Soft x-ray spectroscopy of high pressure liquid

DOE PAGES

Qiao, Ruimin; Xia, Yujian; Feng, Xuefei; ...

2018-01-01

Here, we describe a new experimental technique that allows for soft x-ray spectroscopy studies (~100-1000 eV) of high pressure liquid (~100 bars). We achieve this through a liquid cell with a 100 nm-thick Si 3N 4 membrane window, which is sandwiched by two identical O-rings for vacuum sealing. The thin Si 3N 4 membrane allows soft x-rays to penetrate, while separating the high-pressure liquid under investigation from the vacuum required for soft x-ray transmission and detection. The burst pressure of the Si 3N 4 membrane increases with decreasing size and more specifically is inversely proportional to the side length ofmore » the square window. It also increases proportionally with the membrane thickness. Pressures > 60 bars could be achieved for 100 nm-thick square Si 3N 4 windows that are smaller than 65 μm. However, above a certain pressure, the failure of the Si wafer becomes the limiting factor. The failure pressure of the Si wafer is sensitive to the wafer thickness. Moreover, the deformation of the Si 3N 4 membrane is quantified using vertical scanning interferometry. As an example of the performance of the high-pressure liquid cell optimized for total-fluorescence detected soft x-ray absorption spectroscopy (sXAS), the sXAS spectra at the Ca L edge (~350 eV) of a CaCl 2 aqueous solution are collected under different pressures up to 41 bars.« less

Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

DOE PAGES

Miaja-Avila, L.; O'Neil, G. C.; Uhlig, J.; ...

2015-03-02

We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ~10 6 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >10 7 laser pulses, wemore » also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.« less

Note: application of a pixel-array area detector to simultaneous single crystal X-ray diffraction and X-ray absorption spectroscopy measurements.

PubMed

Sun, Cheng-Jun; Zhang, Bangmin; Brewe, Dale L; Chen, Jing-Sheng; Chow, G M; Venkatesan, T; Heald, Steve M

2014-04-01

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr0.67Sr0.33MnO3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.

Scanning transmission x-ray microscope for materials science spectromicroscopy at the ALS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Warwick, T.; Seal, S.; Shin, H.

1997-04-01

The brightness of the Advanced Light Source will be exploited by several new instruments for materials science spectromicroscopy over the next year or so. The first of these to become operational is a scanning transmission x-ray microscope with which near edge x-ray absorption spectra (NEXAFS) can be measured on spatial features of sub-micron size. Here the authors describe the instrument as it is presently implemented, its capabilities, some studies made to date and the developments to come. The Scanning Transmission X-ray Microscope makes use of a zone plate lens to produce a small x-ray spot with which to perform absorptionmore » spectroscopy through thin samples. The x-ray beam from ALS undulator beamline 7.0 emerges into the microscope vessel through a silicon nitride vacuum window 160nm thick and 300{mu}m square. The vessel is filled with helium at atmospheric pressure. The zone plate lens is illuminated 1mm downstream from the vacuum window and forms an image in first order of a pinhole which is 3m upstream in the beamline. An order sorting aperture passes the first order converging light and blocks the unfocused zero order. The sample is at the focus a few mm downstream of the zone plate and mounted from a scanning piezo stage which rasters in x and y so that an image is formed, pixel by pixel, by an intensity detector behind the sample. Absorption spectra are measured point-by-point as the photon energy is scanned by rotating the diffraction grating in the monochromator and changing the undulator gap.« less

A whole-system approach to x-ray spectroscopy in cargo inspection systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Langeveld, Willem G. J.; Gozani, Tsahi; Ryge, Peter

The bremsstrahlung x-ray spectrum used in high-energy, high-intensity x-ray cargo inspection systems is attenuated and modified by the materials in the cargo in a Z-dependent way. Therefore, spectroscopy of the detected x rays yields information about the Z of the x-rayed cargo material. It has previously been shown that such ZSpectroscopy (Z-SPEC) is possible under certain circumstances. A statistical approach, Z-SCAN (Z-determination by Statistical Count-rate ANalysis), has also been shown to be effective, and it can be used either by itself or in conjunction with Z-SPEC when the x-ray count rate is too high for individual x-ray spectroscopy. Both techniquesmore » require fast x-ray detectors and fast digitization electronics. It is desirable (and possible) to combine all techniques, including x-ray imaging of the cargo, in a single detector array, to reduce costs, weight, and overall complexity. In this paper, we take a whole-system approach to x-ray spectroscopy in x-ray cargo inspection systems, and show how the various parts interact with one another. Faster detectors and read-out electronics are beneficial for both techniques. A higher duty-factor x-ray source allows lower instantaneous count rates at the same overall x-ray intensity, improving the range of applicability of Z-SPEC in particular. Using an intensity-modulated advanced x-ray source (IMAXS) allows reducing the x-ray count rate for cargoes with higher transmission, and a stacked-detector approach may help material discrimination for the lowest attenuations. Image processing and segmentation allow derivation of results for entire objects, and subtraction of backgrounds. We discuss R and D performed under a number of different programs, showing progress made in each of the interacting subsystems. We discuss results of studies into faster scintillation detectors, including ZnO, BaF{sub 2} and PbWO{sub 4}, as well as suitable photo-detectors, read-out and digitization electronics. We discuss high

X-Ray Scan Detection for Cargo Integrity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Valencia, Juan D.; Miller, Steven D.

ABSTRACT The increase of terrorism and its global impact has made the determination of the contents of cargo containers a necessity. Existing technology allows non-intrusive inspections to determine the contents of a container rapidly and accurately. However, some cargo shipments are exempt from such inspections. Hence, there is a need for a technology that enables rapid and accurate means of detecting whether such containers were non-intrusively inspected. Non-intrusive inspections are most commonly performed utilizing high powered X-ray equipment. The challenge is creating a device that can detect short duration X-ray scans while maintaining a portable, battery powered, low cost, andmore » easy to use platform. The Pacific Northwest National Laboratory (PNNL) has developed a methodology and prototype device focused on this challenge. The prototype, developed by PNNL, is a battery powered electronic device that continuously measures its X-ray and Gamma exposure, calculates the dose equivalent rate, and makes a determination of whether the device has been exposed to the amount of radiation experienced during an X-ray inspection. Once an inspection is detected, the device will record a timestamp of the event and relay the information to authorized personnel via a visual alert, USB connection, and/or wireless communication. The results of this research demonstrate that PNNL’s prototype device can be effective at determining whether a container was scanned by X-ray equipment typically used for cargo container inspections. This paper focuses on laboratory measurements and test results acquired with the PNNL prototype device using several X-ray radiation levels. Keywords: Radiation, Scan, X-ray, Gamma, Detection, Cargo, Container, Wireless, RF« less

Ultrafast X-Ray Spectroscopy of Conical Intersections

NASA Astrophysics Data System (ADS)

Neville, Simon P.; Chergui, Majed; Stolow, Albert; Schuurman, Michael S.

2018-06-01

Ongoing developments in ultrafast x-ray sources offer powerful new means of probing the complex nonadiabatically coupled structural and electronic dynamics of photoexcited molecules. These non-Born-Oppenheimer effects are governed by general electronic degeneracies termed conical intersections, which play a key role, analogous to that of a transition state, in the electronic-nuclear dynamics of excited molecules. Using high-level ab initio quantum dynamics simulations, we studied time-resolved x-ray absorption (TRXAS) and photoelectron spectroscopy (TRXPS) of the prototypical unsaturated organic chromophore, ethylene, following excitation to its S2(π π*) state. The TRXAS, in particular, is highly sensitive to all aspects of the ensuing dynamics. These x-ray spectroscopies provide a clear signature of the wave packet dynamics near conical intersections, related to charge localization effects driven by the nuclear dynamics. Given the ubiquity of charge localization in excited state dynamics, we believe that ultrafast x-ray spectroscopies offer a unique and powerful route to the direct observation of dynamics around conical intersections.

Solar X-Ray and Gamma-Ray Imaging Spectroscopy

NASA Astrophysics Data System (ADS)

Dennis, B. R.; Christe, S. D.; Shih, A. Y.; Holman, G. D.; Emslie, A. G.; Caspi, A.

2018-02-01

X-ray and gamma-ray Sun observations from a lunar-based observatory would provide unique information on solar atmosphere thermal and nonthermal processes. EUV and energetic neutral atom imaging spectroscopy would augment the scientific value.

X-ray echo spectroscopy (Conference Presentation)

NASA Astrophysics Data System (ADS)

Shvyd'ko, Yuri V.

2016-09-01

X-ray echo spectroscopy, a counterpart of neutron spin-echo, was recently introduced [1] to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a point-like x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x-rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-meV and 0.02-meV ultra-high-resolution IXS applications (resolving power > 10^8) with broadband 5-13 meV dispersing systems will be presented featuring more than 1000-fold signal enhancement. The technique is general, applicable in different photon frequency domains. [1.] Yu. Shvyd'ko, Phys. Rev. Lett. 116, accepted (2016), arXiv:1511.01526.

X-ray absorption spectroscopy using a self-seeded soft X-ray free-electron laser

DOE PAGES

Kroll, Thomas; Kern, Jan; Kubin, Markus; ...

2016-09-19

X-ray free electron lasers (XFELs) enable unprecedented new ways to study the electronic structure and dynamics of transition metal systems. L-edge absorption spectroscopy is a powerful technique for such studies and the feasibility of this method at XFELs for solutions and solids has been demonstrated. But, the required x-ray bandwidth is an order of magnitude narrower than that of self-amplified spontaneous emission (SASE), and additional monochromatization is needed. We compare L-edge x-ray absorption spectroscopy (XAS) of a prototypical transition metal system based on monochromatizing the SASE radiation of the linac coherent light source (LCLS) with a new technique based onmore » self-seeding of LCLS. We demonstrate how L-edge XAS can be performed using the self-seeding scheme without the need of an additional beam line monochromator. Lastly, we show how the spectral shape and pulse energy depend on the undulator setup and how this affects the x-ray spectroscopy measurements.« less

X-ray absorption spectroscopy using a self-seeded soft X-ray free-electron laser

PubMed Central

Kroll, Thomas; Kern, Jan; Kubin, Markus; Ratner, Daniel; Gul, Sheraz; Fuller, Franklin D.; Löchel, Heike; Krzywinski, Jacek; Lutman, Alberto; Ding, Yuantao; Dakovski, Georgi L.; Moeller, Stefan; Turner, Joshua J.; Alonso-Mori, Roberto; Nordlund, Dennis L.; Rehanek, Jens; Weniger, Christian; Firsov, Alexander; Brzhezinskaya, Maria; Chatterjee, Ruchira; Lassalle-Kaiser, Benedikt; Sierra, Raymond G.; Laksmono, Hartawan; Hill, Ethan; Borovik, Andrew; Erko, Alexei; Föhlisch, Alexander; Mitzner, Rolf; Yachandra, Vittal K.; Yano, Junko; Wernet, Philippe; Bergmann, Uwe

2016-01-01

X-ray free electron lasers (XFELs) enable unprecedented new ways to study the electronic structure and dynamics of transition metal systems. L-edge absorption spectroscopy is a powerful technique for such studies and the feasibility of this method at XFELs for solutions and solids has been demonstrated. However, the required x-ray bandwidth is an order of magnitude narrower than that of self-amplified spontaneous emission (SASE), and additional monochromatization is needed. Here we compare L-edge x-ray absorption spectroscopy (XAS) of a prototypical transition metal system based on monochromatizing the SASE radiation of the linac coherent light source (LCLS) with a new technique based on self-seeding of LCLS. We demonstrate how L-edge XAS can be performed using the self-seeding scheme without the need of an additional beam line monochromator. We show how the spectral shape and pulse energy depend on the undulator setup and how this affects the x-ray spectroscopy measurements. PMID:27828320

Automatic tool alignment in a backscatter X-ray scanning system

DOEpatents

Garretson, Justin; Hobart, Clinton G.; Gladwell, Thomas S.; Monda, Mark J.

2015-11-17

Technologies pertaining to backscatter x-ray scanning systems are described herein. The backscatter x-ray scanning system includes an x-ray source, which directs collimated x-rays along a plurality of output vectors towards a target. A detector detects diffusely reflected x-rays subsequent to respective collimated x-rays impacting the target, and outputs signals indicative of parameters of the detected x-rays. An image processing system generates an x-ray image based upon parameters of the detected x-rays, wherein each pixel in the image corresponds to a respective output vector. A user selects a particular portion of the image, and a medical device is positioned such that its directional axis is coincident with the output vector corresponding to at least one pixel in the portion of the image.

Automatic tool alignment in a backscatter x-ray scanning system

DOEpatents

Garretson, Justin; Hobart, Clinton G.; Gladwell, Thomas S.; Monda, Mark J.

2015-06-16

Technologies pertaining to backscatter x-ray scanning systems are described herein. The backscatter x-ray scanning system includes an x-ray source, which directs collimated x-rays along a plurality of output vectors towards a target. A detector detects diffusely reflected x-rays subsequent to respective collimated x-rays impacting the target, and outputs signals indicative of parameters of the detected x-rays. An image processing system generates an x-ray image based upon parameters of the detected x-rays, wherein each pixel in the image corresponds to a respective output vector. A user selects a particular portion of the image, and a tool is positioned such that its directional axis is coincident with the output vector corresponding to at least one pixel in the portion of the image.

In Situ Industrial Bimetallic Catalyst Characterization using Scanning Transmission Electron Microscopy and X-ray Absorption Spectroscopy at One Atmosphere and Elevated Temperature.

PubMed

Prestat, Eric; Kulzick, Matthew A; Dietrich, Paul J; Smith, Mr Matthew; Tien, Mr Eu-Pin; Burke, M Grace; Haigh, Sarah J; Zaluzec, Nestor J

2017-08-18

We have developed a new experimental platform for in situ scanning transmission electron microscope (STEM) energy dispersive X-ray spectroscopy (EDS) which allows real time, nanoscale, elemental and structural changes to be studied at elevated temperature (up to 1000 °C) and pressure (up to 1 atm). Here we demonstrate the first application of this approach to understand complex structural changes occurring during reduction of a bimetallic catalyst, PdCu supported on TiO 2 , synthesized by wet impregnation. We reveal a heterogeneous evolution of nanoparticle size, distribution, and composition with large differences in reduction behavior for the two metals. We show that the data obtained is complementary to in situ STEM electron energy loss spectroscopy (EELS) and when combined with in situ X-ray absorption spectroscopy (XAS) allows correlation of bulk chemical state with nanoscale changes in elemental distribution during reduction, facilitating new understanding of the catalytic behavior for this important class of materials. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

Energy dispersive X-ray analysis on an absolute scale in scanning transmission electron microscopy.

PubMed

Chen, Z; D'Alfonso, A J; Weyland, M; Taplin, D J; Allen, L J; Findlay, S D

2015-10-01

We demonstrate absolute scale agreement between the number of X-ray counts in energy dispersive X-ray spectroscopy using an atomic-scale coherent electron probe and first-principles simulations. Scan-averaged spectra were collected across a range of thicknesses with precisely determined and controlled microscope parameters. Ionization cross-sections were calculated using the quantum excitation of phonons model, incorporating dynamical (multiple) electron scattering, which is seen to be important even for very thin specimens. Copyright © 2015 Elsevier B.V. All rights reserved.

X-ray scan detection for cargo integrity

NASA Astrophysics Data System (ADS)

Valencia, Juan; Miller, Steve

2011-04-01

The increase of terrorism and its global impact has made the determination of the contents of cargo containers a necessity. Existing technology allows non-intrusive inspections to determine the contents of a container rapidly and accurately. However, some cargo shipments are exempt from such inspections. Hence, there is a need for a technology that enables rapid and accurate means of detecting whether such containers were non-intrusively inspected. Non-intrusive inspections are most commonly performed utilizing high powered X-ray equipment. The challenge is creating a device that can detect short duration X-ray scans while maintaining a portable, battery powered, low cost, and easy to use platform. The Pacific Northwest National Laboratory (PNNL) has developed a methodology and prototype device focused on this challenge. The prototype, developed by PNNL, is a battery powered electronic device that continuously measures its X-ray and Gamma exposure, calculates the dose equivalent rate, and makes a determination of whether the device has been exposed to the amount of radiation experienced during an X-ray inspection. Once an inspection is detected, the device will record a timestamp of the event and relay the information to authorized personnel via a visual alert, USB connection, and/or wireless communication. The results of this research demonstrate that PNNL's prototype device can be effective at determining whether a container was scanned by X-ray equipment typically used for cargo container inspections. This paper focuses on laboratory measurements and test results acquired with the PNNL prototype device using several X-ray radiation levels.

Imaging properties and its improvements of scanning/imaging x-ray microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takeuchi, Akihisa, E-mail: take@spring8.or.jp; Uesugi, Kentaro; Suzuki, Yoshio

A scanning / imaging X-ray microscope (SIXM) system has been developed at SPring-8. The SIXM consists of a scanning X-ray microscope with a one-dimensional (1D) X-ray focusing device and an imaging (full-field) X-ray microscope with a 1D X-ray objective. The motivation of the SIXM system is to realize a quantitative and highly-sensitive multimodal 3D X-ray tomography by taking advantages of both the scanning X-ray microscope using multi-pixel detector and the imaging X-ray microscope. Data acquisition process of a 2D image is completely different between in the horizontal direction and in the vertical direction; a 1D signal is obtained with themore » linear-scanning while the other dimensional signal is obtained with the imaging optics. Such condition have caused a serious problem on the imaging properties that the imaging quality in the vertical direction has been much worse than that in the horizontal direction. In this paper, two approaches to solve this problem will be presented. One is introducing a Fourier transform method for phase retrieval from one phase derivative image, and the other to develop and employ a 1D diffuser to produce an asymmetrical coherent illumination.« less

Differentiation of dental restorative materials combining energy-dispersive X-ray fluorescence spectroscopy and post-mortem CT.

PubMed

Merriam, Tim; Kaufmann, Rolf; Ebert, Lars; Figi, Renato; Erni, Rolf; Pauer, Robin; Sieberth, Till

2018-06-01

Today, post-mortem computed tomography (CT) is routinely used for forensic identification. Mobile energy-dispersive X-ray fluorescence (EDXRF) spectroscopy of a dentition is a method of identification that has the potential to be easier and cheaper than CT, although it cannot be used with every dentition. In challenging cases, combining both techniques could facilitate the process of identification and prove to be advantageous over chemical analyses. Nine dental restorative material brands were analyzed using EDXRF spectroscopy. Their differentiability was assessed by comparing each material's x-ray fluorescence spectrum and then comparing the spectra to previous research investigating differentiability in CT. To verify EDXRF's precision and accuracy, select dental specimens underwent comparative electron beam excited x-ray spectroscopy (EDS) scans, while the impact of the restorative surface area was studied by scanning a row of dental specimens with varying restorative surface areas (n = 10). EDXRF was able to differentiate all 36 possible pairs of dental filling materials; however, dual-energy CT was only able to differentiate 33 out of 36. The EDS scans showed correlating x-ray fluorescence peaks on the x-ray spectra compared to our EDXRF. In addition, the surface area showed no influence on the differentiability of the dental filling materials. EDXRF has the potential to facilitate corpse identification by differentiating and comparing restorative materials, providing more information compared to post-mortem CT alone. Despite not being able to explicitly identify a brand without a control sample or database, its fast and mobile use could accelerate daily routines or mass victim identification processes. To achieve this goal, further development of EDXRF scanners for this application and further studies evaluating the method within a specific routine need to be performed.

Simultaneous X-ray fluorescence and scanning X-ray diffraction microscopy at the Australian Synchrotron XFM beamline

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jones, Michael W. M.; Phillips, Nicholas W.; van Riessen, Grant A.

2016-08-11

Owing to its extreme sensitivity, quantitative mapping of elemental distributionsviaX-ray fluorescence microscopy (XFM) has become a key microanalytical technique. The recent realisation of scanning X-ray diffraction microscopy (SXDM) meanwhile provides an avenue for quantitative super-resolved ultra-structural visualization. The similarity of their experimental geometries indicates excellent prospects for simultaneous acquisition. Here, in both step- and fly-scanning modes, robust, simultaneous XFM-SXDM is demonstrated.

Recent applications of hard x-ray photoelectron spectroscopy

DOE PAGES

Weiland, Conan; Rumaiz, Abdul K.; Pianetta, Piero; ...

2016-05-05

Recent applications of hard x-ray photoelectron spectroscopy (HAXPES) demonstrate its many capabilities in addition to several of its limitations. Examples are given, including measurement of buried interfaces and materials under in-situ or in-operando conditions, as well as measurements under x-ray standing-wave and resonant excitation. We also present physical considerations that differentiate HAXPES from photoemission measurements utilizing soft and ultraviolet x rays.

