scholarly journals High-sensitivity nanoscale chemical imaging with hard x-ray nano-XANES

2020 ◽  
Vol 6 (37) ◽  
pp. eabb3615 ◽  
Author(s):  
A. Pattammattel ◽  
R. Tappero ◽  
M. Ge ◽  
Y. S. Chu ◽  
X. Huang ◽  
...  
Keyword(s):  
Lithium Iron Phosphate ◽  
Reference Sample ◽  
Chemical Species ◽  
High Sensitivity ◽  
Chemical Imaging ◽  
Resolving Power ◽  
X Rays ◽  
Secondary Phases ◽  
Edge Structure ◽  
X Ray

Resolving chemical species at the nanoscale is of paramount importance to many scientific and technological developments across a broad spectrum of disciplines. Hard x-rays with excellent penetration power and high chemical sensitivity are suitable for speciation of heterogeneous (thick) materials. Here, we report nanoscale chemical speciation by combining scanning nanoprobe and fluorescence-yield x-ray absorption near-edge structure (nano-XANES). First, the resolving power of nano-XANES was demonstrated by mapping Fe(0) and Fe(III) states of a reference sample composed of stainless steel and hematite nanoparticles with 50-nm scanning steps. Nano-XANES was then used to study the trace secondary phases in lithium iron phosphate (LFP) particles. We observed individual Fe-phosphide nanoparticles in pristine LFP, whereas partially (de)lithiated particles showed Fe-phosphide nanonetworks. These findings shed light on the contradictory reports on Fe-phosphide morphology in the literature. Nano-XANES bridges the capability gap of spectromicroscopy methods and provides exciting research opportunities across multiple disciplines.

Chemical Species Identification in an SEM by Changes in Emitted X-Ray Energies

1974 ◽  
Vol 32 ◽  
pp. 570-571
Author(s):  
R. H. Duff
Keyword(s):  
Species Identification ◽  
Valence Electron ◽  
Chemical Species ◽  
X Rays ◽  
Chemical Bonds ◽  
Small Shift ◽  
X Ray ◽  
Electron Transitions ◽  
Peak Energy ◽  
Chemical Combination

A material irradiated with electrons emits x-rays having energies characteristic of the elements present. Chemical combination between elements results in a small shift of the peak energies of these characteristic x-rays because chemical bonds between different elements have different energies. The energy differences of the characteristic x-rays resulting from valence electron transitions can be used to identify the chemical species present and to obtain information about the chemical bond itself. Although these peak-energy shifts have been well known for a number of years, their use for chemical-species identification in small volumes of material was not realized until the development of the electron microprobe.

An x-ray microprobe based upon a close-coupled focal-spot / glass capillary arrangement

1992 ◽  
Vol 50 (2) ◽  
pp. 1758-1759
Author(s):  
D. A. Carpenter ◽  
M. A. Taylor
Keyword(s):  
Imaging Techniques ◽  
Fluorescence Analysis ◽  
High Sensitivity ◽  
Specimen Preparation ◽  
X Rays ◽  
Glass Capillary ◽  
Close Coupling ◽  
X Ray ◽  
Point To Point ◽  
Beam Damage

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.

scholarly journals Physical and chemical imaging of adhesive interfaces with soft X-rays

2021 ◽  
Vol 2 (1) ◽  
Author(s):  
Hiroyuki Yamane ◽  
Masaki Oura ◽  
Osamu Takahashi ◽  
Tomoko Ishihara ◽  
Noriko Yamazaki ◽  
...  
Keyword(s):  
Molecular Level ◽  
Covalent Bond ◽  
Chemical Imaging ◽  
Diglycidyl Ether ◽  
X Rays ◽  
X Ray ◽  
Covalent Bond Formation ◽  
Chemical States ◽  
The Individual ◽  
Physical And Chemical

AbstractAdhesion is an interfacial phenomenon that is critical for assembling carbon structural composites for next-generation aircraft and automobiles. However, there is limited understanding of adhesion on the molecular level because of the difficulty in revealing the individual bonding factors. Here, using soft X-ray spectromicroscopy we show the physical and chemical states of an adhesive interface composed of a thermosetting polymer of 4,4’-diaminodiphenylsulfone-cured bisphenol A diglycidyl ether adhered to a thermoplastic polymer of plasma-treated polyetheretherketone. We observe multiscale phenomena in the adhesion mechanisms, including sub-mm complex interface structure, sub-μm distribution of the functional groups, and molecular-level covalent-bond formation. These results provide a benchmark for further research to examine how physical and chemical states correlate with adhesion, and demonstrate that soft X-ray imaging is a promising approach for visualizing the physical and chemical states at adhesive interfaces from the sub-mm level to the molecular level.

