X-ray fluorescence element-mapping spectrometer with improved spatial resolution

We developed an X-ray fluorescence element mapping spectrometer (XEMS) based on commercially available energy dispersive XRF equipment several years ago. Using XEMS, we found that this technique is applicable to realtime observation of the elemental distributions in living biological samples. This kind of observation is almost impossible by conventional techniques such as EPMA, PIXE etc. But the spatial resolution of the previous system was about 200pm, Inferior by almost two orders to that of EPMA for example. So we developed a new spectrometer with an improved resolution of better than 20um and almost the same sensitivity.

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Spatial resolution of X-ray microanalysis in thin foils

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100109860 ◽

1978 ◽

Vol 36 (1) ◽

pp. 544-545

Author(s):

R. Hutchings ◽

I.P. Jones ◽

M.H. Loretto ◽

R.E. Smallman

Keyword(s):

Spatial Resolution ◽

Electron Probe ◽

Beam Divergence ◽

Inelastic Interaction ◽

Specimen Thickness ◽

High Current ◽

Beam Spreading ◽

X Ray ◽

Thin Foils ◽

Complex Calculation

There is increasing interest in X-ray microanalysis of thin specimens and the present paper attempts to define some of the factors which govern the spatial resolution of this type of microanalysis. One of these factors is the spreading of the electron probe as it is transmitted through the specimen. There will always be some beam-spreading with small electron probes, because of the inevitable beam divergence associated with small, high current probes; a lower limit to the spatial resolution is thus 2αst where 2αs is the beam divergence and t the specimen thickness.In addition there will of course be beam spreading caused by elastic and inelastic interaction between the electron beam and the specimen. The angle through which electrons are scattered by the various scattering processes can vary from zero to 180° and it is clearly a very complex calculation to determine the effective size of the beam as it propagates through the specimen.

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High spatial resolution x-ray microanalysis of interfaces

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100137793 ◽

1995 ◽

Vol 53 ◽

pp. 284-285

Author(s):

J. R. Michael

Keyword(s):

Spatial Resolution ◽

Electron Probe ◽

Solid Angle ◽

Collection Efficiency ◽

Spatial Scales ◽

Energy Dispersive Spectrometer ◽

X Rays ◽

X Ray ◽

Probe Size ◽

Brightness Field

X-ray microanalysis in the analytical electron microscope (AEM) refers to a technique by which chemical composition can be determined on spatial scales of less than 10 nm. There are many factors that influence the quality of x-ray microanalysis. The minimum probe size with sufficient current for microanalysis that can be generated determines the ultimate spatial resolution of each individual microanalysis. However, it is also necessary to collect efficiently the x-rays generated. Modern high brightness field emission gun equipped AEMs can now generate probes that are less than 1 nm in diameter with high probe currents. Improving the x-ray collection solid angle of the solid state energy dispersive spectrometer (EDS) results in more efficient collection of x-ray generated by the interaction of the electron probe with the specimen, thus reducing the minimum detectability limit. The combination of decreased interaction volume due to smaller electron probe size and the increased collection efficiency due to larger solid angle of x-ray collection should enhance our ability to study interfacial segregation.

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Scanning x-ray fluorescence microscopy and principal component analysis

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100133394 ◽

1992 ◽

Vol 50 (2) ◽

pp. 1752-1753

Author(s):

Brian Cross

Keyword(s):

Principal Component Analysis ◽

Fluorescence Microscopy ◽

Spatial Resolution ◽

High Speed ◽

Image Acquisition ◽

Principal Component ◽

Fluorescence Microscope ◽

Acquisition Rate ◽

X Ray ◽

Speed Up

A relatively new entry, in the field of microscopy, is the Scanning X-Ray Fluorescence Microscope (SXRFM). Using this type of instrument (e.g. Kevex Omicron X-ray Microprobe), one can obtain multiple elemental x-ray images, from the analysis of materials which show heterogeneity. The SXRFM obtains images by collimating an x-ray beam (e.g. 100 μm diameter), and then scanning the sample with a high-speed x-y stage. To speed up the image acquisition, data is acquired "on-the-fly" by slew-scanning the stage along the x-axis, like a TV or SEM scan. To reduce the overhead from "fly-back," the images can be acquired by bi-directional scanning of the x-axis. This results in very little overhead with the re-positioning of the sample stage. The image acquisition rate is dominated by the x-ray acquisition rate. Therefore, the total x-ray image acquisition rate, using the SXRFM, is very comparable to an SEM. Although the x-ray spatial resolution of the SXRFM is worse than an SEM (say 100 vs. 2 μm), there are several other advantages.

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Practical Importance of Spatial Resolution and Analytical Sensitivity in AEM X-ray Microanalysis

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100135769 ◽

1990 ◽

Vol 48 (2) ◽

pp. 432-433

Author(s):

J. Zhang ◽

D.B. Williams ◽

J.I. Goldstein

Keyword(s):

Spatial Resolution ◽

Practical Importance ◽

Beam Current ◽

Specimen Thickness ◽

Analytical Sensitivity ◽

Related Factors ◽

X Ray ◽

Probe Size ◽

Excitation Volume ◽

Two Parameters

Analytical sensitivity and spatial resolution are important and closely related factors in x-ray microanalysis using the AEM. Analytical sensitivity is the ability to distinguish, for a given element under given conditions, between two concentrations that are nearly equal. The analytical sensitivity is directly related to the number of x-ray counts collected and, therefore, to the probe current, specimen thickness and counting time. The spatial resolution in AEM analysis is determined by the probe size and beam broadening in the specimen. A finer probe and a thinner specimen give a higher spatial resolution. However, the resulting lower beam current and smaller X-ray excitation volume degrade analytical sensitivity. A compromise must be made between high spatial resolution and an acceptable analytical sensitivity. In this paper, we show the necessity of evaluating these two parameters in order to determine the low temperature Fe-Ni phase diagram.A Phillips EM400T AEM with an EDAX/TN2000 EDS/MCA system and a VG HB501 FEG STEM with a LINK AN10 EDS/MCA system were used.

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Low-voltage EDS of magnesium ferrite Dendrites in a FEG-SEM

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100164854 ◽

1996 ◽

Vol 54 ◽

pp. 478-479

Author(s):

Matthew T. Johnson ◽

Ian M. Anderson ◽

Jim Bentley ◽

C. Barry Carter

Keyword(s):

Monte Carlo ◽

Quantitative Analysis ◽

Monte Carlo Simulations ◽

Cross Section ◽

Spatial Resolution ◽

Low Voltage ◽

Magnesium Ferrite ◽

X Ray ◽

Interaction Volume ◽

Ferrite Spinel

Energy-dispersive X-ray spectrometry (EDS) performed at low (≤ 5 kV) accelerating voltages in the SEM has the potential for providing quantitative microanalytical information with a spatial resolution of ∼100 nm. In the present work, EDS analyses were performed on magnesium ferrite spinel [(MgxFe1−x)Fe2O4] dendrites embedded in a MgO matrix, as shown in Fig. 1. spatial resolution of X-ray microanalysis at conventional accelerating voltages is insufficient for the quantitative analysis of these dendrites, which have widths of the order of a few hundred nanometers, without deconvolution of contributions from the MgO matrix. However, Monte Carlo simulations indicate that the interaction volume for MgFe2O4 is ∼150 nm at 3 kV accelerating voltage and therefore sufficient to analyze the dendrites without matrix contributions.Single-crystal {001}-oriented MgO was reacted with hematite (Fe2O3) powder for 6 h at 1450°C in air and furnace cooled. The specimen was then cleaved to expose a clean cross-section suitable for microanalysis.

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