Hard X-ray imaging spectroscopy of FOXSI microflares

NASA Astrophysics Data System (ADS)

Glesener, Lindsay; Krucker, Sam; Christe, Steven; Buitrago-Casas, Juan Camilo; Ishikawa, Shin-nosuke; Foster, Natalie

2015-04-01

The ability to investigate particle acceleration and hot thermal plasma in solar flares relies on hard X-ray imaging spectroscopy using bremsstrahlung emission from high-energy electrons. Direct focusing of hard X-rays (HXRs) offers the ability to perform cleaner imaging spectroscopy of this emission than has previously been possible. Using direct focusing, spectra for different sources within the same field of view can be obtained easily since each detector segment (pixel or strip) measures the energy of each photon interacting within that segment. The Focusing Optics X-ray Solar Imager (FOXSI) sounding rocket payload has successfully completed two flights, observing microflares each time. Flare images demonstrate an instrument imaging dynamic range far superior to the indirect methods of previous instruments like the RHESSI spacecraft.In this work, we present imaging spectroscopy of microflares observed by FOXSI in its two flights. Imaging spectroscopy performed on raw FOXSI images reveals the temperature structure of flaring loops, while more advanced techniques such as deconvolution of the point spread function produce even more detailed images.

X-ray-induced photo-chemistry and X-ray absorption spectroscopy of biological samples

PubMed Central

George, Graham N.; Pickering, Ingrid J.; Pushie, M. Jake; Nienaber, Kurt; Hackett, Mark J.; Ascone, Isabella; Hedman, Britt; Hodgson, Keith O.; Aitken, Jade B.; Levina, Aviva; Glover, Christopher; Lay, Peter A.

2012-01-01

As synchrotron light sources and optics deliver greater photon flux on samples, X-ray-induced photo-chemistry is increasingly encountered in X-ray absorption spectroscopy (XAS) experiments. The resulting problems are particularly pronounced for biological XAS experiments. This is because biological samples are very often quite dilute and therefore require signal averaging to achieve adequate signal-to-noise ratios, with correspondingly greater exposures to the X-ray beam. This paper reviews the origins of photo-reduction and photo-oxidation, the impact that they can have on active site structure, and the methods that can be used to provide relief from X-ray-induced photo-chemical artifacts. PMID:23093745

X-ray phase scanning setup for non-destructive testing using Talbot-Lau interferometer

NASA Astrophysics Data System (ADS)

Bachche, S.; Nonoguchi, M.; Kato, K.; Kageyama, M.; Koike, T.; Kuribayashi, M.; Momose, A.

2016-09-01

X-ray grating interferometry has a great potential for X-ray phase imaging over conventional X-ray absorption imaging which does not provide significant contrast for weakly absorbing objects and soft biological tissues. X-ray Talbot and Talbot-Lau interferometers which are composed of transmission gratings and measure the differential X-ray phase shifts have gained popularity because they operate with polychromatic beams. In X-ray radiography, especially for nondestructive testing in industrial applications, the feasibility of continuous sample scanning is not yet completely revealed. A scanning setup is frequently advantageous when compared to a direct 2D static image acquisition in terms of field of view, exposure time, illuminating radiation, etc. This paper demonstrates an efficient scanning setup for grating-based Xray phase imaging using laboratory-based X-ray source. An apparatus consisting of an X-ray source that emits X-rays vertically, optical gratings and a photon-counting detector was used with which continuously moving objects across the field of view as that of conveyor belt system can be imaged. The imaging performance of phase scanner was tested by scanning a long continuous moving sample at a speed of 5 mm/s and absorption, differential-phase and visibility images were generated by processing non-uniform moire movie with our specially designed phase measurement algorithm. A brief discussion on the feasibility of phase scanner with scanning setup approach including X-ray phase imaging performance is reported. The successful results suggest a breakthrough for scanning objects those are moving continuously on conveyor belt system non-destructively using the scheme of X-ray phase imaging.

Time-resolved X-ray spectroscopies of chemical systems: New perspectives

PubMed Central

Chergui, Majed

2016-01-01

The past 3–5 years have witnessed a dramatic increase in the number of time-resolved X-ray spectroscopic studies, mainly driven by novel technical and methodological developments. The latter include (i) the high repetition rate optical pump/X-ray probe studies, which have greatly boosted the signal-to-noise ratio for picosecond (ps) X-ray absorption spectroscopy studies, while enabling ps X-ray emission spectroscopy (XES) at synchrotrons; (ii) the X-ray free electron lasers (XFELs) are a game changer and have allowed the first femtosecond (fs) XES and resonant inelastic X-ray scattering experiments to be carried out; (iii) XFELs are also opening the road to the development of non-linear X-ray methods. In this perspective, I will mainly focus on the most recent technical developments and briefly address some examples of scientific questions that have been addressed thanks to them. I will look at the novel opportunities in the horizon. PMID:27376102

Impact of Oriented Clay Particles on X-Ray Spectroscopy Analysis

NASA Astrophysics Data System (ADS)

Lim, A. J. M. S.; Syazwani, R. N.; Wijeyesekera, D. C.

2016-07-01

Understanding the engineering properties of the mineralogy and microfabic of clayey soils is very complex and thus very difficult for soil characterization. Micromechanics of soils recognize that the micro structure and mineralogy of clay have a significant influence on its engineering behaviour. To achieve a more reliable quantitative evaluation of clay mineralogy, a proper sample preparation technique for quantitative clay mineral analysis is necessary. This paper presents the quantitative evaluation of elemental analysis and chemical characterization of oriented and random oriented clay particles using X-ray spectroscopy. Three different types of clays namely marine clay, bentonite and kaolin clay were studied. The oriented samples were prepared by placing the dispersed clay in water and left to settle on porous ceramic tiles by applying a relatively weak suction through a vacuum pump. Images form a Scanning Electron Microscope (SEM) was also used to show the comparison between the orientation patterns of both the sample preparation techniques. From the quantitative analysis of the X-ray spectroscopy, oriented sampling method showed more accuracy in identifying mineral deposits, because it produced better peak intensity on the spectrum and more mineral content can be identified compared to randomly oriented samples.

A combined scanning tunnelling microscope and x-ray interferometer

NASA Astrophysics Data System (ADS)

Yacoot, Andrew; Kuetgens, Ulrich; Koenders, Ludger; Weimann, Thomas

2001-10-01

A monolithic x-ray interferometer made from silicon and a scanning tunnelling microscope have been combined and used to calibrate grating structures with periodicities of 100 nm or less. The x-ray interferometer is used as a translation stage which moves in discrete steps of 0.192 nm, the lattice spacing of the silicon (220) planes. Hence, movements are traceable to the definition of the metre and the nonlinearity associated with the optical interferometers used to measure displacement in more conventional metrological scanning probe microscopes (MSPMs) removed.

Large Area X-ray Spectroscopy Mission

NASA Technical Reports Server (NTRS)

Tananbaum, Harvey

1996-01-01

The Large Area X-ray Spectroscopy (LAXS) mission study concept has evolved strongly over the last year culminating in the merging of LAXS with the Goddard Space Flight Center (GSFC) proposal for a similar mission, the Next Generation X-ray Observatory (NGXO, PI: Nick White). The resulting merger, re-named the High Throughput X-rays Spectroscopy (HTXS) Mission has also expanded by the inclusion of another SAO proposed new mission concept proposal, the Hard X-Ray Telescope (PI: Paul Gorenstein). The resultant multi-instrument mission retains much of heritage from the LAXS proposal, including the use of multiple satellites for robustness. These mergers resulted from a series of contacts between various team members, via e-mail, telecons, and in-person meetings. The impetus for the mergers was the fundamental similarity between the missions, and the recognition that all three proposal teams had significant contributions to make in the effort to define the next stage in the X-ray exploration of the universe. We have enclosed four items that represent some of the work that has occurred during the first year of the study: first, a presentation at the Leicester meeting, second a presentation that was made to Dan Goldin following the merging of LAXS and NGXO, third a copy of the first announcement for the Workshop, and finally the interim report that was prepared by the HTXS study team towards the end of the first year. This last document provides the foundation for the HTXS Technology Roadmap that is being generated. The HTXS roadmap will define the near-term goals that the merged mission must achieve over the next few years. A web site has been developed and populated that contains much of the material that has been generated over the past year.

Development of Compton X-ray spectrometer for high energy resolution single-shot high-flux hard X-ray spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kojima, Sadaoki, E-mail: kojima-s@ile.osaka-u.ac.jp, E-mail: sfujioka@ile.osaka-u.ac.jp; Ikenouchi, Takahito; Arikawa, Yasunobu

Hard X-ray spectroscopy is an essential diagnostics used to understand physical processes that take place in high energy density plasmas produced by intense laser-plasma interactions. A bundle of hard X-ray detectors, of which the responses have different energy thresholds, is used as a conventional single-shot spectrometer for high-flux (>10{sup 13} photons/shot) hard X-rays. However, high energy resolution (Δhv/hv < 0.1) is not achievable with a differential energy threshold (DET) X-ray spectrometer because its energy resolution is limited by energy differences between the response thresholds. Experimental demonstration of a Compton X-ray spectrometer has already been performed for obtaining higher energy resolutionmore » than that of DET spectrometers. In this paper, we describe design details of the Compton X-ray spectrometer, especially dependence of energy resolution and absolute response on photon-electron converter design and its background reduction scheme, and also its application to the laser-plasma interaction experiment. The developed spectrometer was used for spectroscopy of bremsstrahlung X-rays generated by intense laser-plasma interactions using a 200 μm thickness SiO{sub 2} converter. The X-ray spectrum obtained with the Compton X-ray spectrometer is consistent with that obtained with a DET X-ray spectrometer, furthermore higher certainly of a spectral intensity is obtained with the Compton X-ray spectrometer than that with the DET X-ray spectrometer in the photon energy range above 5 MeV.« less

STROBE-X: X-ray Timing & Spectroscopy on Dynamical Timescales from Milliseconds to Years

NASA Technical Reports Server (NTRS)

Wilson-Hodge, Colleen A.; Ray, P. S.; Maccarone, T; Chakrabarty, D.; Gendreau, K.; Arzoumanian, Z.; Jenke, P.; Ballantyne, D.; Bozzo, E.; Brandt, S.;

STROBE-X: X-Ray Timing Spectroscopy on Dynamical Timescales from Microseconds to Years

NASA Technical Reports Server (NTRS)

Wilson-Hodge, Colleen A.; Ray, P. S.; Gendreau, K.; Arzoumanian, Z.; Chakrabarty, D.; Remillard, R.; Feroci, M.; Maccarone, T.; Wood, K.; Jenke, P.

2017-01-01

We describe a probe-class mission concept that provides an unprecedented view of the X-ray sky, performing timing and 0.2-30 keV spectroscopy over timescales from microseconds to years. The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) comprises three primary instruments. The first uses an array of lightweight optics (3-m focal length) that concentrate incident photons onto solid state detectors with CCD-level (85-130 eV) energy resolution, 100 ns time resolution, and low background rates to cover the 0.2-12 keV band. This technology is scaled up from NICER, with enhanced optics to take advantage of the longer focal length of STROBE-X. The second uses large-area collimated silicon drift detectors, developed for ESA's LOFT, to cover the 2-30 keV band. These two instruments each provide an order of magnitude improvement in effective area compared with its predecessor (NICER and RXTE, respectively). Finally, a sensitive sky monitor triggers pointed observations, provides high duty cycle, high time resolution, high spectral resolution monitoring of the X-ray sky with approx. 20 times the sensitivity of the RXTE ASM, and enables multi-wavelength and multi-messenger studies on a continuous, rather than scanning basis.For the first time, the broad coverage provides simultaneous study of thermal components, non-thermal components, iron lines, and reflection features from a single platform for accreting black holes at all scales. The enormous collecting area allows detailed studies of the dense matter equation of state using both thermal emission from rotation-powered pulsars and harder emission from X-ray burst oscillations. The combination of the wide-field monitor and the sensitive pointed instruments enables observations of potential electromagnetic counterparts to LIGO and neutrino events. Additional extragalactic science, such as high quality spectroscopy of clusters of galaxies and unprecedented timing investigations of active

STROBE-X: X-ray Timing & Spectroscopy on Dynamical Timescales from Microseconds to Years

NASA Astrophysics Data System (ADS)

Wilson-Hodge, Colleen A.; Ray, Paul S.; Gendreau, Keith; Chakrabarty, Deepto; Feroci, Marco; Maccarone, Thomas J.; Arzoumanian, Zaven; Remillard, Ronald A.; Wood, Kent; Griffith, Christopher; Jenke, Peter

2017-08-01

We describe a probe-class mission concept that provides an unprecedented view of the X-ray sky, performing timing and 0.2-30 keV spectroscopy over timescales from microseconds to years. The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) comprises three primary instruments. The first uses an array of lightweight optics (3-m focal length) that concentrate incident photons onto solid state detectors with CCD-level (85-130 eV) energy resolution, 100 ns time resolution, and low background rates to cover the 0.2-12 keV band. This technology is scaled up from NICER, with enhanced optics to take advantage of the longer focal length of STROBE-X. The second uses large-area collimated silicon drift detectors, developed for ESA's LOFT, to cover the 2-30 keV band. These two instruments each provide an order of magnitude improvement in effective area compared with its predecessor (NICER and RXTE, respectively). Finally, a sensitive sky monitor triggers pointed observations, provides high duty cycle, high time resolution, high spectral resolution monitoring of the X-ray sky with ~20 times the sensitivity of the RXTE ASM, and enables multi-wavelength and multi-messenger studies on a continuous, rather than scanning basis.For the first time, the broad coverage provides simultaneous study of thermal components, non-thermal components, iron lines, and reflection features from a single platform for accreting black holes at all scales. The enormous collecting area allows detailed studies of the dense matter equation of state using both thermal emission from rotation-powered pulsars and harder emission from X-ray burst oscillations. The combination of the wide-field monitor and the sensitive pointed instruments enables observations of potential electromagnetic counterparts to LIGO and neutrino events. Additional extragalactic science, such as high quality spectroscopy of clusters of galaxies and unprecedented timing investigations of active galactic

Examining the ground layer of St. Anthony from Padua 19th century oil painting by Raman spectroscopy, scanning electron microscopy and X-ray diffraction

NASA Astrophysics Data System (ADS)

Vančo, Ľubomír; Kadlečíková, Magdaléna; Breza, Juraj; Čaplovič, Ľubomír; Gregor, Miloš

2013-01-01

In this paper we studied the material composition of the ground layer of a neoclassical painting. We used Raman spectroscopy (RS) as a prime method. Thereafter scanning electron microscopy combined with energy dispersive spectroscopy (SEM-EDS) and X-ray powder diffraction (XRD) were employed as complementary techniques. The painting inspected was of the side altar in King St. Stephen's Church in Galanta (Slovakia), signed and dated by Jos. Chr. Mayer 1870. Analysis was carried out on both covered and uncovered ground layers. Four principal compounds (barite, lead white, calcite, dolomite) and two minor compounds (sphalerite, quartz) were identified. This ground composition is consistent with the 19th century painting technique used in Central Europe consisting of white pigments and white fillers. Transformation of lead white occurred under laser irradiation. Subdominant Raman peaks of the components were measured. The observed results elucidate useful partnership of RS and SEM-EDS measurements supported by X-ray powder diffraction as well as possibilities and limitations of non-destructive analysis of covered lower layers by RS.

Mode-Locked Multichromatic X-Rays in a Seeded Free-Electron Laser for Single-Shot X-Ray Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xiang, Dao; Ding, Yuantao; Raubenheimer, Tor

2012-05-10

We present the promise of generating gigawatt mode-locked multichromatic x rays in a seeded free-electron laser (FEL). We show that, by using a laser to imprint periodic modulation in electron beam phase space, a single-frequency coherent seed can be amplified and further translated to a mode-locked multichromatic output in an FEL. With this configuration the FEL output consists of a train of mode-locked ultrashort pulses which span a wide frequency gap with a series of equally spaced sharp lines. These gigawatt multichromatic x rays may potentially allow one to explore the structure and dynamics of a large number of atomicmore » states simultaneously. The feasibility of generating mode-locked x rays ranging from carbon K edge ({approx}284 eV) to copper L{sub 3} edge ({approx}931 eV) is confirmed with numerical simulation using the realistic parameters of the linac coherent light source (LCLS) and LCLS-II. We anticipate that the mode-locked multichromatic x rays in FELs may open up new opportunities in x-ray spectroscopy (i.e. resonant inelastic x-ray scattering, time-resolved scattering and spectroscopy, etc.).« less

X-Ray photoelectron Spectroscopy Applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Engelhard, Mark H.; Droubay, Timothy C.; Du, Yingge

2017-01-03

With capability for obtaining quantitative elemental composition, chemical and electronic state, and overlayer thickness information from the top ~10 nm of a sample surface, X-ray Photoelectron Spectroscopy (XPS) or Electron Spectroscopy for Chemical Analysis (ESCA) is a versatile and widely used technique for analyzing surfaces. The technique is applied to a host of materials, from insulators to conductors in virtually every scientific field and sub-discipline. More recently, XPS has been extended under in-situ and operando conditions. Following a brief introduction to XPS principles and instrument components, this article exemplifies widely ranging XPS applications in material and life sciences.

Local Structure Determination of Carbon/Nickel Ferrite Composite Nanofibers Probed by X-ray Absorption Spectroscopy.

PubMed

Nilmoung, Sukunya; Kidkhunthod, Pinit; Maensiri, Santi

2015-11-01

Carbon/NiFe2O4 composite nanofibers have been successfully prepared by electrospinning method using a various concentration solution of Ni and Fe nitrates dispersed into polyacrylonitride (PAN) solution in N,N' dimethylformamide. The phase and mophology of PAN/NiFe2O4 composite samples were characterized and investigated by X-ray diffraction and scanning electron microscopy. The magnetic properties of the prepared samples were measured at ambient temperature by a vibrating sample magnetometer. It is found that all composite samples exhibit ferromagnetism. This could be local-structurally explained by the existed oxidation states of Ni2+ and Fe3+ in the samples. Moreover, local environments around Ni and Fe ions could be revealed by X-ray absorption spectroscopy (XAS) measurement including X-ray absorption near edge structure (XANES) and Extended X-ray absorption fine structure (EXAFS).

Stimulated x-ray emission spectroscopy in transition metal complexes

DOE PAGES

Kroll, Thomas; Weninger, Clemens; Alonso-Mori, Roberto; ...

2018-03-27

We report the observation and analysis of the gain curve of amplified Kα X-ray emission from solutions of Mn(II) and Mn(VII) complexes using an X-ray free electron laser to create the 1s core-hole population inversion. We find spectra at amplification levels extending over four orders of magnitude until saturation. We observe bandwidths below the Mn 1s core-hole lifetime broadening in the onset of the stimulated emission. In the exponential amplification regime the resolution corrected spectral width of ~1.7 eV FWHM is constant over three orders of magnitude, pointing to the build-up of transform limited pulses of ~1fs duration. Driving the amplification into saturation leads to broadening and shift of the line. Importantly, the chemical sensitivity of the stimulated X-ray emission to the Mn oxidation state is preserved at power densities ofmore » $$\\sim10 20$$~W/cm 2 for the incoming X-ray pulses. Differences in signal sensitivity and spectral information compared to conventional (spontaneous) X-ray emission spectroscopy are discussed. Our findings build a baseline for nonlinear X-ray spectroscopy for a wide range of transition metal complexes in inorganic chemistry, catalysis and materials science.« less

Stimulated x-ray emission spectroscopy in transition metal complexes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kroll, Thomas; Weninger, Clemens; Alonso-Mori, Roberto

We report the observation and analysis of the gain curve of amplified Kα X-ray emission from solutions of Mn(II) and Mn(VII) complexes using an X-ray free electron laser to create the 1s core-hole population inversion. We find spectra at amplification levels extending over four orders of magnitude until saturation. We observe bandwidths below the Mn 1s core-hole lifetime broadening in the onset of the stimulated emission. In the exponential amplification regime the resolution corrected spectral width of ~1.7 eV FWHM is constant over three orders of magnitude, pointing to the build-up of transform limited pulses of ~1fs duration. Driving the amplification into saturation leads to broadening and shift of the line. Importantly, the chemical sensitivity of the stimulated X-ray emission to the Mn oxidation state is preserved at power densities ofmore » $$\\sim10 20$$~W/cm 2 for the incoming X-ray pulses. Differences in signal sensitivity and spectral information compared to conventional (spontaneous) X-ray emission spectroscopy are discussed. Our findings build a baseline for nonlinear X-ray spectroscopy for a wide range of transition metal complexes in inorganic chemistry, catalysis and materials science.« less

Stimulated X-Ray Emission Spectroscopy in Transition Metal Complexes

NASA Astrophysics Data System (ADS)

Kroll, Thomas; Weninger, Clemens; Alonso-Mori, Roberto; Sokaras, Dimosthenis; Zhu, Diling; Mercadier, Laurent; Majety, Vinay P.; Marinelli, Agostino; Lutman, Alberto; Guetg, Marc W.; Decker, Franz-Josef; Boutet, Sébastien; Aquila, Andy; Koglin, Jason; Koralek, Jake; DePonte, Daniel P.; Kern, Jan; Fuller, Franklin D.; Pastor, Ernest; Fransson, Thomas; Zhang, Yu; Yano, Junko; Yachandra, Vittal K.; Rohringer, Nina; Bergmann, Uwe

2018-03-01

We report the observation and analysis of the gain curve of amplified K α x-ray emission from solutions of Mn(II) and Mn(VII) complexes using an x-ray free electron laser to create the 1 s core-hole population inversion. We find spectra at amplification levels extending over 4 orders of magnitude until saturation. We observe bandwidths below the Mn 1 s core-hole lifetime broadening in the onset of the stimulated emission. In the exponential amplification regime the resolution corrected spectral width of ˜1.7 eV FWHM is constant over 3 orders of magnitude, pointing to the buildup of transform limited pulses of ˜1 fs duration. Driving the amplification into saturation leads to broadening and a shift of the line. Importantly, the chemical sensitivity of the stimulated x-ray emission to the Mn oxidation state is preserved at power densities of ˜1020 W /cm2 for the incoming x-ray pulses. Differences in signal sensitivity and spectral information compared to conventional (spontaneous) x-ray emission spectroscopy are discussed. Our findings build a baseline for nonlinear x-ray spectroscopy for a wide range of transition metal complexes in inorganic chemistry, catalysis, and materials science.

