Fast, High-Resolution X-ray Microfluorescence Imaging

1990 ◽  
Vol 34 ◽  
pp. 217-221 ◽  
Author(s):  
D. A. Carpenter ◽  
M. A. Taylor

X-ray micro fluorescence imaging refers to the use of an x-ray beam as a probe to excite XRF in a specimen and produce a spatially resolved image of the element distribution. The advantages of high sensitivity and low background, together with the nondestructive nature of the measurement, have lead to applications of x-ray microfluorescence analysis in biology, geology, materials science, as well as in the area of nondestructive evaluation. Previous reports have described the development of an x-ray microprobe which uses a conventional source of x-rays to produce a 10-μm beam. This paper describes improvements to the microprobe which have increased the beam power and the solid angle of detection. The data collection and display software have also been enhanced.

1998 ◽  
Vol 4 (S2) ◽  
pp. 378-379
Author(s):  
Z. W. Chen ◽  
D. B. Wittry

A monochromatic x-ray microprobe based on a laboratory source has recently been developed in our laboratory and used for fluorescence excitation. This technique provides high sensitivity (ppm to ppb), nondestructive, quantitative microanalysis with minimum sample preparation and does not require a high vacuum specimen chamber. It is expected that this technique (MMXRF) will have important applications in materials science, geological sciences and biological science.Three-dimensional focusing of x-rays can be obtained by using diffraction from doubly curved crystals. In our MMXRF setup, a small x-ray source was produced by the bombardment of a selected target with a focused electron beam and a toroidal mica diffractor with Johann pointfocusing geometry was used to focus characteristic x-rays from the source. In the previous work ∼ 108 photons/s were obtained in a Cu Kα probe of 75 μm × 43 μm in the specimen plane using the fifth order reflection of the (002) planes of mica.


1997 ◽  
Vol 487 ◽  
Author(s):  
P. Fougères ◽  
Ch. Burggraf ◽  
Chr. Burggraf ◽  
J. M. Koebel ◽  
C. Koenig ◽  
...  

AbstractThe control of the concentration of Zn and its fluctuation in the high pressure Bridgman grown CdZnTe crystals is part of our characterization work on the ternary grown ingots grown in house. In order to reach both high sensitivity and high position resolution, we have developed a new system consisting of a X-ray generator, coupled to a focusing X-ray capillary, delivering intense beams in the micron scale, since the intensity gain is around a factor of 100 compared to conventional methods.The characteristic X-rays are measured through a high resolution CdZnTe detector (225 eV at 5.9 keV FWHM) cooled by a Peltier system. The results of our investigations on different kinds of crystals will be discussed.


1997 ◽  
Vol 3 (S2) ◽  
pp. 281-282
Author(s):  
Anthony J. Garratt-Reed

The Center for Materials Science and Engineering at MIT, a Materials Research Science and Engineering Center sponsored by the National Science Foundation, maintains and supports, amongst others, an Electron Microscopy Shared Experimental Facility. The purpose of this paper is to highlight selected recent research results for high-resolution investigations performed in that facility.The facility owns the first VG HB603 intermediate-voltage FEG-STEM, which operates at 250KeV and is equipped with a high-solid-angle x-ray detector and a Gatan Digi-Peels. It was intended to be, and has been, used for high sensitivity, high spatial resolution microanalysis. It is well-known that the “resolution” of an x-ray analysis is intimately (and inversely) related to its sensitivity; one extreme situation occurs when analyzing, for example, a diffusion profile, when the need is to determine the composition to the highest precision. An example of such an analysis is given in fig. 1. In this case, the sample is a 1.4Cr-0.8C pearlitic steel, and the chromium analysis is carried out across a cementite plate. During the growth of the pearlite, the chromium, which is not thermodynamically required to redistribute, nevertheless diffuses along the growth interface towards the cementite, resulting in a comparatively wide depletion profile in the ferrite, and a very narrow enrichment in the cementite.


2015 ◽  
Vol 825-826 ◽  
pp. 814-821 ◽  
Author(s):  
Bernd R. Müller ◽  
Fabien Léonard ◽  
Axel Lange ◽  
Andreas Kupsch ◽  
Giovanni Bruno

X-ray refraction is based on optical deflection of X-rays, similar to the well-known small angle X-ray scattering, but hundreds of times more intense, thus enabling shorter measurement time. We show that X-ray refraction techniques are suitable for the detection of pores, cracks, and in general defects. Indeed, the deflected X-ray intensity is directly proportional to the internal specific surface (i.e., surface per unit volume) of the objects. Although single defects cannot be imaged, the presence of populations of those defects can be detected even if the defects have sizes in the nanometer range.We present several applications of X-ray refraction techniques to composite materials:- To visualize macro and microcracks in Ti-SiC metal matrix composites (MMC);- To correlate fatigue damage (fibre de-bonding) of carbon fibre reinforced plastics (CFRP) to X-ray refraction intensity;- To quantify the impact damage by spatially resolved single fibre de-bonding fraction as a function of impact energy in CFRP laminates.An example of classic high-resolution computer tomography of an impact-damaged CFRP will also be presented, as a benchmark to the present state-of-the-art imaging capabilities. It will be shown that while (absorption) tomography can well visualize and quantify delamination, X-ray refraction techniques directly yield (spatially resolved) quantitative information about fibre de-bonding, inaccessible to absorption tomography.