Recent Developments In Monochromatic Microprobe X-Ray Fluorescence (MMXRF)

1998 ◽  
Vol 4 (S2) ◽  
pp. 378-379
Author(s):  
Z. W. Chen ◽  
D. B. Wittry
Keyword(s):  
Materials Science ◽  
High Vacuum ◽  
Three Dimensional ◽  
High Sensitivity ◽  
X Rays ◽  
Fluorescence Excitation ◽  
X Ray ◽  
Quantitative Microanalysis ◽  
Recent Developments ◽  
Fifth Order

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.

scholarly journals The XXL Survey

2018 ◽  
Vol 620 ◽  
pp. A18 ◽  
Author(s):  
C. H. A. Logan ◽  
B. J. Maughan ◽  
M. N. Bremer ◽  
P. Giles ◽  
M. Birkinshaw ◽  
...  
Keyword(s):  
Angular Resolution ◽  
False Positive Rate ◽  
High Sensitivity ◽  
Point Sources ◽  
Selection Function ◽  
X Rays ◽  
Cluster Emission ◽  
X Ray ◽  
Wide Range ◽  
Function Modelling

Context. The XMM-XXL survey has used observations from the XMM-Newton observatory to detect clusters of galaxies over a wide range in mass and redshift. The moderate PSF (FWHM ~ 6″ on-axis) of XMM-Newton means that point sources within or projected onto a cluster may not be separated from the cluster emission, leading to enhanced luminosities and affecting the selection function of the cluster survey. Aims. We present the results of short Chandra observations of 21 galaxy clusters and cluster candidates at redshifts z > 1 detected in the XMM-XXL survey in X-rays or selected in the optical and infra-red. Methods. With the superior angular resolution of Chandra, we investigate whether there are any point sources within the cluster region that were not detected by the XMM-XXL analysis pipeline, and whether any point sources were misclassified as distant clusters. Results. Of the 14 X-ray selected clusters, 9 are free from significant point source contamination, either having no previously unresolved sources detected by Chandra or with less than about 10% of the reported XXL cluster flux being resolved into point sources. Of the other five sources, one is significantly contaminated by previously unresolved AGN, and four appear to be AGN misclassified as clusters. All but one of these cases are in the subset of less secure X-ray selected cluster detections and the false positive rate is consistent with that expected from the XXL selection function modelling. We also considered a further seven optically selected cluster candidates associated with faint XXL sources that were not classed as clusters. Of these, three were shown to be AGN by Chandra, one is a cluster whose XXL survey flux was highly contaminated by unresolved AGN, while three appear to be uncontaminated clusters. By decontaminating and vetting these distant clusters, we provide a pure sample of clusters at redshift z > 1 for deeper follow-up observations, and demonstrate the utility of using Chandra snapshots to test for AGN in surveys with high sensitivity but poor angular resolution.

Early commissioning results for spectroscopic X-ray Nano-Imaging Beamline BL 7C sXNI at PLS-II

2017 ◽  
Vol 24 (6) ◽  
pp. 1276-1282 ◽  
Author(s):  
Sangsul Lee ◽  
Ik hwan Kwon ◽  
Jae-Young Kim ◽  
Sung-Sun Yang ◽  
Sechang Kang ◽  
...  
Keyword(s):  
Lithium Iron Phosphate ◽  
Phase Distribution ◽  
Lithium Ion ◽  
Feedback System ◽  
Double Crystal ◽  
Pilot Studies ◽  
Beam Position ◽  
Edge Structure ◽  
X Ray