X-ray scattering and spectroscopy studies on diesel soot from oxygenated fuel under various engine load conditions

USGS Publications Warehouse

Braun, Andreas; Shah, N.; Huggins, Frank E.; Kelly, K.E.; Sarofim, A.; Jacobsen, C.; Wirick, S.; Francis, H.; Ilavsky, J.; Thomas, G.E.; Huffman, G.P.

2005-01-01

Diesel soot from reference diesel fuel and oxygenated fuel under idle and load engine conditions was investigated with X-ray scattering and X-ray carbon K-edge absorption spectroscopy. Up to five characteristic size ranges were found. Idle soot was generally found to have larger primary particles and aggregates but smaller crystallites, than load soot. Load soot has a higher degree of crystallinity than idle soot. Adding oxygenates to diesel fuel enhanced differences in the characteristics of diesel soot, or even reversed them. Aromaticity of idle soot from oxygenated diesel fuel was significantly larger than from the corresponding load soot. Carbon near-edge X-ray absorption fine structure (NEXAFS) spectroscopy was applied to gather information about the presence of relative amounts of carbon double bonds (CC, CO) and carbon single bonds (C-H, C-OH, COOH). Using scanning X-ray transmission microspectroscopy (STXM), the relative amounts of these carbon bond states were shown to vary spatially over distances approximately 50 to 100 nm. The results from the X-ray techniques are supported by thermo-gravimetry analysis and high-resolution transmission electron microscopy. ?? 2005 Elsevier Ltd. All rights reserved.

Optimizing soft X-ray NEXAFS spectroscopy in the laboratory

NASA Astrophysics Data System (ADS)

Mantouvalou, I.; Jonas, A.; Witte, K.; Jung, R.; Stiel, H.; Kanngießer, B.

2017-05-01

Near edge X-ray absorption fine structure (NEXAFS) spectroscopy in the soft X-ray range is feasible in the laboratory using laser-produced plasma sources. We present a study using seven different target materials for optimized data analysis. The emission spectra of the materials with atomic numbers ranging from Z = 6 to Z = 79 show distinct differences, rendering the adapted selection of a suitable target material for specialized experiments feasible. For NEXAFS spectroscopy a 112.5 nm thick polyimide film is investigated as a reference exemplifying the superiority of quasi-continuum like emission spectra.

Resonant Polarization Spectroscopy for Hot X-ray Plasmas

DOE PAGES

Chen, Guo -Xin

2016-04-28

X-ray line polarization spectroscopy is a method of choice for probing hot plasma conditions. The precise roles of resonant structures in this method have not been realized and fully understood. With a sophisticated relativistic close coupling Dirac R-matrix calculation of polarized radiation of the quadrupole magnetic M2 line at 2.717 Å in Ba 46+, we revealed the nature of resonant structures in x-ray line polarization spectroscopy. We found that signatures with a heavy resonance forest imprinting on polarization may be used for a sensitive new spectroscopic method. The resonant polarization spectrum was used to determine or constrain the directional beammore » electron distribution of the laboratory Ba plasma. Lastly, our results provide a start of resonant polarization spectroscopy as a method for diagnostics of laboratory, fusion and astrophysical plasma source conditions.« less

Soft X-ray absorption spectroscopy and resonant inelastic X-ray scattering spectroscopy below 100 eV: probing first-row transition-metal M-edges in chemical complexes.

PubMed

Wang, Hongxin; Young, Anthony T; Guo, Jinghua; Cramer, Stephen P; Friedrich, Stephan; Braun, Artur; Gu, Weiwei

2013-07-01

X-ray absorption and scattering spectroscopies involving the 3d transition-metal K- and L-edges have a long history in studying inorganic and bioinorganic molecules. However, there have been very few studies using the M-edges, which are below 100 eV. Synchrotron-based X-ray sources can have higher energy resolution at M-edges. M-edge X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS) could therefore provide complementary information to K- and L-edge spectroscopies. In this study, M2,3-edge XAS on several Co, Ni and Cu complexes are measured and their spectral information, such as chemical shifts and covalency effects, are analyzed and discussed. In addition, M2,3-edge RIXS on NiO, NiF2 and two other covalent complexes have been performed and different d-d transition patterns have been observed. Although still preliminary, this work on 3d metal complexes demonstrates the potential to use M-edge XAS and RIXS on more complicated 3d metal complexes in the future. The potential for using high-sensitivity and high-resolution superconducting tunnel junction X-ray detectors below 100 eV is also illustrated and discussed.

STROBE-X: X-ray Timing & Spectroscopy on Dynamical Timescales from Microseconds to Years

NASA Astrophysics Data System (ADS)

Wilson-Hodge, Colleen A.; Ray, Paul S.; Gendreau, Keith; Chakrabarty, Deepto; Feroci, Marco; Maccarone, Tom; Arzoumanian, Zaven; Remillard, Ronald A.; Wood, Kent; Griffith, Christopher; STROBE-X Collaboration

2017-01-01

We describe a proposed probe-class mission concept that will provide an unprecedented view of the X-ray sky, performing timing and spectroscopy over a broad band (0.2-30 keV) probing timescales from microseconds to years. The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) comprises two primary instruments. The soft band (0.2-12 keV) will be covered by an array of lightweight optics (3-m focal length) that concentrate incident photons onto small solid state detectors with CCD-level (85-130 eV) energy resolution, 100 ns time resolution, and low background rates. This technology, fully developed for NICER, would be scaled up with enhanced optics to take advantage of the longer focal length of STROBE-X. The harder band (2 to at least 30 keV) would be covered by large-area collimated silicon drift detectors,developed for the European LOFT mission concept. Each instrument would provide an order of magnitude improvement in effective area compared with its predecessor (NICER in the soft band and RXTE in the hard band). A sensitive sky monitor would act as a trigger for pointed observations, provide high duty cycle, high time resolution, high spectral resolution monitoring of the X-ray sky with ~20 times the sensitivity of the RXTE ASM, and enable multi-wavelength and multi-messenger studies on a continuous, rather than scanning basis.The broad coverage will enable thermal components, non-thermal components, iron lines, and reflection features to be studied simultaneously from a single platform for the first time in accreting black holes at all scales. The enormous collecting area will enable studies of the dense matter equation of state using both soft thermal emission from rotation-powered pulsars and harder emission from X-ray burst oscillations. Revolutionary science, such as high quality spectroscopy of clusters of galaxies and unprecedented timing investigations of active galactic nuclei, would also be obtained.We describe the mission

Characterization of CuHal-intercalated carbon nanotubes with x-ray absorption spectroscopy combined with x-ray photoelectron and resonant photoemission spectroscopies

NASA Astrophysics Data System (ADS)

Brzhezinskaya, M.; Generalov, A.; Vinogdradov, A.; Eliseev, A.

2013-04-01

Encapsulated single-walled carbon nanotubes (SWCNTs) with inner channels filled by different compounds present the new class of composite materials. Such CNTs give opportunity to form 1D nanocrystals as well as quantum nanowires with new physical and chemical properties inside the tubes. The present study is aimed to characterize the possible chemical interaction between CuHal (Hal=I, Cl, Br) and SWCNTs in CuHal@SWCNTs and electronic structure of the latter using high-resolution near edge X-ray absorption fine structure (NEXAFS) spectroscopy combined with high-resolution X-ray photoelectron spectroscopy and resonant photoemission spectroscopy. The present study has shown that there is a chemical interaction between the filler and π-electron subsystem of CNTs which is accompanied by changes of the atomic and electronic structure of the filler during the encapsulating it inside CNTs.

X-Ray Spectroscopy of Photoionized Plasmas

NASA Technical Reports Server (NTRS)

Kallman, Tim

2008-01-01

Spectroscopy allows study of sources on small spatial scales, and can provide detailed diagnostic information about elemental abundances, temperature, density and gas dynamics. For compact sources such as accreting black holes in active galactic nuclei (AGN) and X-ray binaries X-ray spectra provide truly unique insight. Observations using Chandra and XMM have revealed components of gas in these systems which were previously unknown or poorly studied. Interpretation of these data presents modeling and analysis challenges, and requires an understanding of atomic physics, ionization and spectrum formation in a radiation-dominated environment. In this talk I will discuss examples, and how they have contributed to our understanding of accreting sources and the nearby gas.

High-Resolution Detector For X-Ray Diffraction

NASA Technical Reports Server (NTRS)

Carter, Daniel C.; Withrow, William K.; Pusey, Marc L.; Yost, Vaughn H.

1988-01-01

Proposed x-ray-sensitive imaging detector offers superior spatial resolution, counting-rate capacity, and dynamic range. Instrument based on laser-stimulated luminescence and reusable x-ray-sensitive film. Detector scans x-ray film line by line. Extracts latent image in film and simultaneously erases film for reuse. Used primarily for protein crystallography. Principle adapted to imaging detectors for electron microscopy and fluorescence spectroscopy and general use in astronomy, engineering, and medicine.

X-ray absorption fine structure (XAFS) spectroscopy using synchrotron radiation

NASA Astrophysics Data System (ADS)

Shrivastava, B. D.

2012-05-01

The X-ray absorption fine structure (XAFS) spectra are best recorded when a highly intense beam of X-rays from a synchrotron is used along with a good resolution double crystal or curved crystal spectrometer and detectors like ionization chambers, scintillation counters, solid state detectors etc. Several synchrotrons around the world have X-ray beamlines dedicated specifically to XAFS spectroscopy. Fortunately, the Indian synchrotron (Indus-2) at Raja Ramanna Centre for Advanced Technology (RRCAT) at Indore has started operation. A dispersive type EXAFS beamline called BL-8 has been commissioned at this synchrotron and another beamline having double crystal monochromator (DCM) is going to be commissioned shortly. In Indian context, in order that more research workers use these beamlines, the study of XAFS spectroscopy using synchrotron radiation becomes important. In the present work some of the works done by our group on XAFS spectroscopy using synchrotron radiation have been described.

Ultrafast Time-Resolved Hard X-Ray Emission Spectroscopy on a Tabletop

NASA Astrophysics Data System (ADS)

Miaja-Avila, Luis; O'Neil, Galen C.; Joe, Young I.; Alpert, Bradley K.; Damrauer, Niels H.; Doriese, William B.; Fatur, Steven M.; Fowler, Joseph W.; Hilton, Gene C.; Jimenez, Ralph; Reintsema, Carl D.; Schmidt, Daniel R.; Silverman, Kevin L.; Swetz, Daniel S.; Tatsuno, Hideyuki; Ullom, Joel N.

2016-07-01

Experimental tools capable of monitoring both atomic and electronic structure on ultrafast (femtosecond to picosecond) time scales are needed for investigating photophysical processes fundamental to light harvesting, photocatalysis, energy and data storage, and optical display technologies. Time-resolved hard x-ray (>3 keV ) spectroscopies have proven valuable for these measurements due to their elemental specificity and sensitivity to geometric and electronic structures. Here, we present the first tabletop apparatus capable of performing time-resolved x-ray emission spectroscopy. The time resolution of the apparatus is better than 6 ps. By combining a compact laser-driven plasma source with a highly efficient array of microcalorimeter x-ray detectors, we are able to observe photoinduced spin changes in an archetypal polypyridyl iron complex [Fe (2 ,2'-bipyridine)3]2 + and accurately measure the lifetime of the quintet spin state. Our results demonstrate that ultrafast hard x-ray emission spectroscopy is no longer confined to large facilities and now can be performed in conventional laboratories with 10 times better time resolution than at synchrotrons. Our results are enabled, in part, by a 100- to 1000-fold increase in x-ray collection efficiency compared to current techniques.

Coherent x-ray zoom condenser lens for diffractive and scanning microscopy.

PubMed

Kimura, Takashi; Matsuyama, Satoshi; Yamauchi, Kazuto; Nishino, Yoshinori

2013-04-22

We propose a coherent x-ray zoom condenser lens composed of two-stage deformable Kirkpatrick-Baez mirrors. The lens delivers coherent x-rays with a controllable beam size, from one micrometer to a few tens of nanometers, at a fixed focal position. The lens is suitable for diffractive and scanning microscopy. We also propose non-scanning coherent diffraction microscopy for extended objects by using an apodized focused beam produced by the lens with a spatial filter. The proposed apodized-illumination method will be useful in highly efficient imaging with ultimate storage ring sources, and will also open the way to single-shot coherent diffraction microscopy of extended objects with x-ray free-electron lasers.

Scanning force microscope for in situ nanofocused X-ray diffraction studies

PubMed Central

Ren, Zhe; Mastropietro, Francesca; Davydok, Anton; Langlais, Simon; Richard, Marie-Ingrid; Furter, Jean-Jacques; Thomas, Olivier; Dupraz, Maxime; Verdier, Marc; Beutier, Guillaume; Boesecke, Peter; Cornelius, Thomas W.

2014-01-01

A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials. PMID:25178002

Study of X-ray transients with Scanning Sky Monitor (SSM) onboard AstroSat

NASA Astrophysics Data System (ADS)

Ramadevi, M. C.; Ravishankar, B. T.; Sarwade, Abhilash R.; Vaishali, S.; Iyer, Nirmal Kumar; Nandi, Anuj; Girish, V.; Agarwal, Vivek Kumar; Baby, Blessy Elizabeth; Hasan, Mohammed; Seetha, S.; Bhattacharya, Dipankar

2018-02-01

Scanning Sky Monitor (SSM) onboard AstroSat is an X-ray sky monitor in the energy range 2.5-10 keV. SSM scans the sky for X-ray transient sources in this energy range of interest. If an X-ray transient source is detected in outburst by SSM, the information will be provided to the astronomical community for follow-up observations to do a detailed study of the source in various other bands. SSM instrument, since its power-ON in orbit, has observed a number of X-ray sources. This paper discusses observations of few X-ray transients by SSM. The flux reported by SSM for few sources during its Performance Verification phase (PV phase) is studied and the results are discussed.

X-ray Photoelectron Spectroscopy (XPS), Rutherford Back Scattering (RBS) studies

NASA Technical Reports Server (NTRS)

Neely, W. C.; Bozak, M. J.; Williams, J. R.

1993-01-01

X-ray photoelectron spectroscopy (XPS), Rutherford Back Scattering (RBS) studies of each of sample received were completed. Since low angle X-ray could not be performed because of instrumentation problems, Auger spectrometry was employed instead. The results of these measurements for each of the samples is discussed in turn.

An upgraded x-ray spectroscopy diagnostic on MST.

PubMed

Clayton, D J; Almagri, A F; Burke, D R; Forest, C B; Goetz, J A; Kaufman, M C; O'Connell, R

2010-10-01

An upgraded x-ray spectroscopy diagnostic is used to measure the distribution of fast electrons in MST and to determine Z(eff) and the particle diffusion coefficient D(r). A radial array of 12 CdZnTe hard-x-ray detectors measures 10-150 keV Bremsstrahlung from fast electrons, a signature of reduced stochasticity and improved confinement in the plasma. A new Si soft-x-ray detector measures 2-10 keV Bremsstrahlung from thermal and fast electrons. The shaped output pulses from both detector types are digitized and the resulting waveforms are fit with Gaussians to resolve pileup and provide good time and energy resolution. Lead apertures prevent detector saturation and provide a well-known etendue, while lead shielding prevents pickup from stray x-rays. New Be vacuum windows transmit >2 keV x-rays, and additional Al and Be filters are sometimes used to reduce low energy flux for better resolution at higher energies. Measured spectra are compared to those predicted by the Fokker-Planck code CQL3D to deduce Z(eff) and D(r).

Photon statistics and speckle visibility spectroscopy with partially coherent X-rays.

PubMed

Li, Luxi; Kwaśniewski, Paweł; Orsi, Davide; Wiegart, Lutz; Cristofolini, Luigi; Caronna, Chiara; Fluerasu, Andrei

2014-11-01

A new approach is proposed for measuring structural dynamics in materials from multi-speckle scattering patterns obtained with partially coherent X-rays. Coherent X-ray scattering is already widely used at high-brightness synchrotron lightsources to measure dynamics using X-ray photon correlation spectroscopy, but in many situations this experimental approach based on recording long series of images (i.e. movies) is either not adequate or not practical. Following the development of visible-light speckle visibility spectroscopy, the dynamic information is obtained instead by analyzing the photon statistics and calculating the speckle contrast in single scattering patterns. This quantity, also referred to as the speckle visibility, is determined by the properties of the partially coherent beam and other experimental parameters, as well as the internal motions in the sample (dynamics). As a case study, Brownian dynamics in a low-density colloidal suspension is measured and an excellent agreement is found between correlation functions measured by X-ray photon correlation spectroscopy and the decay in speckle visibility with integration time obtained from the analysis presented here.

Ultrasound detection of pneumothorax compared with chest X-ray and computed tomography scan.

PubMed

Nagarsheth, Khanjan; Kurek, Stanley

2011-04-01

Pneumothorax after trauma can be a life threatening injury and its care requires expeditious and accurate diagnosis and possible intervention. We performed a prospective, single blinded study with convenience sampling at a Level I trauma center comparing thoracic ultrasound with chest X-ray and CT scan in the detection of traumatic pneumothorax. Trauma patients that received a thoracic ultrasound, chest X-ray, and chest CT scan were included in the study. The chest X-rays were read by a radiologist who was blinded to the thoracic ultrasound results. Then both were compared with CT scan results. One hundred and twenty-five patients had a thoracic ultrasound performed in the 24-month period. Forty-six patients were excluded from the study due to lack of either a chest X-ray or chest CT scan. Of the remaining 79 patients there were 22 positive pneumothorax found by CT and of those 18 (82%) were found on ultrasound and 7 (32%) were found on chest X-ray. The sensitivity of thoracic ultrasound was found to be 81.8 per cent and the specificity was found to be 100 per cent. The sensitivity of chest X-ray was found to be 31.8 per cent and again the specificity was found to be 100 per cent. The negative predictive value of thoracic ultrasound for pneumothorax was 0.934 and the negative predictive value for chest X-ray for pneumothorax was found to be 0.792. We advocate the use of chest ultrasound for detection of pneumothorax in trauma patients.

X-ray absorption spectroscopy: EXAFS (Extended X-ray Absorption Fine Structure) and XANES (X-ray Absorption Near Edge Structure)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Alp, E.E.; Mini, S.M.; Ramanathan, M.

1990-04-01

The x-ray absorption spectroscopy (XAS) had been an essential tool to gather spectroscopic information about atomic energy level structure in the early decades of this century. It has also played an important role in the discovery and systematization of rare-earth elements. The discovery of synchrotron radiation in 1952, and later the availability of broadly tunable synchrotron based x-ray sources have revitalized this technique since the 1970's. The correct interpretation of the oscillatory structure in the x-ray absorption cross-section above the absorption edge by Sayers et. al. has transformed XAS from a spectroscopic tool to a structural technique. EXAFS (Extended X-raymore » Absorption Fine Structure) yields information about the interatomic distances, near neighbor coordination numbers, and lattice dynamics. An excellent description of the principles and data analysis techniques of EXAFS is given by Teo. XANES (X-ray Absorption Near Edge Structure), on the other hand, gives information about the valence state, energy bandwidth and bond angles. Today, there are about 50 experimental stations in various synchrotrons around the world dedicated to collecting x-ray absorption data from the bulk and surfaces of solids and liquids. In this chapter, we will give the basic principles of XAS, explain the information content of essentially two different aspects of the absorption process leading to EXAFS and XANES, and discuss the source and samples limitations.« less

X-ray astronomical spectroscopy

NASA Technical Reports Server (NTRS)

Holt, Stephen S.

