STEM-EDS X-RAY MICROANALYSIS IN THIN METAL FOILS

Instruments combining a 100 kV transmission electron microscope (TEM) with scanning transmission (STEM), secondary electron (SEM) and x-ray energy dispersive spectrometer (EDS) attachments to give analytical capabilities are becoming increasingly available and useful. Some typical applications in the field of materials science which make use of the small probe size and thin specimen geometry are the chemical analysis of small precipitates contained within a thin foil and the measurement of chemical concentration profiles near microstructural features such as grain boundaries, point defect clusters, dislocations, or precipitates. Quantitative x-ray analysis of bulk samples using EDS on a conventional SEM is reasonably well established, but much less work has been performed on thin metal foils using the higher accelerating voltages available in TEM based instruments.

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Reply to “comments on energy dispersive x-ray measurements of thin metal foils”

Scripta Metallurgica ◽

10.1016/0036-9748(77)90197-1 ◽

1977 ◽

Vol 11 (4) ◽

pp. 261-263 ◽

Cited By ~ 9

Author(s):

J. Bentley ◽

E.A. Kenik

Keyword(s):

Thin Metal ◽

Energy Dispersive ◽

X Ray ◽

Metal Foils

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Microchemical Analysis of thin Metal Foils

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100092062 ◽

1976 ◽

Vol 34 ◽

pp. 420-421 ◽

Cited By ~ 1

Author(s):

N. J. Zaluzec ◽

H. L. Fraser

Keyword(s):

Thin Metal ◽

Specimen Thickness ◽

Marked Variation ◽

X Ray ◽

Metal Foils ◽

Elemental Concentrations ◽

Microchemical Analysis

Several techniques have been developed for quantitative x-ray microanalysis of thin metal foils. These techniques usually provide relative elemental concentrations, and assume that for a “thin” homogeneous alloy of elements A and B, the ratio of intensity (I) of any two characteristic x-ray peaks (e.g.IAKα/IBKα) should be independent of specimen thickness. Recently, Fraser et al., conducted experiments using a highly ordered alloy (β-NiAl) to investigate this assumption, and indeed showed that in electron transparent regions of the foils there was a marked variation in the ratio of the Ka peaks of Ni and Al, respectively. The results given by Fraser et al., are summarized in Fig. 1.

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X-ray determination of the thickness of thin metal foils

Journal of X-Ray Science and Technology ◽

10.3233/xst-130383 ◽

2013 ◽

Vol 21 (3) ◽

pp. 347-355 ◽

Cited By ~ 3

Author(s):

Robert C. Block ◽

Jeffrey A. Geuther ◽

Brian Methe ◽

Devin P. Barry ◽

Gregory Leinweber

Keyword(s):

Thin Metal ◽

X Ray ◽

Metal Foils

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Comments on “energy dispersive x-ray measurements of thin metal foils”

Scripta Metallurgica ◽

10.1016/0036-9748(77)90196-x ◽

1977 ◽

Vol 11 (4) ◽

pp. 256-258 ◽

Cited By ~ 2

Author(s):

Nestor J. Zaluzec ◽

John B. Woodhouse ◽

Hamish L. Fraser

Keyword(s):

Thin Metal ◽

Energy Dispersive ◽

X Ray ◽

Metal Foils

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Microanalytical Identification of a New Zr-Nb-Fe Phase

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100134259 ◽

1990 ◽

Vol 48 (2) ◽

pp. 132-133

Author(s):

O.T. Woo ◽

G.J.C. Carpenter

Keyword(s):

Trace Elements ◽

Cold Rolling ◽

Proportionality Factor ◽

Tube Material ◽

X Ray ◽

Metal Foils ◽

Arc Melting ◽

Intermetallic Particles ◽

Intermetallic Precipitates ◽

Cold Worked

To study the influence of trace elements on the corrosion and hydrogen ingress in Zr-2.5 Nb pressure tube material, buttons of this alloy containing up to 0.83 at% Fe were made by arc-melting. The buttons were then annealed at 973 K for three days, furnace cooled, followed by ≈80% cold-rolling. The microstructure of cold-worked Zr-2.5 at% Nb-0.83 at% Fe (Fig. 1) contained both β-Zr and intermetallic precipitates in the α-Zr grains. The particles were 0.1 to 0.7 μm in size, with shapes ranging from spherical to ellipsoidal and often contained faults. β-Zr appeared either roughly spherical or as irregular elongated patches, often extending to several micrometres.The composition of the intermetallic particles seen in Fig. 1 was determined using Van Cappellen’s extrapolation technique for energy dispersive X-ray analysis of thin metal foils. The method was employed to avoid corrections for absorption and fluorescence via the Cliff-Lorimer equation: CA/CB = kAB · IA/IB, where CA and CB are the concentrations by weight of the elements A and B, and IA and IB are the X-ray intensities; kAB is a proportionality factor.

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