For spectral imaging of chemical distributions using X-ray absorption near-edge structure (XANES) spectra, a modified double-crystal monochromator, a focusing plane mirrors system and a newly developed fluorescence-type X-ray beam-position monitoring and feedback system have been implemented. This major hardware upgrade provides a sufficiently stable X-ray source during energy scanning of more than hundreds of eV for acquisition of reliable XANES spectra in two-dimensional and three-dimensional images. In recent pilot studies discussed in this paper, heavy-metal uptake by plant rootsin vivoand iron's phase distribution in the lithium–iron–phosphate cathode of a lithium-ion battery have been imaged. Also, the spatial resolution of computed tomography has been improved from 70 nm to 55 nm by means of run-out correction and application of a reconstruction algorithm.

scholarly journals The sensitivity of atomic analysis by X-rays

1932 ◽  
Vol 135 (828) ◽  
pp. 637-656 ◽  
Keyword(s):  
Atomic Number ◽  
Target Material ◽  
High Sensitivity ◽  
Major Constituent ◽  
X Rays ◽  
Depth Of Penetration ◽  
X Ray ◽  
Constituent Element ◽  
The Difference ◽  
Atomic Analysis

In a previous paper it was shown that 0·0007 per cent, of 29 Cu and 0·0003 per cent, of 26 Fe could be detected in 30 Zn by atomic analysis by X-ray spectroscopy. This sensitivity is greater than that which was claimed by Noddack, Tacke, and Berg, who set the limit at about 0·1 per cent, for non-metals, and by Hevesy, who stated it to be about 0·01 per cent, for an element present in an alloy. It was later suggested by Hevesy that the high value of the sensitivity which we found might result from the fact that some of the alloys we had used were composed of elements of almost equal atomic number, and that the sensitivity would be smaller for a constituent of low atomic number mixed with a major constituent of high atomic number. To elucidate these disagreements we have made further observations of the sensitivity with elements of different atomic number and have investigated the conditions which can influence the sensitivity. The Factors Determining Sensitivity . The detection of one element in a mixture of elements depends upon the identification of its K or L lines in the general spectrum emitted by the mixture under examination. The intensity with which these lines are excited in the target (“excited intensity”) is proportional to the number of atoms of the constituent element excited, i. e ., to its concentration and to the volume of the target in which the cathode ray energy is absorbed. The depth of penetration of the cathode rays is determined by the density of the target material and by their velocity ( i. e ., by the voltage applied to the X-ray tube). Schonland has shown that the range of homogeneous cathode rays in different elements, expressed as a mass per unit area, is approximately constant and is independent of the atomic number of the absorbing element. When their velocity is increased, the cathode rays will penetrate to a greater depth, and therefore a greater number of atoms of all constituents will be ionised. This will increase the “excited intensity” of the lines due to the particular constituent sought equally with those lines of the other elements present. The intensity of a line further depends upon the difference between the voltage applied to the X-ray tube and that necessary to excite the series. For these reasons, a high applied voltage is required for a high sensitivity.

scholarly journals Testing the disk-corona interplay in radiatively-efficient broad-line AGN

2019 ◽  
Vol 628 ◽  
pp. A135 ◽  
Author(s):  
R. Arcodia ◽  
A. Merloni ◽  
K. Nandra ◽  
G. Ponti
Keyword(s):  
Accretion Disk ◽  
Reference Sample ◽  
Selection Effect ◽  
Galactic Nuclei ◽  
Theoretical Explanation ◽  
X Rays ◽  
Broad Line ◽  
Coronal Emission ◽  
X Ray ◽  
Intrinsic Scatter