1987-01-01

The contributions of the Goddard group to the history of X-ray astronomy are numerous and varied. One role that the group has continued to play involves the pursuit of techniques for the measurement and interpretation of the X-ray spectra of cosmic sources. The latest development is the selection of the X-ray microcalorimeter for the Advanced X-ray Astrophysics Facility (AXAF) study payload. This technology is likely to revolutionize the study of cosmic X-ray spectra.

Soft X-ray absorption spectroscopy and resonant inelastic X-ray scattering spectroscopy below 100 eV: probing first-row transition-metal M-edges in chemical complexes

PubMed Central

Wang, Hongxin; Young, Anthony T.; Guo, Jinghua; Cramer, Stephen P.; Friedrich, Stephan; Braun, Artur; Gu, Weiwei

2013-01-01

X-ray absorption and scattering spectroscopies involving the 3d transition-metal K- and L-edges have a long history in studying inorganic and bioinorganic molecules. However, there have been very few studies using the M-edges, which are below 100 eV. Synchrotron-based X-ray sources can have higher energy resolution at M-edges. M-edge X-ray absorption spectroscopy (XAS) and resonant inelastic X-ray scattering (RIXS) could therefore provide complementary information to K- and L-edge spectroscopies. In this study, M 2,3-edge XAS on several Co, Ni and Cu complexes are measured and their spectral information, such as chemical shifts and covalency effects, are analyzed and discussed. In addition, M 2,3-edge RIXS on NiO, NiF2 and two other covalent complexes have been performed and different d–d transition patterns have been observed. Although still preliminary, this work on 3d metal complexes demonstrates the potential to use M-edge XAS and RIXS on more complicated 3d metal complexes in the future. The potential for using high-sensitivity and high-resolution superconducting tunnel junction X-ray detectors below 100 eV is also illustrated and discussed. PMID:23765304

Luminescent properties under X-ray excitation of Ba(1-x)PbxWO4 disordered solid solution

NASA Astrophysics Data System (ADS)

Bakiz, B.; Hallaoui, A.; Taoufyq, A.; Benlhachemi, A.; Guinneton, F.; Villain, S.; Ezahri, M.; Valmalette, J.-C.; Arab, M.; Gavarri, J.-R.

2018-02-01

A series of polycrystalline barium-lead tungstate Ba1-xPbxWO4 with 0 ≤ x ≤ 1 was synthesized using a classical solid-state method with thermal treatment at 1000 °C. These materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Raman (FT-Raman) spectroscopy. X-ray diffraction profile analyses were performed using Rietveld method. These materials crystallized in the scheelite tetragonal structure and behaved as quasi ideal solid solution. Raman spectroscopy confirmed the formation of the solid solution. Structural distortions were evidenced in X-ray diffraction profiles and in vibration Raman spectra. The scanning electron microscopy experiments showed large and rounded irregular grains. Luminescence experiments were performed under X-ray excitation. The luminescence emission profiles have been interpreted in terms of four Gaussian components, with a major contribution of blue emission. The integrated intensity of luminescence reached a maximum value in the composition range x = 0.3-0.6, in relation with distortions of crystal lattice.

Effect of X-ray flux on polytetrafluoroethylene in X-ray photoelectron spectroscopy

NASA Technical Reports Server (NTRS)

Wheeler, D. R.; Pepper, S. V.

1982-01-01

The effect of the X-ray flux in X-ray photoelectron spectroscopy (STAT) on the constitution of the polytetrafluoroethylene (PTFE) surface has been examined. The radiation dose rate for our specimen was about 10 to the 7th rad/s. The structure, magnitude and binding energy of the C(1s) and F(1s) features of the XPS spectrum and the mass spectrum of gaseous species evolved during irradiation are observed. The strong time dependence of these signals over a period of several hours indicated that the surface constitution of PTFE is greatly affected by this level of radiation dose. The results are consistent with the development of a heavily cross-linked or branched structure in the PTFE surface region and the evolution of short chain fragments into the gas phase.

Kinoform optics applied to X-ray photon correlation spectroscopy.

PubMed

Sandy, A R; Narayanan, S; Sprung, M; Su, J-D; Evans-Lutterodt, K; Isakovic, A F; Stein, A

2010-05-01

Moderate-demagnification higher-order silicon kinoform focusing lenses have been fabricated to facilitate small-angle X-ray photon correlation spectroscopy (XPCS) experiments. The geometric properties of such lenses, their focusing performance and their applicability for XPCS measurements are described. It is concluded that one-dimensional vertical X-ray focusing via silicon kinoform lenses significantly increases the usable coherent flux from third-generation storage-ring light sources for small-angle XPCS experiments.

Soft X-ray spectroscopy of transition metal compounds: a theoretical perspective

NASA Astrophysics Data System (ADS)

Bokarev, S. I.; Hilal, R.; Aziz, S. G.; Kühn, O.

2017-01-01

To date, X-ray spectroscopy has become a routine tool that can reveal highly local and element-specific information on the electronic structure of atoms in complex environments. Here, we report on the development of an efficient and versatile theoretical methodology for the treatment of soft X-ray spectra of transition metal compounds based on the multi-configurational self-consistent field electronic structure theory. A special focus is put on the L-edge photon-in/photon-out and photon-in/electron-out processes, i.e. X-ray absorption, resonant inelastic scattering, partial fluorescence yield, and photoelectron spectroscopy, all treated on the same theoretical footing. The investigated systems range from small prototypical coordination compounds and catalysts to aggregates of biomolecules.

X-Ray spectroscopy of cooling flows

NASA Technical Reports Server (NTRS)

Prestwich, Andrea

1996-01-01

Cooling flows in clusters of galaxies occur when the cooling time of the gas is shorter than the age of the cluster; material cools and falls to the center of the cluster potential. Evidence for short X-ray cooling times comes from imaging studies of clusters and X-ray spectroscopy of a few bright clusters. Because the mass accretion rate can be high (a few 100 solar mass units/year) the mass of material accumulated over the lifetime of a cluster can be as high as 10(exp 12) solar mass units. However, there is little evidence for this material at other wavelengths, and the final fate of the accretion material is unknown. X-ray spectra obtained with the Einstein SSS show evidence for absorption; if confirmed this result would imply that the accretion material is in the form of cool dense clouds. However ice on the SSS make these data difficult to interpret. We obtained ASCA spectra of the cooling flow cluster Abell 85. Our primary goals were to search for multi-temperature components that may be indicative of cool gas; search for temperature gradients across the cluster; and look for excess absorption in the cooling region.

Soft X-ray scanning transmission X-ray microscopy (STXM) of actinide particles.

PubMed

Nilsson, Hans J; Tyliszczak, Tolek; Wilson, Richard E; Werme, Lars; Shuh, David K

2005-09-01

A descriptive account is given of our most recent research on the actinide dioxides with the Advanced Light Source Molecular Environmental Science (ALS-MES) Beamline 11.0.2 soft X-ray scanning transmission X-ray microscope (STXM) at the Lawrence Berkeley National Laboratory (LBNL). The ALS-MES STXM permits near-edge X-ray absorption fine structure (NEXAFS) and imaging with 30-nm spatial resolution. The first STXM spectromicroscopy NEXAFS spectra at the actinide 4d5/2 edges of the imaged transuranic particles, NpO2 and PuO2, have been obtained. Radiation damage induced by the STXM was observed in the investigation of a mixed oxidation state particle (Np(V,VI)) and was minimized during collection of the actual spectra at the 4d5/2 edge of the Np(V,VI) solid. A plutonium elemental map was obtained from an irregular PuO2 particle with the dimensions of 650 x 650 nm. The Pu 4d5/2 NEXAFS spectra were collected at several different locations from the PuO2 particle and were identical. A representative oxygen K-edge spectrum from UO2 was collected and resembles the oxygen K-edge from the bulk material. The unique and current performance of the ALS-MES STXM at extremely low energies (ca. 100 eV) that may permit the successful measurement of the actinide 5d edge is documented. Finally, the potential of STXM as a tool for actinide investigations is briefly discussed.

Application of ultra-small-angle X-ray scattering / X-ray photon correlation spectroscopy to relate equilibrium or non-equilibrium dynamics to microstructure

NASA Astrophysics Data System (ADS)

Allen, Andrew; Zhang, Fan; Levine, Lyle; Ilavsky, Jan

2013-03-01

Ultra-small-angle X-ray scattering (USAXS) can probe microstructures over the nanometer-to-micrometer scale range. Through use of a small instrument entrance slit, X-ray photon correlation spectroscopy (XPCS) exploits the partial coherence of an X-ray synchrotron undulator beam to provide unprecedented sensitivity to the dynamics of microstructural change. In USAXS/XPCS studies, the dynamics of local structures in a scale range of 100 nm to 1000 nm can be related to an overall hierarchical microstructure extending from 1 nm to more than 1000 nm. Using a point-detection scintillator mode, the equilibrium dynamics at ambient temperature of small particles (which move more slowly than nanoparticles) in aqueous suspension have been quantified directly for the first time. Using a USAXS-XPCS scanning mode for non-equilibrium dynamics incipient processes within dental composites have been elucidated, prior to effects becoming detectable using any other technique. Use of the Advanced Photon Source, an Office of Science User Facility operated for the United States Department of Energy (U.S. DOE) Office of Science by Argonne National Laboratory, was supported by the U.S. DOE under Contract No. DE-AC02-06CH11357.

Novel applications of X-ray photoelectron spectroscopy on unsupported nanoparticles

NASA Astrophysics Data System (ADS)

Kostko, Oleg; Xu, Bo; Jacobs, Michael I.; Ahmed, Musahid

X-ray photoelectron spectroscopy (XPS) is a powerful technique for chemical analysis of surfaces. We will present novel results of XPS on unsupported, gas-phase nanoparticles using a velocity-map imaging (VMI) spectrometer. This technique allows for probes of both the surfaces of nanoparticles via XPS as well as their interiors via near edge X-ray absorption fine structure (NEXAFS) spectroscopy. A recent application of this technique has confirmed that arginine's guanidinium group exists in a protonated state even in strongly basic solution. Moreover, the core-level photoelectron spectroscopy can provide information on the effective attenuation length (EAL) of low kinetic energy electrons. This contradictory value is important for determining the probing depth of XPS and in photolithography. A new method for determining EALs will be presented.

Compact scanning transmission x-ray microscope at the photon factory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takeichi, Yasuo, E-mail: yasuo.takeichi@kek.jp; Inami, Nobuhito; Ono, Kanta

We report the design and performance of a compact scanning transmission X-ray microscope developed at the Photon Factory. Piezo-driven linear stages are used as coarse stages of the microscope to realize excellent compactness, mobility, and vibrational and thermal stability. An X-ray beam with an intensity of ∼10{sup 7} photons/s was focused to a diameter of ∼40 nm at the sample. At the soft X-ray undulator beamline used with the microscope, a wide range of photon energies (250–1600 eV) is available. The microscope has been used to research energy materials and in environmental sciences.

A new endstation at the Swiss Light Source for ultraviolet photoelectron spectroscopy, X-ray photoelectron spectroscopy, and X-ray absorption spectroscopy measurements of liquid solutions.

PubMed

Brown, Matthew A; Redondo, Amaia Beloqui; Jordan, Inga; Duyckaerts, Nicolas; Lee, Ming-Tao; Ammann, Markus; Nolting, Frithjof; Kleibert, Armin; Huthwelker, Thomas; Müächler, Jean-Pierre; Birrer, Mario; Honegger, Juri; Wetter, Reto; Wörner, Hans Jakob; van Bokhoven, Jeroen A

2013-07-01

A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutions and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented.

Feasibility of Valence-to-Core X-ray Emission Spectroscopy for Tracking Transient Species

DOE PAGES

March, Anne Marie; Assefa, Tadesse A.; Bressler, Christian; ...

2015-02-09

X-ray spectroscopies, when combined in laser-pump, X-ray-probe measurement schemes, can be powerful tools for tracking the electronic and geometric structural changes that occur during the course of a photoinitiated chemical reaction. X-ray absorption spectroscopy (XAS) is considered an established technique for such measurements, and X-ray emission spectroscopy (XES) of the strongest core-to-core emission lines (Kα and Kβ) is now being utilized. Flux demanding valence-to-core XES promises to be an important addition to the time-resolved spectroscopic toolkit. Here In this paper we present measurements and density functional theory calculations on laser-excited, solution-phase ferrocyanide that demonstrate the feasibility of valence-to-core XES formore » time-resolved experiments. Lastly, we discuss technical improvements that will make valence-to-core XES a practical pump–probe technique.« less

Extracting chemical information from high-resolution Kβ X-ray emission spectroscopy

NASA Astrophysics Data System (ADS)

Limandri, S.; Robledo, J.; Tirao, G.

2018-06-01

High-resolution X-ray emission spectroscopy allows studying the chemical environment of a wide variety of materials. Chemical information can be obtained by fitting the X-ray spectra and observing the behavior of some spectral features. Spectral changes can also be quantified by means of statistical parameters calculated by considering the spectrum as a probability distribution. Another possibility is to perform statistical multivariate analysis, such as principal component analysis. In this work the performance of these procedures for extracting chemical information in X-ray emission spectroscopy spectra for mixtures of Mn2+ and Mn4+ oxides are studied. A detail analysis of the parameters obtained, as well as the associated uncertainties is shown. The methodologies are also applied for Mn oxidation state characterization of double perovskite oxides Ba1+xLa1-xMnSbO6 (with 0 ≤ x ≤ 0.7). The results show that statistical parameters and multivariate analysis are the most suitable for the analysis of this kind of spectra.

Scanning electron microscopy and X-ray energy dispersive spectroscopy - useful tools in the analysis of pharmaceutical products

NASA Astrophysics Data System (ADS)

Sarecka-Hujar, Beata; Balwierz, Radoslaw; Ostrozka-Cieslik, Aneta; Dyja, Renata; Lukowiec, Dariusz; Jankowski, Andrzej

2017-11-01

The quality of the drug, its purity and identification of degradation products provide the highest quality of pharmaceutical products. The energy dispersive spectroscopy (EDS) method analyses the percentage of each element form as well as their distribution, and morphological characteristics of the drug form. We analysed the usefulness of EDS method in testing orally disintegrating tablets (ODT) with trimetazidine hydrochloride with high resolution scanning electron microscopy (SEM, SUPRA25 Carl Zeiss company) with spectrophotometer equipped with an X-ray energy dispersion (EDAX Company). The samples of the analysed tablets were imaged after applying conductive layers of gold on their surface. In the EDS analysis the compositions of each sample of the obtained tablets were observed to be virtually identical. The differences in the content of carbon and oxygen came from differences in the composition of particular tablets. The presence of gold in the composition resulted from the sputtering the surface of tablets with gold during the analysis. Knowing the composition of the tablet, SEM-EDS method helps to locate and identify the impurities and degradation products of the compounds, leading to a better understanding of the mechanisms of their formation.

STROBE-X: X-ray Timing & Spectroscopy on Dynamical Timescales from Microseconds to Years

NASA Astrophysics Data System (ADS)

Wilson-Hodge, Colleen A.; Ray, Paul S.; Maccarone, Thomas J.; Chakrabarty, Deepto; Gendreau, Keith C.; Arzoumanian, Zaven; Jenke, Peter; Ballantyne, David; Bozzo, Enrico; Brandt, Soren; Brenneman, Laura; Christophersen, Marc; DeRosa, Alessandra; Feroci, Marco; Goldstein, Adam; Hartmann, Dieter; Hernanz, Margarita; McDonald, Michael; Phlips, Bernard; Remillard, Ronald; Stevens, Abigail; Tomsick, John; Watts, Anna; Wood, Kent S.; Zane, Silvia; STROBE-X Collaboration

2018-01-01

We describe a probe-class mission concept that provides an unprecedented view of the X-ray sky, performing timing and 0.2-30 keV spectroscopy over timescales from microseconds to years. The Spectroscopic Time-Resolving Observatory for Broadband Energy X-rays (STROBE-X) comprises three primary instruments. The first uses an array of lightweight optics (3-m focal length) that concentrate incident photons onto solid state detectors with CCD-level (85-130 eV) energy resolution, 100 ns time resolution, and low background rates to cover the 0.2-12 keV band. This technology is scaled up from NICER, with enhanced optics to take advantage of the longer focal length of STROBE-X. The second uses large-area collimated silicon drift detectors, developed for ESA's LOFT, to cover the 2-30 keV band. These two instruments each provide an order of magnitude improvement in effective area compared with its predecessor (NICER and RXTE, respectively). Finally, a sensitive sky monitor triggers pointed observations, provides high duty cycle, high time resolution, high spectral resolution monitoring of the X-ray sky with ~20 times the sensitivity of the RXTE ASM, and enables multi-wavelength and multi-messenger studies on a continuous, rather than scanning basis. We include updated instrument designs resulting from the GSFC IDL run in November 2017.For the first time, the broad coverage provides simultaneous study of thermal components, non-thermal components, iron lines, and reflection features from a single platform for accreting black holes at all scales. The enormous collecting area allows detailed studies of the dense matter equation of state using both thermal emission from rotation-powered pulsars and harder emission from X-ray burst oscillations. The combination of the wide-field monitor and the sensitive pointed instruments enables observations of potential electromagnetic counterparts to LIGO/Virgo and neutrino events. Extragalactic science, such as constraining bulk metalicity

Hetero-site-specific X-ray pump-probe spectroscopy for femtosecond intramolecular dynamics

PubMed Central

Picón, A.; Lehmann, C. S.; Bostedt, C.; Rudenko, A.; Marinelli, A.; Osipov, T.; Rolles, D.; Berrah, N.; Bomme, C.; Bucher, M.; Doumy, G.; Erk, B.; Ferguson, K. R.; Gorkhover, T.; Ho, P. J.; Kanter, E. P.; Krässig, B.; Krzywinski, J.; Lutman, A. A.; March, A. M.; Moonshiram, D.; Ray, D.; Young, L.; Pratt, S. T.; Southworth, S. H.

2016-01-01

New capabilities at X-ray free-electron laser facilities allow the generation of two-colour femtosecond X-ray pulses, opening the possibility of performing ultrafast studies of X-ray-induced phenomena. Particularly, the experimental realization of hetero-site-specific X-ray-pump/X-ray-probe spectroscopy is of special interest, in which an X-ray pump pulse is absorbed at one site within a molecule and an X-ray probe pulse follows the X-ray-induced dynamics at another site within the same molecule. Here we show experimental evidence of a hetero-site pump-probe signal. By using two-colour 10-fs X-ray pulses, we are able to observe the femtosecond time dependence for the formation of F ions during the fragmentation of XeF2 molecules following X-ray absorption at the Xe site. PMID:27212390

Hetero-site-specific X-ray pump-probe spectroscopy for femtosecond intramolecular dynamics

DOE PAGES

Picón, A.; Lehmann, C. S.; Bostedt, C.; ...

2016-05-23

New capabilities at X-ray free-electron laser facilities allow the generation of two-colour femtosecond X-ray pulses, opening the possibility of performing ultrafast studies of X-ray-induced phenomena. Specifically, the experimental realization of hetero-site-specific X-ray-pump/X-ray-probe spectroscopy is of special interest, in which an X-ray pump pulse is absorbed at one site within a molecule and an X-ray probe pulse follows the X-ray-induced dynamics at another site within the same molecule. In this paper, we show experimental evidence of a hetero-site pump-probe signal. By using two-colour 10-fs X-ray pulses, we are able to observe the femtosecond time dependence for the formation of F ionsmore » during the fragmentation of XeF 2 molecules following X-ray absorption at the Xe site.« less

Hetero-site-specific X-ray pump-probe spectroscopy for femtosecond intramolecular dynamics.

PubMed

Picón, A; Lehmann, C S; Bostedt, C; Rudenko, A; Marinelli, A; Osipov, T; Rolles, D; Berrah, N; Bomme, C; Bucher, M; Doumy, G; Erk, B; Ferguson, K R; Gorkhover, T; Ho, P J; Kanter, E P; Krässig, B; Krzywinski, J; Lutman, A A; March, A M; Moonshiram, D; Ray, D; Young, L; Pratt, S T; Southworth, S H

2016-05-23

New capabilities at X-ray free-electron laser facilities allow the generation of two-colour femtosecond X-ray pulses, opening the possibility of performing ultrafast studies of X-ray-induced phenomena. Particularly, the experimental realization of hetero-site-specific X-ray-pump/X-ray-probe spectroscopy is of special interest, in which an X-ray pump pulse is absorbed at one site within a molecule and an X-ray probe pulse follows the X-ray-induced dynamics at another site within the same molecule. Here we show experimental evidence of a hetero-site pump-probe signal. By using two-colour 10-fs X-ray pulses, we are able to observe the femtosecond time dependence for the formation of F ions during the fragmentation of XeF2 molecules following X-ray absorption at the Xe site.

Multispecies Biofilms Transform Selenium Oxyanions into Elemental Selenium Particles: Studies Using Combined Synchrotron X-ray Fluorescence Imaging and Scanning Transmission X-ray Microscopy.