Author(s):  
J. R. Michael

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.


Author(s):  
D. A. Carpenter ◽  
M. A. Taylor

The development of intense sources of x rays has led to renewed interest in the use of microbeams of x rays in x-ray fluorescence analysis. Sparks pointed out that the use of x rays as a probe offered the advantages of high sensitivity, low detection limits, low beam damage, and large penetration depths with minimal specimen preparation or perturbation. In addition, the option of air operation provided special advantages for examination of hydrated systems or for nondestructive microanalysis of large specimens.The disadvantages of synchrotron sources prompted the development of laboratory-based instrumentation with various schemes to maximize the beam flux while maintaining small point-to-point resolution. Nichols and Ryon developed a microprobe using a rotating anode source and a modified microdiffractometer. Cross and Wherry showed that by close-coupling the x-ray source, specimen, and detector, good intensities could be obtained for beam sizes between 30 and 100μm. More importantly, both groups combined specimen scanning with modern imaging techniques for rapid element mapping.


Author(s):  
Y. Sato ◽  
T. Hashimoto ◽  
M. Ichihashi ◽  
Y. Ueki ◽  
K. Hirose ◽  
...  

Analytical TEMs have two variations in x-ray detector geometry, high and low angle take off. The high take off angle is advantageous for accuracy of quantitative analysis, because the x rays are less absorbed when they go through the sample. The low take off angle geometry enables better sensitivity because of larger detector solid angle.Hitachi HF-2000 cold field emission TEM has two versions; high angle take off and low angle take off. The former allows an energy dispersive x-ray detector above the objective lens. The latter allows the detector beside the objective lens. The x-ray take off angle is 68° for the high take off angle with the specimen held at right angles to the beam, and 22° for the low angle take off. The solid angle is 0.037 sr for the high angle take off, and 0.12 sr for the low angle take off, using a 30 mm2 detector.


2021 ◽  
Vol 11 (4) ◽  
pp. 1446
Author(s):  
Jacopo Orsilli ◽  
Anna Galli ◽  
Letizia Bonizzoni ◽  
Michele Caccia

Among the possible variants of X-Ray Fluorescence (XRF), applications exploiting scanning Macro-XRF (MA-XRF) are lately widespread as they allow the visualization of the element distribution maintaining a non-destructive approach. The surface is scanned with a focused or collimated X-ray beam of millimeters or less: analyzing the emitted fluorescence radiation, also elements present below the surface contribute to the elemental distribution image obtained, due to the penetrative nature of X-rays. The importance of this method in the investigation of historical paintings is so obvious—as the elemental distribution obtained can reveal hidden sub-surface layers, including changes made by the artist, or restorations, without any damage to the object—that recently specific international conferences have been held. The present paper summarizes the advantages and limitations of using MA-XRF considering it as an imaging technique, in synergy with other hyperspectral methods, or combining it with spot investigations. The most recent applications in the cultural Heritage field are taken into account, demonstrating how obtained 2D-XRF maps can be of great help in the diagnostic applied on Cultural Heritage materials. Moreover, a pioneering analysis protocol based on the Spectral Angle Mapper (SAM) algorithm is presented, unifying the MA-XRF standard approach with punctual XRF, exploiting information from the mapped area as a database to extend the comprehension to data outside the scanned region, and working independently from the acquisition set-up. Experimental application on some reference pigment layers and a painting by Giotto are presented as validation of the proposed method.


1998 ◽  
Vol 5 (3) ◽  
pp. 515-517 ◽  
Author(s):  
M. Frank ◽  
C. A. Mears ◽  
S. E. Labov ◽  
L. J. Hiller ◽  
J. B. le Grand ◽  
...  

Experimental results are presented obtained with a cryogenically cooled high-resolution X-ray spectrometer based on a 141 × 141 µm Nb-Al-Al2O3-Al-Nb superconducting tunnel junction (STJ) detector in an SR-XRF demonstration experiment. STJ detectors can operate at count rates approaching those of semiconductor detectors while still providing a significantly better energy resolution for soft X-rays. By measuring fluorescence X-rays from samples containing transition metals and low-Z elements, an FWHM energy resolution of 6–15 eV for X-rays in the energy range 180–1100 eV has been obtained. The results show that, in the near future, STJ detectors may prove very useful in XRF and microanalysis applications.


2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.


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