Measuring grain boundary segregation using Wavelength Dispersive X-ray Spectroscopy: Further developments

2011 ◽  
Vol 605 (7-8) ◽  
pp. 848-858 ◽  
Author(s):  
P. Nowakowski ◽  
F. Christien ◽  
M. Allart ◽  
Y. Borjon-Piron ◽  
R. Le Gall
Keyword(s):  
Grain Boundary ◽  
Boundary Segregation ◽  
Grain Boundary Segregation ◽  
X Ray

Recent Developments in the Study of Grain Boundary Segregation by Wavelength Dispersive X-Ray Spectroscopy (WDS)

2011 ◽  
Vol 309-310 ◽  
pp. 39-44
Author(s):  
Pawel Nowakowski ◽  
Frédéric Christien ◽  
Marion Allart ◽  
René Le Gall
Keyword(s):  
Electron Beam ◽  
Fracture Surface ◽  
Grain Boundary ◽  
Electron Probe Microanalysis ◽  
Electron Probe ◽  
Boundary Segregation ◽  
Normal Incidence ◽  
Grain Boundary Segregation ◽  
X Ray ◽  
Recent Developments

It was recently shown [1] that EMPA-WDS (Electron Probe MicroAnalysis by Wavelength Dispersive X-ray Spectroscopy) can be used to detect and to accurately quantify monolayer surface and grain boundary segregation. This paper presents the last developments of this application. It focuses on the measurement of sulphur grain boundary segregation in nickel on fractured surfaces. A special attention was paid to the quantification of the sulphur coverage, taking into account the non-normal incidence of the electron beam on a fracture surface. Sulphur grain boundary segregation kinetics was measured at 750°C in nickel to document the quantitative possibilities of the technique.

scholarly journals Mechanical and Spectroscopic Characterization of Solute Elements in Aluminum

2020 ◽  
Vol 326 ◽  
pp. 09001
Author(s):  
Seiichiro Ii ◽  
Toru Hara
Keyword(s):  
Electron Microscopy ◽  
Grain Boundary ◽  
Boundary Segregation ◽  
Spectroscopic Characterization ◽  
Dislocation Nucleation ◽  
Grain Boundary Segregation ◽  
X Ray ◽  
Minor Elements ◽  
Si Doped

We characterized the distribution of minor elements such as Si and Fe in Al utilizing a nanoindentation and electron microscopy with an energy dispersed X-ray spectroscopy (EDS) system. Nanoindentation can detect the dislocation nucleation known as “pop-in” event, the critical load (Pc) depends on the solute amount of Fe. However, that in Si-doped Al is rarely changed up to 1.0 at% of Si. That independent Pc in Al-Si is caused by the inhomogeneity of the Si, which is the grain boundary segregation, in Al. The grain boundary segregation of Si was clearly detected by using a newly developed microcalorimeter type EDS system, even at the 0.1 at% Si.

The Effect of Coherent Bremsstrahlung Peaks in AEM Studies of Grain Boundary Segregation

1985 ◽  
Vol 43 ◽  
pp. 248-249
Author(s):  
K. S. Vecchio
Keyword(s):  
Electron Microscope ◽  
Grain Boundary ◽  
Boundary Segregation ◽  
Grain Boundary Segregation ◽  
X Ray ◽  
Interaction Volume ◽  
Peak Intensity ◽  
Coherent Bremsstrahlung ◽  
Analytical Electron ◽  
Analytical Electron Microscope

Recently coherent bremsstrahlung (CB) peaks have been detected in x-ray spectra in the analytical electron microscope (AEM). It has been suggested that CB peaks, which are Gaussian, may either mask, or be misinterpreted as elemental peaks in x-ray spectra. A method for identifying and isolating these peaks has been presented, The problem of CB peaks is particularly severe in AEM grain boundary segregation studies, because the amount of segregant in the interaction volume is small (<∼3 wt%), the x-ray counting times are long, and as a result the CB peak intensities can approximate to the expected segregant peak intensity. The misleading effects of CB can be either to produce pseudo-element peaks close to true element peak positions, or to overestimate the true element peak intensity when the CB peaks are superimposed on the x-ray peak of the segregant. This article reports an investigation of the effects of CB on segregation studies in Cu and Fe.