PubMed

Yang, Soo In; George, Graham N; Lawrence, John R; Kaminskyj, Susan G W; Dynes, James J; Lai, Barry; Pickering, Ingrid J

2016-10-04

Selenium (Se) is an element of growing environmental concern, because low aqueous concentrations can lead to biomagnification through the aquatic food web. Biofilms, naturally occurring microbial consortia, play numerous important roles in the environment, especially in biogeochemical cycling of toxic elements in aquatic systems. The complexity of naturally forming multispecies biofilms presents challenges for characterization because conventional microscopic techniques require chemical and physical modifications of the sample. Here, multispecies biofilms biotransforming selenium oxyanions were characterized using X-ray fluorescence imaging (XFI) and scanning transmission X-ray microscopy (STXM). These complementary synchrotron techniques required minimal sample preparation and were applied correlatively to the same biofilm areas. Sub-micrometer XFI showed distributions of Se and endogenous metals, while Se K-edge X-ray absorption spectroscopy indicated the presence of elemental Se (Se 0 ). Nanoscale carbon K-edge STXM revealed the distributions of microbial cells, extracellular polymeric substances (EPS), and lipids using the protein, saccharide, and lipid signatures, respectively, together with highly localized Se 0 using the Se L III edge. Transmission electron microscopy showed the electron-dense particle diameter to be 50-700 nm, suggesting Se 0 nanoparticles. The intimate association of Se 0 particles with protein and polysaccharide biofilm components has implications for the bioavailability of selenium in the environment.

Multispecies Biofilms Transform Selenium Oxyanions into Elemental Selenium Particles: Studies Using Combined Synchrotron X-ray Fluorescence Imaging and Scanning Transmission X-ray Microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Soo In; George, Graham N.; Lawrence, John R.

2016-10-04

Selenium (Se) is an element of growing environmental concern, because low aqueous concentrations can lead to biomagnification through the aquatic food web. Biofilms, naturally occurring microbial consortia, play numerous important roles in the environment, especially in biogeochemical cycling of toxic elements in aquatic systems. The complexity of naturally forming multispecies biofilms presents challenges for characterization because conventional microscopic techniques require chemical and physical modifications of the sample. Here, multispecies biofilms biotransforming selenium oxyanions were characterized using X-ray fluorescence imaging (XFI) and scanning transmission X-ray microscopy (STXM). These complementary synchrotron techniques required minimal sample preparation and were applied correlatively to themore » same biofilm areas. Sub-micrometer XFI showed distributions of Se and endogenous metals, while Se K-edge X-ray absorption spectroscopy indicated the presence of elemental Se (Se0). Nanoscale carbon K-edge STXM revealed the distributions of microbial cells, extracellular polymeric substances (EPS), and lipids using the protein, saccharide, and lipid signatures, respectively, together with highly localized Se0 using the Se LIII edge. Transmission electron microscopy showed the electron-dense particle diameter to be 50–700 nm, suggesting Se0 nanoparticles. The intimate association of Se0 particles with protein and polysaccharide biofilm components has implications for the bioavailability of selenium in the environment.« less

Coherent Multidimensional Core Spectroscopy of Molecules with Multiple X-ray pulses

NASA Astrophysics Data System (ADS)

Mukamel, Shaul

2017-04-01

Multidimensional spectroscopy uses sequences of optical pulses to study dynamical processes in complex molecules through correlation plots involving several time delay periods. Extensions of these techniques to the x-ray regime will be discussed. Ultrafast nonlinear x-ray spectroscopy is made possible by newly developed free electron laser and high harmonic generation sources. The attosecond duration of X-ray pulses and the atomic selectivity of core X-ray excitations offer a uniquely high spatial and temporal resolution. We demonstrate how stimulated Raman detection of an X-ray probe may be used to monitor the phase and dynamics of the nonequilibrium valence electronic state wavepacket created by e.g. photoexcitation, photoionization and Auger processes. Spectroscopy of multiplecore excitations provides a new window into electron correlations. Applications will be presented to long-range charge transfer in proteins and to excitation energy transfer in porphyrin arrays. Conical intersections (CoIn) dominate the pathways and outcomes of virtually all photophysical and photochemical molecular processes. Despite extensive experimental and theoretical effort CoIns have not been directly observed yet and the experimental evidence is being inferred from fast reaction rates and some vibrational signatures. Novel ultrafast X ray probes for these processes will be presented. Short X-ray pulses can directly detect the passage through a CoIn with the adequate temporal and spectral sensitivity. The technique is based on a coherent Raman process that employs a composite femtosecond/attosecond X-ray pulse to directly detect the electronic coherences (rather than populations) that are generated as the system passes through the CoIn. Streaking of time-resolved photoelectron spectroscopy (TRPES) signals offers another powerful window into the joint electronic/vibrational dynamics at concial intersections. Strong coupling of molecules to the vacuum field of micro cavities can modify

Pixel detectors for x-ray imaging spectroscopy in space

NASA Astrophysics Data System (ADS)

Treis, J.; Andritschke, R.; Hartmann, R.; Herrmann, S.; Holl, P.; Lauf, T.; Lechner, P.; Lutz, G.; Meidinger, N.; Porro, M.; Richter, R. H.; Schopper, F.; Soltau, H.; Strüder, L.

2009-03-01

Pixelated semiconductor detectors for X-ray imaging spectroscopy are foreseen as key components of the payload of various future space missions exploring the x-ray sky. Located on the platform of the new Spectrum-Roentgen-Gamma satellite, the eROSITA (extended Roentgen Survey with an Imaging Telescope Array) instrument will perform an imaging all-sky survey up to an X-ray energy of 10 keV with unprecedented spectral and angular resolution. The instrument will consist of seven parallel oriented mirror modules each having its own pnCCD camera in the focus. The satellite born X-ray observatory SIMBOL-X will be the first mission to use formation-flying techniques to implement an X-ray telescope with an unprecedented focal length of around 20 m. The detector instrumentation consists of separate high- and low energy detectors, a monolithic 128 × 128 DEPFET macropixel array and a pixellated CdZTe detector respectively, making energy band between 0.5 to 80 keV accessible. A similar concept is proposed for the next generation X-ray observatory IXO. Finally, the MIXS (Mercury Imaging X-ray Spectrometer) instrument on the European Mercury exploration mission BepiColombo will use DEPFET macropixel arrays together with a small X-ray telescope to perform a spatially resolved planetary XRF analysis of Mercury's crust. Here, the mission concepts and their scientific targets are briefly discussed, and the resulting requirements on the detector devices together with the implementation strategies are shown.

Elemental-sensitive Detection of the Chemistry in Batteries through Soft X-ray Absorption Spectroscopy and Resonant Inelastic X-ray Scattering.

PubMed

Wu, Jinpeng; Sallis, Shawn; Qiao, Ruimin; Li, Qinghao; Zhuo, Zengqing; Dai, Kehua; Guo, Zixuan; Yang, Wanli

2018-04-17

Energy storage has become more and more a limiting factor of today's sustainable energy applications, including electric vehicles and green electric grid based on volatile solar and wind sources. The pressing demand of developing high-performance electrochemical energy storage solutions, i.e., batteries, relies on both fundamental understanding and practical developments from both the academy and industry. The formidable challenge of developing successful battery technology stems from the different requirements for different energy-storage applications. Energy density, power, stability, safety, and cost parameters all have to be balanced in batteries to meet the requirements of different applications. Therefore, multiple battery technologies based on different materials and mechanisms need to be developed and optimized. Incisive tools that could directly probe the chemical reactions in various battery materials are becoming critical to advance the field beyond its conventional trial-and-error approach. Here, we present detailed protocols for soft X-ray absorption spectroscopy (sXAS), soft X-ray emission spectroscopy (sXES), and resonant inelastic X-ray scattering (RIXS) experiments, which are inherently elemental-sensitive probes of the transition-metal 3d and anion 2p states in battery compounds. We provide the details on the experimental techniques and demonstrations revealing the key chemical states in battery materials through these soft X-ray spectroscopy techniques.

Soft x-ray spectromicroscopy using compact scanning transmission x-ray microscope at the photon factory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takeichi, Yasuo, E-mail: yasuo.takeichi@kek.jp; Inami, Nobuhito; Ono, Kanta

We report the stability and recent performances of a new type of scanning transmission X-ray microscopy. The optics and compact design of the microscope realized mobility and robust performance. Detailed consideration to the vibration control will be described. The insertion device upgraded to elliptical polarization undulator enabled linear dichroism and circular dichroism experiments.

3D chemical mapping: application of scanning transmission (soft) X-ray microscopy (STXM) in combination with angle-scan tomography in bio-, geo-, and environmental sciences.

PubMed

Obst, Martin; Schmid, Gregor

2014-01-01

The identification of environmental processes and mechanisms often requires information on the organochemical and inorganic composition of specimens at high spatial resolution. X-ray spectroscopy (XAS) performed in the soft X-ray range (100-2,200 eV) provides chemical speciation information for elements that are of high biogeochemical relevance such as carbon, nitrogen, and oxygen but also includes transition metals such as iron, manganese, or nickel. Synchrotron-based scanning transmission X-ray microscopy (STXM) combines XAS with high resolution mapping on the 20-nm scale. This provides two-dimensional (2D) quantitative information about the distribution of chemical species such as organic macromolecules, metals, or mineral phases within environmental samples. Furthermore, the combination of STXM with angle-scan tomography allows for three-dimensional (3D) spectromicroscopic analysis of bio-, geo-, or environmental samples. For the acquisition of STXM tomography data, the sample is rotated around an axis perpendicular to the X-ray beam. Various sample preparation approaches such as stripes cut from TEM grids or the preparation of wet cells allow for preparing environmentally relevant specimens in a dry or in a fully hydrated state for 2D and 3D STXM measurements. In this chapter we give a short overview about the principles of STXM, its application to environmental sciences, different preparation techniques, and the analysis and 3D reconstruction of STXM tomography data.

Probing molecular dynamics in solution with x-ray valence-to-core spectroscopy

NASA Astrophysics Data System (ADS)

Doumy, Gilles; March, Anne Marie; Tu, Ming-Feng; Al Haddad, Andre; Southworth, Stephen; Young, Linda; Walko, Donald; Bostedt, Christoph

2017-04-01

Hard X-ray spectroscopies are powerful tools for probing the electronic and geometric structure of molecules in complex or disordered systems and have been particularly useful for studying molecules in the solution phase. They are element specific, sensitive to the electronic structure and the local arrangements of surrounding atoms of the element being selectively probed. When combined in a pump-probe scheme with ultrafast lasers, X-ray spectroscopies can be used to track the evolution of structural changes that occur after photoexcitation. Efficient use of hard x-ray radiation coming from high brilliance synchrotrons and upcoming high repetition rate X-ray Free Electron Lasers requires MHz repetition rate lasers and data acquisition systems. High information content Valence-to-Core x-ray emission is directly sensitive to the molecular orbitals involved in photochemistry. We report on recent progress towards fully enabling this photon-hungry technique for the study of time-resolved molecular dynamics, including efficient detection and use of polychromatic x-ray micro-probe at the Advanced Photon Source. Work was supported by the U.S. Department of Energy, Office of Science, Chemical Sciences, Geosciences, and Biosciences Division.

New developments in high pressure x-ray spectroscopy beamline at High Pressure Collaborative Access Team

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xiao, Y. M., E-mail: yxiao@carnegiescience.edu; Chow, P.; Boman, G.

The 16 ID-D (Insertion Device - D station) beamline of the High Pressure Collaborative Access Team at the Advanced Photon Source is dedicated to high pressure research using X-ray spectroscopy techniques typically integrated with diamond anvil cells. The beamline provides X-rays of 4.5-37 keV, and current available techniques include X-ray emission spectroscopy, inelastic X-ray scattering, and nuclear resonant scattering. The recent developments include a canted undulator upgrade, 17-element analyzer array for inelastic X-ray scattering, and an emission spectrometer using a polycapillary half-lens. Recent development projects and future prospects are also discussed.

Hard x-ray scanning imaging achieved with bonded multilayer Laue lenses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Xiaojing; Xu, Weihe; Nazaretski, Evgeny

Here, we report scanning hard x-ray imaging with a monolithic focusing optic consisting of two multilayer Laue lenses (MLLs) bonded together. With optics pre-characterization and accurate control of the bonding process, we show that a common focal plane for both MLLs can be realized at 9.317 keV. Using bonded MLLs, we obtained a scanning transmission image of a star test pattern with a resolution of 50 × 50 nm 2. By applying a ptychography algorithm, we obtained a probe size of 17 × 38 nm 2 and an object image with a resolution of 13 × 13 nm 2. Finally,more » the significant reduction in alignment complexity for bonded MLLs will greatly extend the application range in both scanning and full-field x-ray microscopies.« less

Hard x-ray scanning imaging achieved with bonded multilayer Laue lenses

DOE PAGES

Huang, Xiaojing; Xu, Weihe; Nazaretski, Evgeny; ...

2017-04-05

Here, we report scanning hard x-ray imaging with a monolithic focusing optic consisting of two multilayer Laue lenses (MLLs) bonded together. With optics pre-characterization and accurate control of the bonding process, we show that a common focal plane for both MLLs can be realized at 9.317 keV. Using bonded MLLs, we obtained a scanning transmission image of a star test pattern with a resolution of 50 × 50 nm 2. By applying a ptychography algorithm, we obtained a probe size of 17 × 38 nm 2 and an object image with a resolution of 13 × 13 nm 2. Finally,more » the significant reduction in alignment complexity for bonded MLLs will greatly extend the application range in both scanning and full-field x-ray microscopies.« less

Soft x-ray spectroscopy studies of novel electronic materials using synchrotron radiation

NASA Astrophysics Data System (ADS)

Newby, David, Jr.

Soft x-ray spectroscopy can provide a wealth of information on the electronic structure of solids. In this work, a suite of soft x-ray spectroscopies is applied to organic and inorganic materials with potential applications in electronic and energy generation devices. Using the techniques of x-ray absorption (XAS), x-ray emission spectroscopy (XES), and x-ray photoemission spectroscopy (XPS), the fundamental properties of these different materials are explored. Cycloparaphenylenes (CPPs) are a recently synthesized family of cyclic hydrocarbons with very interesting properties and many potential applications. Unusual UV/Visible fluorescence trends have spurred a number of theoretical investigations into the electronic properties of the CPP family, but thus far no comprehensive electronic structure measurements have been conducted. XPS, XAS, and XES data for two varieties, [8]- and [10]-CPP, are presented here, and compared with the results of relevant DFT calculations. Turning towards more application-centered investigations, similar measurements are applied to two materials commonly used in solid oxide fuel cell (SOFC) cathodes: La1-xSrxMnO 3 (LSMO) and La1-xSr1- xCo1-yFe yO3 (LSCF). Both materials are structurally perovskites, but they exhibit strikingly different electronic properties. SOFC systems very efficiently produce electricity by catalyzing reactions between oxygen and petroleum-based hydrocarbons at high temperatures (> 800 C). Such systems are already utilized to great effect in many industries, but more widespread adoption could be had if the cells could operate at lower temperatures. Understanding the electronic structure and operational evolution of the cathode materials is essential for the development of better low-temperature fuel cells. LSCF is a mixed ion-electron conductor which holds promise for low-temperature SOFC applications. XPS spectra of LSCF thin films are collected as the films are heated and gas-dosed in a controlled environment. The

Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

DOE PAGES

Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; ...

2012-11-05

The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as wellmore » as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ 1,3 XES spectra of Mn II and Mn 2 III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. Furthermore, the technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II.« less

Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

PubMed Central

Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Lassalle-Kaiser, Benedikt; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Hellmich, Julia; Glöckner, Carina; Echols, Nathaniel; Sierra, Raymond G.; Schafer, Donald W.; Sellberg, Jonas; Kenney, Christopher; Herbst, Ryan; Pines, Jack; Hart, Philip; Herrmann, Sven; Grosse-Kunstleve, Ralf W.; Latimer, Matthew J.; Fry, Alan R.; Messerschmidt, Marc M.; Miahnahri, Alan; Seibert, M. Marvin; Zwart, Petrus H.; White, William E.; Adams, Paul D.; Bogan, Michael J.; Boutet, Sébastien; Williams, Garth J.; Zouni, Athina; Messinger, Johannes; Glatzel, Pieter; Sauter, Nicholas K.; Yachandra, Vittal K.; Yano, Junko; Bergmann, Uwe

2012-01-01

The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as well as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ1,3 XES spectra of MnII and Mn2III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. The technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II. PMID:23129631

Searching for outflows in ultraluminous X-ray sources through high-resolution X-ray spectroscopy

NASA Astrophysics Data System (ADS)

Kosec, P.; Pinto, C.; Fabian, A. C.; Walton, D. J.

2018-02-01

Ultraluminous X-ray sources (ULXs) are non-nuclear point sources exceeding the Eddington luminosity of a 10 M⊙ black hole. Modern consensus for a majority of the ULX population is that they are powered by stellar-mass black holes or neutron stars accreting well above the Eddington limit. Theoretical models of super-Eddington accretion predict existence of powerful outflows of moderately ionized gas at mildly relativistic velocities. So far, these winds have been found in three systems: NGC 1313 X-1, NGC 5408 X-1 and NGC 55 ULX. In this work, we create a sample of all ULXs with usable archival high-resolution X-ray data, with 10 sources in total, in which we aim to find more signatures of outflows. We perform Gaussian line scans to find any narrow spectral signatures, and physical wind model scans where possible. We tentatively identify an outflow in NGC 5204 X-1, blueshifted to 0.34c, which produces emission features with a total significance of at least 3σ. Next we compare ULXs with similar hardness ratios. Holmberg IX X-1 shows absorption features that could be associated with a photoionized outflowing absorber, similar to that seen in NGC 1313 X-1. The spectrum of Holmberg II X-1 possesses features similar to NGC 5408 X-1 and NGC 6946 X-1 shows O VIII rest-frame emission. All other sources from the sample also show tentative evidence of spectral features in their high-resolution spectra. Further observations with the XMM-Newton and Chandra gratings will place stronger constraints. Future missions like XARM and Athena will be able to detect them at larger distances and increase our sample.

Electron cyclotron resonance ion source plasma characterization by X-ray spectroscopy and X-ray imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mascali, David, E-mail: davidmascali@lns.infn.it; Castro, Giuseppe; Celona, Luigi

2016-02-15

An experimental campaign aiming to investigate electron cyclotron resonance (ECR) plasma X-ray emission has been recently carried out at the ECRISs—Electron Cyclotron Resonance Ion Sources laboratory of Atomki based on a collaboration between the Debrecen and Catania ECR teams. In a first series, the X-ray spectroscopy was performed through silicon drift detectors and high purity germanium detectors, characterizing the volumetric plasma emission. The on-purpose developed collimation system was suitable for direct plasma density evaluation, performed “on-line” during beam extraction and charge state distribution characterization. A campaign for correlating the plasma density and temperature with the output charge states and themore » beam intensity for different pumping wave frequencies, different magnetic field profiles, and single-gas/gas-mixing configurations was carried out. The results reveal a surprisingly very good agreement between warm-electron density fluctuations, output beam currents, and the calculated electromagnetic modal density of the plasma chamber. A charge-coupled device camera coupled to a small pin-hole allowing X-ray imaging was installed and numerous X-ray photos were taken in order to study the peculiarities of the ECRIS plasma structure.« less

Preparation and characterization of polymer layer systems for validation of 3D Micro X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Schaumann, Ina; Malzer, Wolfgang; Mantouvalou, Ioanna; Lühl, Lars; Kanngießer, Birgit; Dargel, Rainer; Giese, Ulrich; Vogt, Carla

2009-04-01

For the validation of the quantification of the newly-developed method of 3D Micro X-ray fluorescence spectroscopy (3D Micro-XRF) samples with a low average Z matrix and minor high Z elements are best suited. In a light matrix the interferences by matrix effects are minimized so that organic polymers are appropriate as basis for analytes which are more easily detected by X-ray fluorescence spectroscopy. Polymer layer systems were assembled from single layers of ethylene-propylene-diene rubber (EPDM) filled with changing concentrations of silica and zinc oxide as inorganic additives. Layer thicknesses were in the range of 30-150 μm. Before the analysis with 3D Micro-XRF all layers have been characterized by scanning micro-XRF with regard to filler dispersion, by infrared microscopy and light microscopy in order to determine the layer thicknesses and by ICP-OES to verify the concentration of the X-ray sensitive elements in the layers. With the results obtained for stacked polymer systems the validity of the analytical quantification model for the determination of stratified materials by 3D Micro-XRF could be demonstrated.

LabVIEW control software for scanning micro-beam X-ray fluorescence spectrometer.