The correlation observed between monochromatic X-ray and UV luminosities in radiatively-efficient active galactic nuclei (AGN) lacks a clear theoretical explanation despite being used for many applications. Such a correlation, with its small intrinsic scatter and its slope that is smaller than unity in log space, represents the compelling evidence that a mechanism regulating the energetic interaction between the accretion disk and the X-ray corona must be in place. This ensures that going from fainter to brighter sources the coronal emission increases less than the disk emission. We discuss here a self-consistently coupled disk-corona model that can identify this regulating mechanism in terms of modified viscosity prescriptions in the accretion disk. The model predicts a lower fraction of accretion power dissipated in the corona for higher accretion states. We then present a quantitative observational test of the model using a reference sample of broad-line AGN and modeling the disk-corona emission for each source in the LX − LUV plane. We used the slope, normalization, and scatter of the observed relation to constrain the parameters of the theoretical model. For non-spinning black holes and static coronae, we find that the accretion prescriptions that match the observed slope of the LX − LUV relation produce X-rays that are too weak with respect to the normalization of the observed relation. Instead, considering moderately-outflowing Comptonizing coronae and/or a more realistic high-spinning black hole population significantly relax the tension between the strength of the observed and modeled X-ray emission, while also predicting very low intrinsic scatter in the LX − LUV relation. In particular, this latter scenario traces a known selection effect of flux-limited samples that preferentially select high-spinning, hence brighter, sources.

Parameters Affecting X-Ray Microfluorescence (XRMF) Analysis

1986 ◽  
Vol 30 ◽  
pp. 45-51 ◽  
Author(s):  
Monte C. Nichols ◽  
Dale R. Boehme ◽  
Richard W. Ryon ◽  
David Wherry ◽  
Brian Cross ◽  
...  
Keyword(s):  
Analytical Techniques ◽  
High Sensitivity ◽  
Sample Surface ◽  
Chemical Information ◽  
X Rays ◽  
X Ray ◽  
Minimal Sample ◽  
Small X ◽  
Fluorescent Radiation ◽  
Channel Analyzer

AbstractX-ray Microfluorescence (XRMF) analysis uses a finely collimated beam of X-rays to excite fluorescent radiation in a sample (Nichols & Ryon 1986). Characteristic fluorescent radiation emanating from the small interaction volume element is acquired using an energy dispersive detector placed in close proximity to the sample. The signal from the detector is processed using a computer-based multi-channel analyzer.XRMF imaging is accomplished by translating the sample through the small X-ray beam in a step or continuous raster mode. As the sample is translated, a pixel by pixel X-ray intensity image is formed for each chemical element in the sample. The resulting digitized image information for each element is stored for subsequent processing and/or display. The images, in the form of elemental maps representing identical areas, may be displayed and color coded by element and/or intensity and then overlayed for spatial correlation.The present study of parameters affecting the performance of an X-ray microfluorescence system has shown how such systems use X-ray beams with effective spot sizes less than 100 micrometers to bridge the gap in analytical capabilities between predominately surface micro analytical techniques such as SEM/EDX and bulk analytical methods such as standard XRF analysis. The combination of XRMF spectroscopy with digital imaging allows chemical information to be obtained and mapped from surface layers as well as from layers or structures beneath the sample surface. Simultaneously, it provides valuable high resolution chemical information in a readily interpreted visual form which displays the homogeneity within a given layer or structure. XRMF systems retain the advantages of minimal sample preparation, non-destructive analysis and high sensitivity inherent to XRF methods.

Applications of a Laboratory X-ray Micropsobe to Materials Analysis

1988 ◽  
Vol 32 ◽  
pp. 115-120 ◽  
Author(s):  
D. A. Carpenter ◽  
M. A. Taylor ◽  
C. E. Holcombe
Keyword(s):  
Spatial Resolution ◽  
High Spatial Resolution ◽  
High Sensitivity ◽  
Specimen Preparation ◽  
X Rays ◽  
Glass Capillary ◽  
Materials Analysis ◽  
X Ray ◽  
Small Glass

A laboratory-based X-ray microprobe, composed of a high-brilliance microfocus X-ray tube, coupled with a small glass capillary, has been developed for materials applications. Because of total external reflectance of X rays from the smooth inside bore of the glass capillary, the microprobe has a high sensitivity as well as a high spatial resolution. The use of X rays to excite elemental fluorescence offers the advantages of good peak-to-background, the ability to operate in air, and minimal specimen preparation. In addition, the development of laboratory-based instrumentation has been of Interest recently because of greater accessibility when compared with synchrotron X-ray microprobes.

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