Electron-Probe Quantitative Energy-Dispersive Analysis of Trace Magnesium Concentrations in Ag-Mg Alloys

Author(s):  
R. B. Marinenko

Internally oxidized Ag-Mg alloys are used as sheaths for high Tc superconductor wires because of their superior mechanical properties. The preparation and characteristics of these materials have been reported. Performance of the sheaths depends on the concentration of the magnesium which generally is less than 0.5 wt. percent. The purpose of this work was to determine whether electron probe microanalysis using energy dispersive spectrometry (EDS) could be used to quantitate three different Ag-Mg alloys. Quantitative EDS analysis can be difficult because the AgL escape peak occurs at the same energy (1.25 keV) as the Mg Kα peak. An EDS spectrum of a Ag-Mg alloy wire is compared to a pure Ag spectrum in Fig. 1.

1989 ◽  
Vol 169 ◽  
Author(s):  
Alexis S. Nash ◽  
K. C. Goretta ◽  
Philip Nash ◽  
R. B. Poeppel ◽  
Donglu Shi

AbstractA series of 4336 Bi‐Sr‐Ca‐Cu oxide samples doped with 1 to 5% metallic Ag was prepared by solid state reaction. The distribution of Ag, the microstructure and the crystal structure of the samples were studied using energy dispersive spectrometry, EDS, scanning electron microscopy, SEM, and x‐ray diffractometry, XRD. Addition of Ag leads to a marked increase in preferred orientation with (001) planes perpendicular to the pressing direction in sintered pellets. The resistivity‐temperature data show an enhanced Tc in Ag‐doped samples under certain conditions. Energy dispersive spectrometry indicates that the dopant mostly segregates to the grain boundaries.


Author(s):  
S.J.B. Reed

INTRODUCTION. Quantitative analysis is possible with an E.D. system, provided its performance is adequate (stability especially). Such a system may be fitted to an electron probe, SEM, TEM, or STEM and used for the analysis of either thick or thin specimens, of which the former are considered primarily here, though in many respects the procedures discussed are equally applicable to thin specimens. Elements in the range Z = 11-30 are primarily of interest (i.e. those with K peaks in the energy range 1-10 keV), though heavy elements with L or M peaks in this energy range can be treated by the methods discussed as well.PEAK IDENTIFICATION. Often the analyst knows the elements present in the specimen. If not,a procedure for identifying peaks in the recorded spectrum is necessary. Various mathematical techniques are available for this purpose (e.g. cross-correlation with a gaussian).


1997 ◽  
Vol 3 (6) ◽  
pp. 504-511
Author(s):  
Ryna B. Marinenko ◽  
Mark Teplitsky

Abstract: Multiple linear least squares (MLLSQ) and sequential simplex spectral processing procedures were used in an electron probe energy-dispersive (EDS) analysis of a 2223 Bi-Sr-Ca-Cu-O (BSCCO) high Tc superconductor specimen. This phase is normally difficult to quantify by EDS at voltages below 25 kV because of the severe overlap of the BiM lines with the M lines from a small amount of Pb that is added to the phase for stability. Quantitative results from the MLLSQ spectral processing and ZAF matrix correction procedures agreed well with wavelength-dispersive analysis (WDS) of the same specimen.


1988 ◽  
Vol 02 (03n04) ◽  
pp. 651-656
Author(s):  
J.G. ZHAO ◽  
L.Y. CAI ◽  
Y.L. ZHANG ◽  
X.R. CHENG ◽  
F.H. Li

Electron diffraction and X-ray energy dispersive analysis are used to determine the phases and chemical composition of the compound Th(Y)-Ba-Cu-O. The main phase is Th(Y)Sa2Cu3O 7−x which has the similar crystal structure as YBa2Cu3O 7−x and shows the superconductivity with Tc=67 K.


Author(s):  
Dale E. Newbury

Conferences on quantitative electron probe X-ray microanalysis are typically highlighted by presentations which seek to advance the state of analytical science in this field through improvements in knowledge of the fundamentals of electron/X-ray-specimen interactions, inter-element (matrix) corrections, corrections for irregular specimen geometry, etc. However, in light of recent developments in computer-assisted, energy dispersive X-ray spectrometry analytical systems, we need to re-evaluate what is actually taking place in the everyday application of this analytical technique. The central paradigm in quantitative electron probe X-ray microanalysis, as established in the earliest work of Castaing and built upon by generations of contributors, is the measurement of the ratio of the intensity of an element in the unknown to the intensity for the same element in a standard under constant conditions of beam energy, known dose, and spectrometer performance. The set of such “k-values” determined for all constituents in the unknown is then converted into a set of concentrations through the use of matrix correction factors calculated through one of several schemes, e.g., “ZAF”, ϕ(ρz), etc. The great power of electron-excited X-ray microanalysis derives from the simplicity of the standards required.


Author(s):  
H.-J. Ou ◽  
J. M. Cowley

Using the dedicate VG-HB5 STEM microscope, the crystal structure of high Tc superconductor of YBa2Cu3O7-x has been studied via high resolution STEM (HRSTEM) imaging and nanobeam (∽3A) diffraction patterns. Figure 1(a) and 2(a) illustrate the HRSTEM image taken at 10' times magnification along [001] direction and [100] direction, respectively. In figure 1(a), a grain boundary with strong field contrast is seen between two crystal regions A and B. The grain boundary appears to be parallel to a (110) plane, although it is not possible to determine [100] and [001] axes as it is in other regions which contain twin planes [3]. Following the horizontal lattice lines, from left to right across the grain boundary, a lattice bending of ∽4° is noticed. Three extra lattice planes, indicated by arrows, were found to terminate at the grain boundary and form dislocations. It is believed that due to different chemical composition, such structure defects occur during crystal growth. No bending is observed along the vertical lattice lines.


1987 ◽  
Vol 48 (10) ◽  
pp. 1623-1625 ◽  
Author(s):  
B. Farnoux ◽  
R. Kahn ◽  
A. Brulet ◽  
G. Collin ◽  
J.P. Pouget

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