PubMed

Wrobel, Pawel; Czyzycki, Mateusz; Furman, Leszek; Kolasinski, Krzysztof; Lankosz, Marek; Mrenca, Alina; Samek, Lucyna; Wegrzynek, Dariusz

2012-05-15

Confocal micro-beam X-ray fluorescence microscope was constructed. The system was assembled from commercially available components - a low power X-ray tube source, polycapillary X-ray optics and silicon drift detector - controlled by an in-house developed LabVIEW software. A video camera coupled to optical microscope was utilized to display the area excited by X-ray beam. The camera image calibration and scan area definition software were also based entirely on LabVIEW code. Presently, the main area of application of the newly constructed spectrometer is 2-dimensional mapping of element distribution in environmental, biological and geological samples with micrometer spatial resolution. The hardware and the developed software can already handle volumetric 3-D confocal scans. In this work, a front panel graphical user interface as well as communication protocols between hardware components were described. Two applications of the spectrometer, to homogeneity testing of titanium layers and to imaging of various types of grains in air particulate matter collected on membrane filters, were presented. Copyright © 2012 Elsevier B.V. All rights reserved.

AXSIS: Exploring the frontiers in attosecond X-ray science, imaging and spectroscopy.

PubMed

Kärtner, F X; Ahr, F; Calendron, A-L; Çankaya, H; Carbajo, S; Chang, G; Cirmi, G; Dörner, K; Dorda, U; Fallahi, A; Hartin, A; Hemmer, M; Hobbs, R; Hua, Y; Huang, W R; Letrun, R; Matlis, N; Mazalova, V; Mücke, O D; Nanni, E; Putnam, W; Ravi, K; Reichert, F; Sarrou, I; Wu, X; Yahaghi, A; Ye, H; Zapata, L; Zhang, D; Zhou, C; Miller, R J D; Berggren, K K; Graafsma, H; Meents, A; Assmann, R W; Chapman, H N; Fromme, P

2016-09-01

X-ray crystallography is one of the main methods to determine atomic-resolution 3D images of the whole spectrum of molecules ranging from small inorganic clusters to large protein complexes consisting of hundred-thousands of atoms that constitute the macromolecular machinery of life. Life is not static, and unravelling the structure and dynamics of the most important reactions in chemistry and biology is essential to uncover their mechanism. Many of these reactions, including photosynthesis which drives our biosphere, are light induced and occur on ultrafast timescales. These have been studied with high time resolution primarily by optical spectroscopy, enabled by ultrafast laser technology, but they reduce the vast complexity of the process to a few reaction coordinates. In the AXSIS project at CFEL in Hamburg, funded by the European Research Council, we develop the new method of attosecond serial X-ray crystallography and spectroscopy, to give a full description of ultrafast processes atomically resolved in real space and on the electronic energy landscape, from co-measurement of X-ray and optical spectra, and X-ray diffraction. This technique will revolutionize our understanding of structure and function at the atomic and molecular level and thereby unravel fundamental processes in chemistry and biology like energy conversion processes. For that purpose, we develop a compact, fully coherent, THz-driven atto-second X-ray source based on coherent inverse Compton scattering off a free-electron crystal, to outrun radiation damage effects due to the necessary high X-ray irradiance required to acquire diffraction signals. This highly synergistic project starts from a completely clean slate rather than conforming to the specifications of a large free-electron laser (FEL) user facility, to optimize the entire instrumentation towards fundamental measurements of the mechanism of light absorption and excitation energy transfer. A multidisciplinary team formed by laser

Probing molecular orientations in thin films by x-ray photoelectron spectroscopy

NASA Astrophysics Data System (ADS)

Li, Y.; Li, P.; Lu, Z.-H.

2018-03-01

A great number of functional organic molecules in active thin-film layers of optoelectronic devices have highly asymmetric structures, such as plate-like, rod-like, etc. This makes molecular orientation an important aspect in thin-films as it can significantly affect both the optical and electrical performance of optoelectronic devices. With a combination of in-situ ultra violet photoelectron spectroscopy (UPS) and x-ray photoelectron spectroscopy (XPS) investigations for organic molecules having a broad range of structural properties, we discovered a rigid connection of core levels and frontier highest occupied molecular orbital levels at organic interfaces. This finding opens up opportunities of using X-ray photoemission spectroscopy as an alternative tool to UPS for providing an easy and unambiguous data interpretation in probing molecular orientations.

Nanoparticle characterization by means of scanning free grazing emission X-ray fluorescence

NASA Astrophysics Data System (ADS)

Kayser, Yves; Sá, Jacinto; Szlachetko, Jakub

2015-05-01

Nanoparticles are considered for applications in domains as various as medical and pharmaceutical sciences, opto- and microelectronics, catalysis, photovoltaics, spintronics or nano- and biotechnology. The applications realized with nanocrystals depend strongly on the physical dimensions (shape and size) and elemental constitution. We demonstrate here that grazing emission X-ray fluorescence (GEXRF) is an element sensitive technique that presents the potential for a reliable and accurate determination of the morphology of nanoparticles deposited on a flat substrate (ready-to-use devices). Thanks to the scanning-free approach of the used GEXRF setup, the composition, shape and average size of nanoparticles are determined in short time intervals, minimizing the exposure to radiation. The (scanning-free) GEXRF technique allows for in situ investigations of the nanoparticulate systems thanks to the penetration properties of both the probe X-ray beam and the emitted X-ray fluorescence signal.

Characterization of copper oxides, iron oxides, and zinc copper ferrite desulfurization sorbents by X-ray photoelectron spectroscopy and scanning electron microscopy

NASA Astrophysics Data System (ADS)

Siriwardane, Ranjani V.; Poston, James A.

1993-05-01

Characterization of copper oxides, iron oxides, and zinc copper ferrite desulfurization sorbents was performed by X-ray photoelectron spectroscopy and scanning electron microscopy/energy-dispersive spectroscopy at temperatures of 298 to 823 K. Analysis of copper oxides indicated that the satellite structure of the Cu22p region was absent in the Cu(I) state but was present in the Cu(II) state. Reduction of CuO at room temperature was observed when the ion gauge was placed close to the sample. The satellite structure was absent in all the copper oxides at 823 K in vacuum. Differentiation of the oxidation state of copper utilizing both Cu(L 3M 4,5M 4,5) X-ray-induced Auger lines and Cu2p satellite structure, indicated that the copper in zinc copper ferrite was in the + 1 oxidation state at 823 K. This + 1 state of copper was not significantly changed after exposure to H 2, CO, and H 2O. There was an increase in Cu/Zn ratio and a decrease in Fe/Zn ratio on the surface of zinc copper ferrite at 823 K compared to that at room temperature. These conditions of copper offered the best sulfidation equilibrium for the zinc copper ferrite desulfurization sorbent. Analysis of iron oxides indicated that there was some reduction of both Fe 2O 3 and FeO at 823K. The iron in zinc copper ferrite was similar to that of Fe 2O 3 at room temperature but there was some reduction of this Fe(III) state to Fe(II) at 823 K. This reduction was more enhanced in the presence of H 2 and CO. Reduction to Fe(II) may not be desirable for the lifetime of the sorbent.

X-ray Photoelectron Spectroscopy Database (Version 4.1)

National Institute of Standards and Technology Data Gateway

SRD 20 X-ray Photoelectron Spectroscopy Database (Version 4.1) (Web, free access)   The NIST XPS Database gives access to energies of many photoelectron and Auger-electron spectral lines. The database contains over 22,000 line positions, chemical shifts, doublet splittings, and energy separations of photoelectron and Auger-electron lines.

Chemical speciation using high energy resolution PIXE spectroscopy in the tender X-ray range

NASA Astrophysics Data System (ADS)

Kavčič, Matjaž; Petric, Marko; Vogel-Mikuš, Katarina

2018-02-01

High energy resolution X-ray emission spectroscopy employing wavelength dispersive (WDS) crystal spectrometers can provide energy resolution on the level of core-hole lifetime broadening of the characteristic emission lines. While crystal spectrometers have been traditionally used in combination with electron excitation for major and minor element analysis, they have been rarely considered in proton induced X-ray emission (PIXE) trace element analysis mainly due to low detection efficiency. Compared to the simplest flat crystal WDS spectrometer the efficiency can be improved by employing cylindrically or even spherically curved crystals in combination with position sensitive X-ray detectors. When such spectrometer is coupled to MeV proton excitation, chemical bonding effects are revealed in the high energy resolution spectra yielding opportunity to extend the analytical capabilities of PIXE technique also towards chemical state analysis. In this contribution we will focus on the high energy resolution PIXE (HR-PIXE) spectroscopy in the tender X-ray range performed in our laboratory with our home-built tender X-ray emission spectrometer. Some general properties of high energy resolution PIXE spectroscopy in the tender X-ray range are presented followed by an example of sulfur speciation in biological tissue illustrating the capabilities as well as limitations of HR-PIXE method used for chemical speciation in the tender X-ray range.

High-resolution X-ray emission spectroscopy with transition-edge sensors: present performance and future potential

DOE Office of Scientific and Technical Information (OSTI.GOV)

Uhlig, J.; Doriese, W. B.; Fowler, J. W.

2015-04-21

X-ray emission spectroscopy (XES) is a powerful element-selective tool to analyze the oxidation states of atoms in complex compounds, determine their electronic configuration, and identify unknown compounds in challenging environments. Until now the low efficiency of wavelength-dispersive X-ray spectrometer technology has limited the use of XES, especially in combination with weaker laboratory X-ray sources. More efficient energy-dispersive detectors have either insufficient energy resolution because of the statistical limits described by Fano or too low counting rates to be of practical use. This paper updates an approach to high-resolution X-ray emission spectroscopy that uses a microcalorimeter detector array of superconducting transition-edgemore » sensors (TESs). TES arrays are discussed and compared with conventional methods, and shown under which circumstances they are superior. It is also shown that a TES array can be integrated into a table-top time-resolved X-ray source and a soft X-ray synchrotron beamline to perform emission spectroscopy with good chemical sensitivity over a very wide range of energies.« less

Development of picosecond time-resolved X-ray absorption spectroscopy by high-repetition-rate laser pump/X-ray probe at Beijing Synchrotron Radiation Facility.

PubMed

Wang, Hao; Yu, Can; Wei, Xu; Gao, Zhenhua; Xu, Guang Lei; Sun, Da Rui; Li, Zhenjie; Zhou, Yangfan; Li, Qiu Ju; Zhang, Bing Bing; Xu, Jin Qiang; Wang, Lin; Zhang, Yan; Tan, Ying Lei; Tao, Ye

2017-05-01

A new setup and commissioning of transient X-ray absorption spectroscopy are described, based on the high-repetition-rate laser pump/X-ray probe method, at the 1W2B wiggler beamline at the Beijing Synchrotron Radiation Facility. A high-repetition-rate and high-power laser is incorporated into the setup with in-house-built avalanche photodiodes as detectors. A simple acquisition scheme was applied to obtain laser-on and laser-off signals simultaneously. The capability of picosecond transient X-ray absorption spectroscopy measurement was demonstrated for a photo-induced spin-crossover iron complex in 6 mM solution with 155 kHz repetition rate.

X-ray magnetic circular dichroism and hard X-ray photoelectron spectroscopy of tetragonal Mn72Ge28 epitaxial thin film

NASA Astrophysics Data System (ADS)

Kim, Jinhyeok; Mizuguchi, Masaki; Inami, Nobuhito; Ueno, Tetsuro; Ueda, Shigenori; Takanashi, Koki

2018-04-01

An epitaxially grown Mn72Ge28 film with a tetragonal crystal structure was fabricated. It was clarified that the film had a perpendicular magnetization and a high perpendicular magnetic anisotropy energy of 14.3 Merg/cm3. The electronic structure was investigated by X-ray magnetic circular dichroism and hard X-ray photoelectron spectroscopy. The obtained X-ray magnetic circular dichroism spectrum revealed that the Mn orbital magnetic moment governed the magnetocrystalline anisotropy of the Mn72Ge28 film. A doublet structure was observed for the Mn 2p3/2 peak of hard X-ray photoelectron spectrum, indicating the spin exchange interaction between the 2p core-hole and 3d valence electrons.

Theory and optical design of x-ray echo spectrometers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shvyd'ko, Yuri

X-ray echo spectroscopy, a space-domain counterpart of neutron spin echo, is a recently proposed inelastic x-ray scattering (IXS) technique. X-ray echo spectroscopy relies on imaging IXS spectra and does not require x-ray monochromatization. Due to this, the echo-type IXS spectrometers are broadband, and thus have a potential to simultaneously provide dramatically increased signal strength, reduced measurement times, and higher resolution compared to the traditional narrow-band scanning-type IXS spectrometers. The theory of x-ray echo spectrometers presented earlier [Yu. Shvyd'ko, Phys. Rev. Lett. 116, 080801 (2016)] is developed here further with a focus on questions of practical importance, which could facilitate opticalmore » design and assessment of the feasibility and performance of the echo spectrometers. Among others, the following questions are addressed: spectral resolution, refocusing condition, echo spectrometer tolerances, refocusing condition adjustment, effective beam size on the sample, spectral window of imaging and scanning range, impact of the secondary source size on the spectral resolution, angular dispersive optics, focusing and collimating optics, and detector's spatial resolution. In conclusion, examples of optical designs and characteristics of echo spectrometers with 1-meV and 0.1-meV resolutions are presented.« less

Theory and optical design of x-ray echo spectrometers

DOE PAGES

Shvyd'ko, Yuri

2017-08-02

X-ray echo spectroscopy, a space-domain counterpart of neutron spin echo, is a recently proposed inelastic x-ray scattering (IXS) technique. X-ray echo spectroscopy relies on imaging IXS spectra and does not require x-ray monochromatization. Due to this, the echo-type IXS spectrometers are broadband, and thus have a potential to simultaneously provide dramatically increased signal strength, reduced measurement times, and higher resolution compared to the traditional narrow-band scanning-type IXS spectrometers. The theory of x-ray echo spectrometers presented earlier [Yu. Shvyd'ko, Phys. Rev. Lett. 116, 080801 (2016)] is developed here further with a focus on questions of practical importance, which could facilitate opticalmore » design and assessment of the feasibility and performance of the echo spectrometers. Among others, the following questions are addressed: spectral resolution, refocusing condition, echo spectrometer tolerances, refocusing condition adjustment, effective beam size on the sample, spectral window of imaging and scanning range, impact of the secondary source size on the spectral resolution, angular dispersive optics, focusing and collimating optics, and detector's spatial resolution. In conclusion, examples of optical designs and characteristics of echo spectrometers with 1-meV and 0.1-meV resolutions are presented.« less

Probing interfacial characteristics of rubrene/pentacene and pentacene/rubrene bilayers with soft X-ray spectroscopy.

PubMed

Seo, J H; Pedersen, T M; Chang, G S; Moewes, A; Yoo, K-H; Cho, S J; Whang, C N

2007-08-16

The electronic structure of rubrene/pentacene and pentacene/rubrene bilayers has been investigated using soft X-ray absorption spectroscopy, resonant X-ray emission spectroscopy, and density-functional theory calculations. X-ray absorption and emission measurements reveal that it has been possible to alter the lowest unoccupied and the highest occupied molecular orbital states of rubrene in rubrene/pentacene bilayer. In the reverse case, one gets p* molecular orbital states originating from the pentacene layer. Resonant X-ray emission spectra suggest a reduction in the hole-transition probabilities for the pentacene/rubrene bilayer in comparison to reference pentacene layer. For the rubrenepentacene structure, the hole-transition probability shows an increase in comparison to the rubrene reference. We also determined the energy level alignment of the pentacene-rubrene interface by using X-ray and ultraviolet photoelectron spectroscopy. From these comparisons, it is found that the electronic structure of the pentacene-rubrene interface has a strong dependence on interface characteristics which depends on the order of the layers used.

Imaging connected porosity of crystalline rock by contrast agent-aided X-ray microtomography and scanning electron microscopy.

PubMed

Kuva, J; Sammaljärvi, J; Parkkonen, J; Siitari-Kauppi, M; Lehtonen, M; Turpeinen, T; Timonen, J; Voutilainen, M

2018-04-01

We set out to study connected porosity of crystalline rock using X-ray microtomography and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) with caesium chloride as a contrast agent. Caesium is an important radionuclide regarding the final deposition of nuclear waste and also forms dense phases that can be readily distinguished by X-ray microtomography and SEM-EDS. Six samples from two sites, Olkiluoto (Finland) and Grimsel (Switzerland), where transport properties of crystalline rock are being studied in situ, were investigated using X-ray microtomography and SEM-EDS. The samples were imaged with X-ray microtomography, immersed in a saturated caesium chloride (CsCl) solution for 141, 249 and 365 days and imaged again with X-ray microtomography. CsCl inside the samples was successfully detected with X-ray microtomography and it had completely penetrated all six samples. SEM-EDS elemental mapping was used to study the location of caesium in the samples in detail with quantitative mineral information. Precipitated CsCl was found in the connected pore space in Olkiluoto veined gneiss and in lesser amounts in Grimsel granodiorite. Only a very small amount of precipitated CsCl was observed in the Grimsel granodiorite samples. In Olkiluoto veined gneiss caesium was found in pinitised areas of cordierite grains. In the pinitised areas caesium was found in notable excess compared to chloride, possibly due to the combination of small pore size and negatively charged surfaces. In addition, elevated concentrations of caesium were found in kaolinite and sphalerite phases. The findings concerning the location of CsCl were congruent with X-ray microtomography. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Nanosecond X-ray Photon Correlation Spectroscopy on Magnetic Skyrmions

DOE PAGES

Seaberg, M. H.; Holladay, B.; Lee, J. C. T.; ...

2017-08-09

We report an X-ray photon correlation spectroscopy method that exploits the recent development of the two-pulse mode at the Linac Coherent Light Source. By using coherent resonant X-ray magnetic scattering, we studied spontaneous fluctuations on nanosecond timescales in thin films of multilayered Fe/Gd that exhibit ordered stripe and skyrmion lattice phases. The correlation time of the fluctuations was found to differ between the skyrmion phase and near the stripe-skyrmion boundary. As a result, this technique will enable a significant new area of research on the study of equilibrium fluctuations in condensed matter.

Nanosecond X-ray Photon Correlation Spectroscopy on Magnetic Skyrmions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Seaberg, M. H.; Holladay, B.; Lee, J. C. T.

We report an X-ray photon correlation spectroscopy method that exploits the recent development of the two-pulse mode at the Linac Coherent Light Source. By using coherent resonant X-ray magnetic scattering, we studied spontaneous fluctuations on nanosecond timescales in thin films of multilayered Fe/Gd that exhibit ordered stripe and skyrmion lattice phases. The correlation time of the fluctuations was found to differ between the skyrmion phase and near the stripe-skyrmion boundary. As a result, this technique will enable a significant new area of research on the study of equilibrium fluctuations in condensed matter.

X-Ray Spectroscopies of Warm Dense Matter

NASA Astrophysics Data System (ADS)

Hoidn, Oliver

This dissertation provides a perspective on the role of x-ray spectroscopy and diffraction diagnostics in experimental studies of warm dense matter (WDM). The primary focus of the work I discuss is the development of techniques to measure the structure and state variables of laboratory-generated WDM with a view towards both phenomenlogy and placing contraints on theoretical models. I present techniques adapted to two experimental venues for WDM studies: large-scale laser plasma facilities and x-ray free electron lasers. My focus is on the latter, in the context of which I have studied a dose enhancement technique that exploits nonlocal heat transport in nanostructured targets and considered several aspects of optimizing x-ray diffraction measurements. This work came into play in beam runs at the Linac Coherent Light Source (LCLS) in which my group performed x-ray diffraction studies of several materials heated to eV-scale temperatures. The results from these experiments include confirmation of the persistence of long-range crystalline order upon heating of metal oxides to tens of eV temperarures on the 40 fs timescale. One material, MgO, additionally manifested a surprising anomalous early onset in delocalization of valence charge density, contradicting predictions of all models based on either ground state electronic structure or (high-energy density) plasma physics. This particular result outlines a future path for studies of ordered insulators heated to temperatures on the order of the band gap. Such experiments will offer strong tests of electronic strucure theory, implementing a scientific approach that sees measurement of real-space charge density via x-ray diffraction (XRD) as a particularly effectve means to constrain density functional theory (DFT)-based modeling of the solid state/plasma transitional regime.

Pushing x-ray photon correlation spectroscopy beyond the continuous frame rate limit

DOE PAGES

Dufresne, Eric M.; Narayanan, Suresh; Sandy, Alec R.; ...

2016-01-06

We demonstrate delayed-frame X-ray Photon Correlation Spectroscopy with 120 microsecond time resolution, limited only by sample scattering rates, with a prototype Pixel-array detector capable of taking two image frames separated by 153 ns or less. Although the overall frame rate is currently limited to about 4 frame pairs per second, we easily measured millisecond correlation functions. In conclusion, this technology, coupled to the use of brighter synchrotrons such as Petra III or the NSLS-II should enable X-ray Photon Correlation Spectroscopy on microsecond time scales on a wider variety of materials.

Quick-scanning x-ray absorption spectroscopy system with a servo-motor-driven channel-cut monochromator with a temporal resolution of 10 ms.