Multivariate statistical analysis of a series of alchemi spectra

1996 ◽  
Vol 54 ◽  
pp. 550-551 ◽  
Author(s):  
Ian M. Anderson ◽  
J. Bentley
Keyword(s):  
Statistical Analysis ◽  
Grain Boundary ◽  
Multivariate Statistical Analysis ◽  
Spectral Component ◽  
Boundary Segregation ◽  
Grain Boundary Segregation ◽  
Multivariate Statistical ◽  
X Ray ◽  
The Matrix ◽  
Electron Energy Loss

Multivariate statistical analysis (MSA) of a series of spectra or images offers an objective and quantitative way to characterize the features of the spectra that vary in a correlated fashion and to determine the number of independently varying components in the series. For example, in a series of spectra showing grain boundary segregation, there may be only one independently varying spectral component, which signifies an increase in the concentrations of the segregants and a corresponding decrease in the concentrations of some of the matrix constituents. The basis of the MSA method has been outlined by Trebbia and Bonnet, with application to the analysis of electron energy-loss spectrum images. Titchmarsh et al., have applied this analysis to a series of energy dispersive X-ray (EDX) spectra for the study of grain boundary segregation. The present paper illustrates the application of MSA methods to a series of EDX spectra acquired for ALCHEMI analysis. The basic method has been modified slightly for the analysis of ALCHEMI data.

scholarly journals Quantification of Grain Boundary Segregation Monolayers by X-ray Spectroscopy in a Scanning Electron Microscope

2011 ◽  
Vol 17 (S2) ◽  
pp. 602-603 ◽  
Author(s):  
P Nowakowski ◽  
F Christien ◽  
M Allart ◽  
Y Borjon-Piron ◽  
R Le Gall ◽  
...  
Keyword(s):  
Electron Microscope ◽  
Scanning Electron Microscope ◽  
Grain Boundary ◽  
Boundary Segregation ◽  
Grain Boundary Segregation ◽  
X Ray ◽  
Scanning Electron

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.

Concentration depth distribution of grain boundary segregation measured by wavelength dispersive X-ray spectroscopy

2015 ◽  
Vol 159 ◽  
pp. 432-437 ◽  
Author(s):  
Wuqiang Yang ◽  
Min Xu ◽  
Huanhuan Bai ◽  
Ye Meng ◽  
Litao Wang ◽  
...  
Keyword(s):  
Grain Boundary ◽  
Depth Distribution ◽  
Boundary Segregation ◽  
Grain Boundary Segregation ◽  
X Ray

Low-magnification Quantitative X-ray Mapping of Grain-boundary Segregation in Aluminum–4 wt.% Copper by Analytical Electron Microscopy

1999 ◽  
Vol 5 (4) ◽  
pp. 254-266 ◽  
Author(s):  
D.T. Carpenter ◽  
M. Watanabe ◽  
K. Barmak ◽  
D.B. Williams
Keyword(s):  
Grain Boundary ◽  
Analytical Electron Microscopy ◽  
Boundary Segregation ◽  
Grain Boundary Segregation ◽  
Acquisition Time ◽  
X Ray ◽  
Fine Grained ◽  
Trade Offs ◽  
Analytical Electron ◽  
Counting Statistics

Abstract: Quantitative X-ray mapping in the analytical electron microscope (AEM) could improve the statistics of grain-boundary segregation measurements if high spatial resolution can be maintained at lower magnifications (<500 kX). Typically, only about 10 boundaries are analyzed because of the difficulty of conventional AEM measurements; however, a low-magnification quantitative X-ray map could contain twice this number of boundaries in a single field of view. Microscope conditions and mapping parameters have been explored for operation at ∼250 kX, under a variety of conditions to illustrate the trade-offs between various characteristics, such as analytical resolution, counting statistics, magnification, and acquisition time. From these data, it is possible to extrapolate to maps generated under different conditions and estimate their limitations with respect to these characteristics. A simple model has been developed to describe the behavior of inclined grain boundaries that can be used to estimate the detectability of segregant as a function of boundary tilt. Using quantitative X-ray maps, grain boundary Cu coverage has been measured from 55 boundaries in Al–4 wt.% Cu with minimal user effort. For fine-grained thin films, mapping is substantially more efficient than other methods of data acquisition and may be used to measure segregation at large numbers of boundaries.

On The Study Of Grain Boundary Segregation Using X-Ray Diffraction And Computer Simulation

1991 ◽  
Vol 238 ◽  
Author(s):  
C. A. Counterman ◽  
I. Majid ◽  
P. D. Bristowe ◽  
R. W. Balluffi
Keyword(s):  
Computer Simulation ◽  
Grain Boundary ◽  
Boundary Segregation ◽  
Grain Boundary Segregation ◽  
Boundary Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Grain Boundary Structure ◽  
Structure Factors ◽  
Diffraction Effects

ABSTRACTThe possibility of studying grain boundary segregation using X-ray diffraction is explored by performing a computer simulation of the diffraction effects expected from the segregation of solute atoms to grain boundaries in two gold alloy systems, i.e. Au-Ag and Au-Ni. Using atomistic Monte-Carlo and molecular statics methods, equilibrium boundary structures are determined and analyzed by computing the grain boundary structure factors. Various changes in both relative and absolute grain boundary structure factors are found which can be directly related to structural and compositional changes due to segregation. In addition, systematic diffraction effects are found as a function of boundary misorientation. The experimental conditions required for verifying these predictions are discussed.

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