydrothermal condition. The resultant MnO2 products have been characterized by x-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Upon control of reaction temperature and duration, it was observed that MnO2 polymorphs of different morphology (e.g., flowery δ-MnO2, β-MnO2 nanowires and octahedrons, α-MnO2 nanowires) can be prepared in an adjustable manner. The phenomenon is mainly attributed to the effect of cuprous ions controllably released from CuCl by the action of HCl at different experimental conditions. The corresponding formation mechanism for the MnO2 crystals will also be proposed and discussed.


Nukleonika ◽  
2017 ◽  
Vol 62 (2) ◽  
pp. 177-181 ◽  
Author(s):  
Agata Stoch ◽  
Jan Maurin ◽  
Paweł Stoch ◽  
Jan Kulawik ◽  
Dorota Szwagierczak

Abstract Multiferroic 0.5BiFeO3-0.5Pb(Fe0.5Ta0.5)O3 solid solution is a material that exhibits ferroelectric and antiferromagnetic orderings in ambient temperature. The solid solution was obtained as a result of a conventional reaction in a solid state. The obtained material is a dense, fine-grained sinter whose surface was observed by scanning electron microscopy (SEM) and stoichiometry was confirmed by energy dispersive X-ray spectroscopic (EDS) analysis. According to the X-ray powder diffraction (XRD) measurements, the main phase is R3c space group with admixture of Pm-3m regular phase. Small contribution of pyrochlore-like phase was also observed. Mössbauer spectroscopy suggested random distribution of Fe3+/Ta5+ cations in the B sites of ABO3 compound. Reduction of the magnetic hyperfine field with an increase in the substitution of Ta5+ in Fe3+ neighbourhood was also observed.


1994 ◽  
Vol 353 ◽  
Author(s):  
S. Hamasaki ◽  
K. Tsukimura ◽  
K. Fujimoto ◽  
K. Omura ◽  
R. Ikeda

AbstractAlteration minerals from a drill-core (maximum depth 2002 m) in the granitic rock at Ashio, central Japan, were studied by optical microscopy, X-ray diffractometry and analytical scanning electron microscopy. In the host rock, biotite is altered to chlorite and plagioclase to illite. Calcite has precipitated in veinlets and grain boundaries. The host rock close to fractures is strongly altered, whereas the rocks distant from fractures are less altered. Quartz, illite, chlorite, laumontite and calcite have precipitated on fracture walls. The alteration minerals are estimated to have formed in the range 140–200°C, higher than the present temperature (13°96°C). The chemical composition of the ground water in the granitic rock at Ashio was estimated thermodynamically from the mineral assemblage. The alteration reaction of palgioclase and the precipitation of calcite may occur simultaneously. The alteration minerals formed in the host rock and in the fractures may adsorb radionuclides effectively, and thus may inhibit radionuclide transport to biosphere.


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