PubMed

Nonaka, T; Dohmae, K; Araki, T; Hayashi, Y; Hirose, Y; Uruga, T; Yamazaki, H; Mochizuki, T; Tanida, H; Goto, S

2012-08-01

We have developed a quick-scanning x-ray absorption fine structure (QXAFS) system and installed it at the recently constructed synchrotron radiation beamline BL33XU at the SPring-8. Rapid acquisition of high-quality QXAFS data was realized by combining a servo-motor-driven Si channel-cut monochromator with a tapered undulator. Two tandemly aligned monochromators with channel-cut Si(111) and Si(220) crystals covered energy ranges of 4.0-28.2 keV and 6.6-46.0 keV, respectively. The system allows the users to adjust instantly the energy ranges of scans, the starting angles of oscillations, and the frequencies. The channel-cut crystals are cooled with liquid nitrogen to enable them to withstand the high heat load from the undulator radiation. Deformation of the reflecting planes is reduced by clamping each crystal with two cooling blocks. Performance tests at the Cu K-edge demonstrated sufficiently high data quality for x-ray absorption near-edge structure and extended x-ray absorption fine-structure analyses with temporal resolutions of up to 10 and 25 ms, respectively.

High-order multilayer coated blazed gratings for high resolution soft x-ray spectroscopy

DOE PAGES

Voronov, Dmitriy L.; Goray, Leonid I.; Warwick, Tony; ...

2015-02-17

A grand challenge in soft x-ray spectroscopy is to drive the resolving power of monochromators and spectrometers from the 10 4 achieved routinely today to well above 10 5. This need is driven mainly by the requirements of a new technique that is set to have enormous impact in condensed matter physics, Resonant Inelastic X-ray Scattering (RIXS). Unlike x-ray absorption spectroscopy, RIXS is not limited by an energy resolution dictated by the core-hole lifetime in the excitation process. Using much higher resolving power than used for normal x-ray absorption spectroscopy enables access to the energy scale of soft excitations inmore » matter. These excitations such as magnons and phonons drive the collective phenomena seen in correlated electronic materials such as high temperature superconductors. RIXS opens a new path to study these excitations at a level of detail not formerly possible. However, as the process involves resonant excitation at an energy of around 1 keV, and the energy scale of the excitations one would like to see are at the meV level, to fully utilize the technique requires the development of monochromators and spectrometers with one to two orders of magnitude higher energy resolution than has been conventionally possible. Here we investigate the detailed diffraction characteristics of multilayer blazed gratings. These elements offer potentially revolutionary performance as the dispersive element in ultra-high resolution x-ray spectroscopy. In doing so, we have established a roadmap for the complete optimization of the grating design. Traditionally 1st order gratings are used in the soft x-ray region, but we show that as in the optical domain, one can work in very high spectral orders and thus dramatically improve resolution without significant loss in efficiency.« less

Calcium in the Oxygen-Evolving Complex: Structural and Mechanistic Role Determined by X-ray Spectroscopy

PubMed Central

Yachandra, Vittal K.; Yano, Junko

2011-01-01

This review describes the results from X-ray absorption spectroscopy studies that have contributed to an understanding of the role of Ca in the photosynthetic water oxidation reaction. The results include the first Mn, Ca and Sr X-ray spectroscopy studies using Ca or Sr-substituted PS II samples that established the presence of a MnCa heteronuclear structure and its orientation, and the most recent Sr X-ray spectroscopy study using biosynthetically prepared Sr-containing PS II in the various S-states that provide important insights into the requirement for Ca in the mechanism of the Mn4Ca catalytic center. PMID:21524917

Characterizing automotive fuel cell materials by soft x-ray scanning transmission x-ray microscopy

NASA Astrophysics Data System (ADS)

Hitchcock, A. P.; Lee, V.; Wu, J.; West, M. M.; Cooper, G.; Berejnov, V.; Soboleva, T.; Susac, D.; Stumper, J.

2016-01-01

Proton-Exchange Membrane Fuel Cell (PEM-FC) based engines are being developed rapidly for near-term implementation in hydrogen fueled, mass production, personal automobiles. Research is focused on understanding and controlling various degradation processes (carbon corrosion, Pt migration, cold start), and reducing cost by reducing or eliminating Pt catalyst. We are using soft X-ray scanning transmission X-ray microscopy (STXM) at the S 2p, C 1s, O 1s and F 1s edges to study a variety of issues related to optimization of PEM-FC materials for automotive applications. A method to efficiently and accurately measure perfluorosulfonic acid distributions was developed and is being used to better understand how different loadings and preparation methods affect the ionomer distribution in the cathode. Progress towards an environmental cell capable of controlling the temperature and humidity of a PEM-FC sample in the STXM is described. Methods for studying the 3D chemical structure of PEM-FC are outlined.

Characterizing automotive fuel cell materials by soft x-ray scanning transmission x-ray microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hitchcock, A. P., E-mail: aph@mcmaster.ca; Lee, V.; Wu, J.

Proton-Exchange Membrane Fuel Cell (PEM-FC) based engines are being developed rapidly for near-term implementation in hydrogen fueled, mass production, personal automobiles. Research is focused on understanding and controlling various degradation processes (carbon corrosion, Pt migration, cold start), and reducing cost by reducing or eliminating Pt catalyst. We are using soft X-ray scanning transmission X-ray microscopy (STXM) at the S 2p, C 1s, O 1s and F 1s edges to study a variety of issues related to optimization of PEM-FC materials for automotive applications. A method to efficiently and accurately measure perfluorosulfonic acid distributions was developed and is being used tomore » better understand how different loadings and preparation methods affect the ionomer distribution in the cathode. Progress towards an environmental cell capable of controlling the temperature and humidity of a PEM-FC sample in the STXM is described. Methods for studying the 3D chemical structure of PEM-FC are outlined.« less

Stochastic stimulated electronic x-ray Raman spectroscopy

PubMed Central

Kimberg, Victor; Rohringer, Nina

2016-01-01

Resonant inelastic x-ray scattering (RIXS) is a well-established tool for studying electronic, nuclear, and collective dynamics of excited atoms, molecules, and solids. An extension of this powerful method to a time-resolved probe technique at x-ray free electron lasers (XFELs) to ultimately unravel ultrafast chemical and structural changes on a femtosecond time scale is often challenging, due to the small signal rate in conventional implementations at XFELs that rely on the usage of a monochromator setup to select a small frequency band of the broadband, spectrally incoherent XFEL radiation. Here, we suggest an alternative approach, based on stochastic spectroscopy, which uses the full bandwidth of the incoming XFEL pulses. Our proposed method is relying on stimulated resonant inelastic x-ray scattering, where in addition to a pump pulse that resonantly excites the system a probe pulse on a specific electronic inelastic transition is provided, which serves as a seed in the stimulated scattering process. The limited spectral coherence of the XFEL radiation defines the energy resolution in this process and stimulated RIXS spectra of high resolution can be obtained by covariance analysis of the transmitted spectra. We present a detailed feasibility study and predict signal strengths for realistic XFEL parameters for the CO molecule resonantly pumped at the O1s→π* transition. Our theoretical model describes the evolution of the spectral and temporal characteristics of the transmitted x-ray radiation, by solving the equation of motion for the electronic and vibrational degrees of freedom of the system self consistently with the propagation by Maxwell equations. PMID:26958585

Structure of the manganese complex in photosystem II: insights from X-ray spectroscopy.

PubMed Central

Yachandra, Vittal K

2002-01-01

We have used Mn K-edge absorption and Kbeta emission spectroscopy to determine the oxidation states of the Mn complex in the various S states. We have started exploring the new technique of resonant inelastic X-ray scattering spectroscopy; this technique can be characterized as a Raman process that uses K-edge energies (1s to 4p, ca. 6550 eV) to obtain L-edge-like spectra (2p to 3d, ca. 650 eV). The relevance of these data to the oxidation states and structure of the Mn complex is presented. We have obtained extended X-ray absorption fine structure data from the S(0) and S(3) states and observed heterogeneity in the Mn-Mn distances leading us to conclude that there may be three rather than two di-mu-oxo-bridged units present per tetranuclear Mn cluster. In addition, we have obtained data using Ca and Sr X-ray spectroscopy that provide evidence for a heteronuclear Mn-Ca cluster. The possibility of three di-mu-oxo-bridged Mn-Mn moieties and the proximity of Ca is incorporated into developing structural models for the Mn cluster. The involvement of bridging and terminal O ligands of Mn in the mechanism of oxygen evolution is discussed in the context of our X-ray spectroscopy results. PMID:12437873

Excited state X-ray absorption spectroscopy: Probing both electronic and structural dynamics

NASA Astrophysics Data System (ADS)

Neville, Simon P.; Averbukh, Vitali; Ruberti, Marco; Yun, Renjie; Patchkovskii, Serguei; Chergui, Majed; Stolow, Albert; Schuurman, Michael S.

2016-10-01

We investigate the sensitivity of X-ray absorption spectra, simulated using a general method, to properties of molecular excited states. Recently, Averbukh and co-workers [M. Ruberti et al., J. Chem. Phys. 140, 184107 (2014)] introduced an efficient and accurate L 2 method for the calculation of excited state valence photoionization cross-sections based on the application of Stieltjes imaging to the Lanczos pseudo-spectrum of the algebraic diagrammatic construction (ADC) representation of the electronic Hamiltonian. In this paper, we report an extension of this method to the calculation of excited state core photoionization cross-sections. We demonstrate that, at the ADC(2)x level of theory, ground state X-ray absorption spectra may be accurately reproduced, validating the method. Significantly, the calculated X-ray absorption spectra of the excited states are found to be sensitive to both geometric distortions (structural dynamics) and the electronic character (electronic dynamics) of the initial state, suggesting that core excitation spectroscopies will be useful probes of excited state non-adiabatic dynamics. We anticipate that the method presented here can be combined with ab initio molecular dynamics calculations to simulate the time-resolved X-ray spectroscopy of excited state molecular wavepacket dynamics.

Rolf Mewe: a career devoted to X-ray spectroscopy

NASA Astrophysics Data System (ADS)

Kaastra, Jelle S.; Mewe, Rolf

2005-06-01

An overview of the life and work of Rolf Mewe (1935-2004) as an X-ray spectroscopist is given. He was one of the pioneers in the field of X-ray spectroscopy. His work illustrates nicely how this field developed from the early days up to the present high-resolution era. His plasma emission codes, developed by him and collaborators over several decades, is one of the most widely used. His thorough knowledge of the field, as well as his ability and enthousiasm to cooperate with many colleagues, made his career a succes. He will be missed by all of us for his work and personality.

Photochemically Generated Thiyl Free Radicals Observed by X-ray Absorption Spectroscopy

DOE PAGES

Sneeden, Eileen Y.; Hackett, Mark J.; Cotelesage, Julien J. H.; ...

2017-07-27

Sulfur-based thiyl radicals are known to be involved in a wide range of chemical and biological processes, but they are often highly reactive, which makes them difficult to observe directly. We report herein X-ray absorption spectra and analysis that support the direct observation of two different thiyl species generated photochemically by X-ray irradiation. The thiyl radical sulfur K-edge X-ray absorption spectra of both species are characterized by a uniquely low energy transition at about 2465 eV, which occurs at a lower energy than any previously observed feature at the sulfur K-edge and corresponds to a 1s → 3p transition tomore » the singly occupied molecular orbital of the free radical. In conclusion, our results constitute the first observation of substantial levels of thiyl radicals generated by X-ray irradiation and detected by sulfur K-edge X-ray absorption spectroscopy.« less

Synchrotron-based ambient pressure X-ray photoelectron spectroscopy of hydrogen and helium

NASA Astrophysics Data System (ADS)

Zhong, Jian-Qiang; Wang, Mengen; Hoffmann, William H.; van Spronsen, Matthijs A.; Lu, Deyu; Boscoboinik, J. Anibal

2018-02-01

Contrary to popular belief, it is possible to obtain X-ray photoelectron spectra for elements lighter than lithium, namely hydrogen and helium. The literature is plagued with claims of this impossibility, which holds true for lab-based X-ray sources. However, this limitation is merely technical and is related mostly to the low X-ray photoionization cross-sections of the 1s orbitals of hydrogen and helium. In this letter, we show that, using ambient pressure X-ray photoelectron spectroscopy (XPS), a bright-enough X-ray source allows the study of these elusive elements. This has important implications in the understanding of the limitations of one of the most useful techniques in materials science, and moreover, it potentially opens the possibility of using XPS to directly study the most abundant element in the universe.

A Broadband X-Ray Imaging Spectroscopy with High-Angular Resolution: the FORCE Mission

NASA Technical Reports Server (NTRS)

Mori, Koji; Tsuru, Takeshi Go; Nakazawac, Kazuhiro; Ueda, Yoshihiro; Okajima, Takashi; Murakami, Hiroshi; Awaki, Hisamitsu; Matsumoto, Hironori; Fukazawai, Yasushi; Tsunemi, Hiroshi;

An alignment method for mammographic X-ray spectroscopy under clinical conditions.

PubMed

Miyajima, S; Imagawa, K; Matsumoto, M

2002-09-01

This paper describes an alignment method for mammographic X-ray spectroscopy under clinical conditions. A pinhole, a fluorescent screen, a laser device and the case for a detector are used for alignment of the focal spot, a collimator and a detector. The method determines the line between the focal spot and the point of interest in an X-ray field radiographically. The method allows alignment for both central axis and off-axis directions.

Reaction of Hydroquinone with Hematite I. Study of Adsorption by Electrochemical-Scanning Tunneling Microscopy and X-ray Photoelectron Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stack, Andrew G; Eggleston, Carrick M; Engelhard, Mark H

2004-06-15

The reaction of hematite with quinones and the quinone moieties of larger molecules may be an important factor in limiting the rate ofreductive dissolution, especially by iron-reducing bacteria. Here, the electrochemical and physical properties of hydroquinone adsorbed on hematite surfaces at pH 2.5–3 were investigated with cyclic voltammetry (CV), electrochemical-scanning tunneling microscopy (EC-STM), and X-ray photoelectron spectroscopy (XPS). An oxidation peak for hydroquinone was observed in the CV experiments, as well as (photo)reduction of iron and decomposition of the solvent. The EC-STM results indicate that hydroquinone sometimes forms an ordered monolayer with ~1.1 H₂/nm², but can be fairly disordered (especiallymore » when viewed at larger scales). XPS results indicate that hydroquinone and benzoquinone are retained at the interface in increasing amounts as the reaction proceeds, but reduced iron is not observed. These results suggest that quinones do not adsorb by an inner-sphere complex where adsorbate–surface interactions determine the adsorbate surface structure, but rather in an outer-sphere complex where interactions among the adsorbate molecules dominate.« less

Reaction of hydroquinone with hematite I. Study of asdsorption by electrochemical-scanning tunneling microscopy and X-ray photoelectron spectroscopy.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stack, Andrew G; Eggleston, Carrick M; Engelhard, Mark H

2003-12-01

The reaction of hematite with quinones and the quinone moieties of larger molecules may be an important factor in limiting the rate of reductive dissolution, especially by iron-reducing bacteria. Here, the electrochemical and physical properties of hydroquinone adsorbed on hematite surfaces at pH 2.5-3 were investigated with cyclic voltammetry (CV), electrochemical-scanning tunneling microscopy (EC-STM), and X-ray photoelectron spectroscopy (XPS). An oxidation peak for hydroquinone was observed in the CV experiments, as well as (photo)reduction of iron and decomposition of the solvent. The EC-STM results indicate that hydroquinone sometimes forms an ordered monolayer with {approx}1.1 QH{sub 2}/nm{sup 2}, but can bemore » fairly disordered (especially when viewed at larger scales). XPS results indicate that hydroquinone and benzoquinone are retained at the interface in increasing amounts as the reaction proceeds, but reduced iron is not observed. These results suggest that quinones do not adsorb by an inner-sphere complex where adsorbate-surface interactions determine the adsorbate surface structure, but rather in an outer-sphere complex where interactions among the adsorbate molecules dominate.« less

Status of the Nanoscopium Scanning Hard X-ray Nanoprobe Beamline of Synchrotron Soleil

NASA Astrophysics Data System (ADS)

Somogyi, A.; Kewish, C. M.; Ribbens, M.; Moreno, T.; Polack, F.; Baranton, G.; Desjardins, K.; Samama, J. P.

2013-10-01

The Nanoscopium 155 m-long scanning hard X-ray nanoprobe beamline of Synchrotron Soleil (St Aubin, France) is dedicated to quantitative multi-modal 2D/3D imaging. The beamline aims to reach down to 30 nm spatial resolution in the 5-20 keV energy range. Two experimental stations working in consecutive operation mode will be dedicated to coherent diffractive imaging and scanning X-ray nanoprobe techniques. The beamline is in the construction phase, the first user experiments are expected in 2014. The main characteristics of the beamline and an overview of its status are given in this paper.

Scanning electron and atomic force microscopy, and raman and x-ray photoelectron spectroscopy characterization of near-isogenic soft and hard wheat kernels and corresponding flours

USDA-ARS?s Scientific Manuscript database

Atomic force microscopy (AFM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) are used to investigate vitreous (hard) and non-vitreous (soft) wheat kernels and their corresponding wheat flours. AFM data reveal two different microstructures. The vitreous kernel reveals a granular text...

Development of fast parallel multi-technique scanning X-ray imaging at Synchrotron Soleil

NASA Astrophysics Data System (ADS)

Medjoubi, K.; Leclercq, N.; Langlois, F.; Buteau, A.; Lé, S.; Poirier, S.; Mercère, P.; Kewish, C. M.; Somogyi, A.

2013-10-01

A fast multimodal scanning X-ray imaging scheme is prototyped at Soleil Synchrotron. It permits the simultaneous acquisition of complementary information on the sample structure, composition and chemistry by measuring transmission, differential phase contrast, small-angle scattering, and X-ray fluorescence by dedicated detectors with ms dwell time per pixel. The results of the proof of principle experiments are presented in this paper.

Detector, collimator and real-time reconstructor for a new scanning-beam digital x-ray (SBDX) prototype.

PubMed

Speidel, Michael A; Tomkowiak, Michael T; Raval, Amish N; Dunkerley, David A P; Slagowski, Jordan M; Kahn, Paul; Ku, Jamie; Funk, Tobias

Scanning-beam digital x-ray (SBDX) is an inverse geometry fluoroscopy system for low dose cardiac imaging. The use of a narrow scanned x-ray beam in SBDX reduces detected x-ray scatter and improves dose efficiency, however the tight beam collimation also limits the maximum achievable x-ray fluence. To increase the fluence available for imaging, we have constructed a new SBDX prototype with a wider x-ray beam, larger-area detector, and new real-time image reconstructor. Imaging is performed with a scanning source that generates 40,328 narrow overlapping projections from 71 × 71 focal spot positions for every 1/15 s scan period. A high speed 2-mm thick CdTe photon counting detector was constructed with 320×160 elements and 10.6 cm × 5.3 cm area (full readout every 1.28 μs), providing an 86% increase in area over the previous SBDX prototype. A matching multihole collimator was fabricated from layers of tungsten, brass, and lead, and a multi-GPU reconstructor was assembled to reconstruct the stream of captured detector images into full field-of-view images in real time. Thirty-two tomosynthetic planes spaced by 5 mm plus a multiplane composite image are produced for each scan frame. Noise equivalent quanta on the new SBDX prototype measured 63%-71% higher than the previous prototype. X-ray scatter fraction was 3.9-7.8% when imaging 23.3-32.6 cm acrylic phantoms, versus 2.3-4.2% with the previous prototype. Coronary angiographic imaging at 15 frame/s was successfully performed on the new SBDX prototype, with live display of either a multiplane composite or single plane image.

Synchrotron-based ambient pressure X-ray photoelectron spectroscopy of hydrogen and helium

DOE PAGES

Zhong, Jian-Qiang; Wang, Mengen; Hoffmann, William H.; ...

2018-03-01

Contrary to popular belief, it is possible to obtain X-ray photoelectron spectra for elements lighter than lithium, namely hydrogen and helium. The literature is plagued with claims of this impossibility, which holds true for lab-based X-ray sources. However, this limitation is merely technical and is related mostly to the low X-ray photoionization cross-sections of the 1s orbitals of hydrogen and helium. Here, we show that, using ambient pressure X-ray photoelectron spectroscopy (XPS), a bright-enough X-ray source allows the study of these elusive elements. This has important implications in the understanding of the limitations of one of the most useful techniquesmore » in materials science, and moreover, it potentially opens the possibility of using XPS to directly study the most abundant element in the universe.« less

Synchrotron-based ambient pressure X-ray photoelectron spectroscopy of hydrogen and helium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhong, Jian-Qiang; Wang, Mengen; Hoffmann, William H.

Contrary to popular belief, it is possible to obtain X-ray photoelectron spectra for elements lighter than lithium, namely hydrogen and helium. The literature is plagued with claims of this impossibility, which holds true for lab-based X-ray sources. However, this limitation is merely technical and is related mostly to the low X-ray photoionization cross-sections of the 1s orbitals of hydrogen and helium. Here, we show that, using ambient pressure X-ray photoelectron spectroscopy (XPS), a bright-enough X-ray source allows the study of these elusive elements. This has important implications in the understanding of the limitations of one of the most useful techniquesmore » in materials science, and moreover, it potentially opens the possibility of using XPS to directly study the most abundant element in the universe.« less

Catalysts at work: From integral to spatially resolved X-ray absorption spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Grunwaldt, Jan-Dierk; Kimmerle, Bertram; Baiker, Alfons

2009-09-25

Spectroscopic studies on heterogeneous catalysts have mostly been done in an integral mode. However, in many cases spatial variations in catalyst structure can occur, e.g. during impregnation of pre-shaped particles, during reaction in a catalytic reactor, or in microstructured reactors as the present overview shows. Therefore, spatially resolved molecular information on a microscale is required for a comprehensive understanding of theses systems, partly in ex situ studies, partly under stationary reaction conditions and in some cases even under dynamic reaction conditions. Among the different available techniques, X-ray absorption spectroscopy (XAS) is a well-suited tool for this purpose as the differentmore » selected examples highlight. Two different techniques, scanning and full-field X-ray microscopy/tomography, are described and compared. At first, the tomographic structure of impregnated alumina pellets is presented using full-field transmission microtomography and compared to the results obtained with a scanning X-ray microbeam technique to analyse the catalyst bed inside a catalytic quartz glass reactor. On the other hand, by using XAS in scanning microtomography, the structure and the distribution of Cu(0), Cu(I), Cu(II) species in a Cu/ZnO catalyst loaded in a quartz capillary microreactor could be reconstructed quantitatively on a virtual section through the reactor. An illustrating example for spatially resolved XAS under reaction conditions is the partial oxidation of methane over noble metal-based catalysts. In order to obtain spectroscopic information on the spatial variation of the oxidation state of the catalyst inside the reactor XAS spectra were recorded by scanning with a micro-focussed beam along the catalyst bed. Alternatively, full-field transmission imaging was used to efficiently determine the distribution of the oxidation state of a catalyst inside a reactor under reaction conditions. The new technical approaches together with

A broadband x-ray imaging spectroscopy with high-angular resolution: the FORCE mission

NASA Astrophysics Data System (ADS)

Mori, Koji; Tsuru, Takeshi Go; Nakazawa, Kazuhiro; Ueda, Yoshihiro; Okajima, Takashi; Murakami, Hiroshi; Awaki, Hisamitsu; Matsumoto, Hironori; Fukazawa, Yasushi; Tsunemi, Hiroshi; Takahashi, Tadayuki; Zhang, William W.

2016-07-01

We are proposing FORCE (Focusing On Relativistic universe and Cosmic Evolution) as a future Japan-lead Xray observatory to be launched in the mid 2020s. Hitomi (ASTRO-H) possesses a suite of sensitive instruments enabling the highest energy-resolution spectroscopy in soft X-ray band, a broadband X-ray imaging spectroscopy in soft and hard X-ray bands, and further high energy coverage up to soft gamma-ray band. FORCE is the direct successor to the broadband X-ray imaging spectroscopy aspect of Hitomi (ASTRO-H) with significantly higher angular resolution. The current design of FORCE defines energy band pass of 1-80 keV with angular resolution of < 15 in half-power diameter, achieving a 10 times higher sensitivity above 10 keV compared to any previous missions with simultaneous soft X-ray coverage. Our primary scientific objective is to trace the cosmic formation history by searching for "missing black holes" in various mass-scales: "buried supermassive black holes (SMBHs)" (> 104 M⊙) residing in the center of galaxies in a cosmological distance, "intermediate-mass black holes" (102-104 M⊙) acting as the possible seeds from which SMBHs grow, and "orphan stellar-mass black holes" (< 102 M⊙) without companion in our Galaxy. In addition to these missing BHs, hunting for the nature of relativistic particles at various astrophysical shocks is also in our scope, utilizing the broadband X-ray coverage with high angular-resolution. FORCE are going to open a new era in these fields. The satellite is proposed to be launched with the Epsilon vehicle that is a Japanese current solid-fuel rocket. FORCE carries three identical pairs of Super-mirror and wide-band X-ray detector. The focal length is currently planned to be 10 m. The silicon mirror with multi-layer coating is our primary choice to achieve lightweight, good angular optics. The detector is a descendant of hard X-ray imager onboard Hitomi (ASTRO-H) replacing its silicon strip detector with SOI-CMOS silicon pixel

Dark-field imaging with the scanning transmission x-ray microscope

NASA Astrophysics Data System (ADS)

Morrison, G. R.; Browne, M. T.

1992-01-01

The King's College London scanning transmission x-ray microscope in use on beam line 5U2 at the SRS, SERC Daresbury Laboratory, has been modified to allow dark-field images to be formed using only the x rays scattered by the specimen. Experiments have been performed with a number of different detector geometries, and this has confirmed that the strongest scattering arises from edges or thickness gradients in the specimen. Although the dark-field signal is only a small fraction of the normal transmitted bright-field signal, features can be revealed with high contrast, and it has proved possible to detect the presence of features that are below the resolution limit of the microscope.

Simultaneous scanning tunneling microscopy and synchrotron X-ray measurements in a gas environment.

PubMed

Mom, Rik V; Onderwaater, Willem G; Rost, Marcel J; Jankowski, Maciej; Wenzel, Sabine; Jacobse, Leon; Alkemade, Paul F A; Vandalon, Vincent; van Spronsen, Matthijs A; van Weeren, Matthijs; Crama, Bert; van der Tuijn, Peter; Felici, Roberto; Kessels, Wilhelmus M M; Carlà, Francesco; Frenken, Joost W M; Groot, Irene M N

2017-11-01

A combined X-ray and scanning tunneling microscopy (STM) instrument is presented that enables the local detection of X-ray absorption on surfaces in a gas environment. To suppress the collection of ion currents generated in the gas phase, coaxially shielded STM tips were used. The conductive outer shield of the coaxial tips can be biased to deflect ions away from the tip core. When tunneling, the X-ray-induced current is separated from the regular, 'topographic' tunneling current using a novel high-speed separation scheme. We demonstrate the capabilities of the instrument by measuring the local X-ray-induced current on Au(1 1 1) in 800 mbar Ar. Copyright © 2017 Elsevier B.V. All rights reserved.

Low-energy d-d excitations in MnO studied by resonant x-ray fluorescence spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Butorin, S.M.; Guo, J.; Magnuson, M.

1997-04-01

Resonant soft X-ray emission spectroscopy has been demonstrated to possess interesting abilities for studies of electronic structure in various systems, such as symmetry probing, alignment and polarization dependence, sensitivity to channel interference, etc. In the present abstract the authors focus on the feasibility of resonant soft X-ray emission to probe low energy excitations by means of resonant electronic X-ray Raman scattering. Resonant X-ray emission can be regarded as an inelastic scattering process where a system in the ground state is transferred to a low excited state via a virtual core excitation. The energy closeness to a core excitation of themore » exciting radiation enhances the (generally) low probability for inelastic scattering at these wavelengths. Therefore soft X-ray emission spectroscopy (in resonant electronic Raman mode) can be used to study low energy d-d excitations in transition metal systems. The involvement of the intermediate core state allows one to use the selection rules of X-ray emission, and the appearance of the elastically scattered line in the spectra provides the reference to the ground state.« less

X-ray Spectroscopy and Magnetism in Mineralogy

NASA Astrophysics Data System (ADS)

Sainctavit, Philippe; Brice-Profeta, Sandrine; Gaudry, Emilie; Letard, Isabelle; Arrio, Marie-Anne

The objective of this paper is to present the kind of information that can be gained in the field of mineralogy from the use of x-ray magnetic spectroscopies. We review some of the questions that are unsettled and that could benefit from an interdisciplinary approach where magnetism, spectroscopy and mineralogy could be mixed. Most of the attention is focused on iron and some other 3d transition elements. The mineralogy of planetary cores and its relation with known meteorites are exemplified. The various oxide phases in the mantle and the nature of iron in these phases is also underlined. The presence of transition elements in insulating minerals and its relation with macroscopic properties such as the color of gemstones are reviewed. Finally an introduction to paleomagnetism is given with a special attention to nanomaghemites.

Infrared x-ray pump-probe spectroscopy of the NO molecule

NASA Astrophysics Data System (ADS)

Guimarães, F. F.; Kimberg, V.; Felicíssimo, V. C.; Gel'Mukhanov, F.; Cesar, A.; Ågren, H.

2005-07-01

Two color infrared x-ray pump-probe spectroscopy of the NO molecule is studied theoretically and numerically in order to obtain a deeper insight of the underlying physics and of the potential of this suggested technology. From the theoretical investigation a number of conclusions could be drawn: It is found that the phase of the infrared field strongly influences the trajectory of the nuclear wave packet, and hence, the x-ray spectrum. The trajectory experiences fast oscillations with the vibrational frequency with a modulation due to the anharmonicity of the potential. The dependences of the x-ray spectra on the delay time, the duration, and the shape of the pulses are studied in detail. It is shown that the x-ray spectrum keep memory about the infrared phase after the pump field left the system. This memory effect is sensitive to the time of switching-off the pump field and the Rabi frequency. The phase effect takes maximum value when the duration of the x-ray pulse is one-fourth of the infrared field period, and can be enhanced by a proper control of the duration and intensity of the pump pulse. The manifestation of the phase is different for oriented and disordered molecules and depends strongly on the intensity of the pump radiation.

King's College London/SERC Daresbury Scanning X-ray Microscope

NASA Astrophysics Data System (ADS)

Burge, R. E.; Browne, M. T.; Buckley, C. J.; Cave, R.; Charalambous, P.; Duke, P. J.; Freake, A. J.; Hare, A.; Hills, C. P. B.; Kenney, J. M.; Kuriyama, T.; Lidiard, D.; MacDowell, A.; Michette, A. G.; Morrison, G. R.; Ogawa, K.; Rogoyski, A. M.

1986-01-01

The present status of the soft X-ray microscope is described and a short description is given, with likely development paths for the future, of the Daresbury synchrotron source, the monochromator, the high-resolution zone-plates, the scanning specimen stage, image recording and methods of image enhancement. It is considered that the instrumental developments needed for images at 10 nm resolution will take a further two or three years.

Solid state structural investigations of the bis(chalcone) compound with single crystal X-ray crystallography, DFT, gamma-ray spectroscopy and chemical spectroscopy methods

NASA Astrophysics Data System (ADS)

Yakalı, Gül; Biçer, Abdullah; Eke, Canel; Cin, Günseli Turgut

2018-04-01

A bis(chalcone), (2E,6E)-2,6-bis((E)-3phenylallidene)cyclohexanone, was characterized by 1H NMR, 13C NMR, FTIR, UV-Vis spectroscopy, gamma-ray spectroscopy and single crystal X- ray structural analysis. The optimized molecular structure of the compound is calculated using DFT/B3LYP with 6-31G (d,p) level. The calculated geometrical parameters are in good agreement with the experimental data obtained from our reported X-ray structure. The powder and single crystal compounds were gama-irradiated using clinical electron linear accelerator and 60Co gamma-ray source, respectively. Spectral studies (1H NMR, 13C NMR, FTIR and UV-Vis) of powder chalcone compound were also investigated before and after irradiation. Depending on the irradiation notable changes were observed in spectral features powder sample. Single crystal X-ray diffraction investigation shows that both unirradiated and irradiated single crystal samples crystallizes in a orthorhombic crystal system in the centrosymmetric space group Pbcn and exhibits an C-H..O intramolecular and intermolecular hydrogen bonds. The crystal packing is stabilised by strong intermolecular bifurcate C-H..O hydrogen bonds and π…π stacking interactions. The asymmetric unit of the title compound contains one-half of a molecule. The other half of the molecule is generated with (1-x,y,-3/2-z) symmetry operator. The molecule is almost planar due to having π conjugated system of chalcones. However, irradiated single crystal compound showed significant changes lattice parameters, crystal volume and density. According to results of gamma-ray spectroscopy, radioactive elements of powder compound which are 123Sb(n,g),124Sb,57Fe(g,p),56Mn, 55Mn(g,n), and 54Mn were determined using photoactivation analysis. However, the most intensive gamma-ray energy signals are 124Sb.

A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Szlachetko, J.; Institute of Physics, Jan Kochanowski University, 25-406 Kielce; Nachtegaal, M.

2012-10-15

We report on the design and performance of a wavelength-dispersive type spectrometer based on the von Hamos geometry. The spectrometer is equipped with a segmented-type crystal for x-ray diffraction and provides an energy resolution in the order of 0.25 eV and 1 eV over an energy range of 8000 eV-9600 eV. The use of a segmented crystal results in a simple and straightforward crystal preparation that allows to preserve the spectrometer resolution and spectrometer efficiency. Application of the spectrometer for time-resolved resonant inelastic x-ray scattering and single-shot x-ray emission spectroscopy is demonstrated.

Tenth International Colloquium on UV and X-Ray Spectroscopy of Astrophysical and Laboratory Plasmas

NASA Astrophysics Data System (ADS)

Silver, Eric H.; Kahn, Steven M.

UV and X-ray spectroscopy of astrophysical and laboratory plasmas draws interest from many disciplines. Contributions from international specialists are collected together in this book from a timely recent conference. In astrophysics, the Hubble Space Telescope, Astro 1 and ROSAT observatories are now providing UV and X-ray spectra and images of cosmic sources in unprecedented detail, while the Yohkoh mission recently collected superb data on the solar corona. In the laboratory, the development of ion-trap facilities and novel laser experiments are providing vital new data on high temperature plasmas. Recent innovations in the technology of spectroscopic instrumentation are discussed. These papers constitute an excellent up-to-date review of developments in short-wavelength spectroscopy and offer a solid introduction to its theoretical and experimental foundations. These proceedings give an up-to-date review of developments in short-wavelength spectroscopy and offer a solid introduction to its theoretical and experimental foundations. Various speakers presented some of the first results from the high resolution spectrograph on the Hubble Space Telescope, the high sensitivity far ultraviolet and X-ray spectrometers of the ASTRO 1 Observatory, the imaging X-ray spectrometer on the ROSAT Observatory, and the high resolution solar X-ray spectrometer on Yohkoh. The development of ion trap devices had brought about a revolution in laboratory investigations of atomic processes in highly charged atoms. X-ray laser experiments had not only yielded considerable insight into electron ion interactions in hot dense plasmas, but also demonstrated the versatility of laser plasmas as laboratory X-ray sources. Such measurements also motivated and led to refinements in the development of large-scale atomic and molecular codes. On the instrumental side, the design and development of the next series of very powerful short wavelength observatories had generated a large number of

Chemical Modification of Graphene Oxide by Nitrogenation: An X-ray Absorption and Emission Spectroscopy Study

DOE PAGES

Chuang, Cheng-Hao; Ray, Sekhar C.; Mazumder, Debarati; ...

2017-02-10

Nitrogen-doped graphene oxides (GO:N x) were synthesized by a partial reduction of graphene oxide (GO) using urea [CO(NH 2) 2 ]. Their electronic/bonding structures were investigated using X-ray absorption near-edge structure (XANES), valence-band photoemission spectroscopy (VB-PES), X-ray emission spectroscopy (XES) and resonant inelastic X-ray scattering (RIXS). During GO:N x synthesis, different nitrogen-bonding species, such as pyrrolic/graphitic-nitrogen, were formed by replacing of oxygen-containing functional groups. At lower N-content (2.7 at%), pyrrolic-N, owing to surface and subsurface diffusion of C, N and NH is deduced from various X-ray spectroscopies. In contrast, at higher N-content (5.0 at%) graphitic nitrogen was formed in whichmore » each N-atom trigonally bonds to three distinct sp 2 -hybridized carbons with substitution of the N-atoms for C atoms in the graphite layer. Upon nitrogen substitution, the total density of state close to Fermi level is increased to raise the valence-band maximum, as revealed by VB-PES spectra, indicating an electron donation from nitrogen, molecular bonding C/N/O coordination or/and lattice structure reorganization in GO:N x . The well-ordered chemical environments induced by nitrogen dopant are revealed by XANES and RIXS measurements.« less

Deconvolving instrumental and intrinsic broadening in core-shell x-ray spectroscopies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fister, T. T.; Seidler, G. T.; Rehr, J. J.

2007-05-01

Intrinsic and experimental mechanisms frequently lead to broadening of spectral features in core-shell spectroscopies. For example, intrinsic broadening occurs in x-ray absorption spectroscopy (XAS) measurements of heavy elements where the core-hole lifetime is very short. On the other hand, nonresonant x-ray Raman scattering (XRS) and other energy loss measurements are more limited by instrumental resolution. Here, we demonstrate that the Richardson-Lucy (RL) iterative algorithm provides a robust method for deconvolving instrumental and intrinsic resolutions from typical XAS and XRS data. For the K-edge XAS of Ag, we find nearly complete removal of {approx}9.3 eV full width at half maximum broadeningmore » from the combined effects of the short core-hole lifetime and instrumental resolution. We are also able to remove nearly all instrumental broadening in an XRS measurement of diamond, with the resulting improved spectrum comparing favorably with prior soft x-ray XAS measurements. We present a practical methodology for implementing the RL algorithm in these problems, emphasizing the importance of testing for stability of the deconvolution process against noise amplification, perturbations in the initial spectra, and uncertainties in the core-hole lifetime.« less

Analysis of passivated A-286 stainless steel surfaces for mass spectrometer inlet systems by Auger electron and X-ray photoelectron spectroscopy and scanning electron microscopy

DOE PAGES

Ajo, Henry; Blankenship, Donnie; Clark, Elliot

2014-07-25

In this study, various commercially available surface treatments are being explored for use on stainless steel components in mass spectrometer inlet systems. Type A-286 stainless steel coupons, approximately 12.5 mm in diameter and 3 mm thick, were passivated with one of five different surface treatments; an untreated coupon served as a control. The surface and near-surface microstructure and chemistry of the coupons were investigated using sputter depth profiling using Auger electron spectroscopy, x-ray photoelectron spectroscopy, and scanning electron microscopy (SEM). All the surface treatments studied appeared to change the surface morphology dramatically, as evidenced by lack of tool marks onmore » the treated samples in SEM images. In terms of the passivation treatment, Vendors A-D appeared to have oxide layers that were very similar in thickness to each other (0.7–0.9 nm thick), as well as to the untreated samples (the untreated sample oxide layers appeared to be somewhat larger). Vendor E’s silicon coating appears to be on the order of 200 nm thick.« less

Application toward Confocal Full-Field Microscopic X-ray Absorption Near Edge Structure Spectroscopy.

PubMed

Tack, Pieter; Vekemans, Bart; Laforce, Brecht; Rudloff-Grund, Jennifer; Hernández, Willinton Y; Garrevoet, Jan; Falkenberg, Gerald; Brenker, Frank; Van Der Voort, Pascal; Vincze, Laszlo

2017-02-07

Using X-ray absorption near edge structure (XANES) spectroscopy, information on the local chemical structure and oxidation state of an element of interest can be acquired. Conventionally, this information can be obtained in a spatially resolved manner by scanning a sample through a focused X-ray beam. Recently, full-field methods have been developed to obtain direct 2D chemical state information by imaging a large sample area. These methods are usually in transmission mode, thus restricting the use to thin and transmitting samples. Here, a fluorescence method is displayed using an energy-dispersive pnCCD detector, the SLcam, characterized by measurement times far superior to what is generally applicable. Additionally, this method operates in confocal mode, thus providing direct 3D spatially resolved chemical state information from a selected subvolume of a sample, without the need of rotating a sample. The method is applied to two samples: a gold-supported magnesia catalyst (Au/MgO) and a natural diamond containing Fe-rich inclusions. Both samples provide XANES spectra that can be overlapped with reference XANES spectra, allowing this method to be used for fingerprinting and linear combination analysis of known XANES reference compounds.

PINPIN a-Si:H based structures for X-ray image detection using the laser scanning technique

NASA Astrophysics Data System (ADS)

Fernandes, M.; Vygranenko, Y.; Vieira, M.

2015-05-01

Conventional film based X-ray imaging systems are being replaced by their digital equivalents. Different approaches are being followed by considering direct or indirect conversion, with the later technique dominating. The typical, indirect conversion, X-ray panel detector uses a phosphor for X-ray conversion coupled to a large area array of amorphous silicon based optical sensors and a couple of switching thin film transistors (TFT). The pixel information can then be readout by switching the correspondent line and column transistors, routing the signal to an external amplifier. In this work we follow an alternative approach, where the electrical switching performed by the TFT is replaced by optical scanning using a low power laser beam and a sensing/switching PINPIN structure, thus resulting in a simpler device. The optically active device is a PINPIN array, sharing both front and back electrical contacts, deposited over a glass substrate. During X-ray exposure, each sensing side photodiode collects photons generated by the scintillator screen (560 nm), charging its internal capacitance. Subsequently a laser beam (445 nm) scans the switching diodes (back side) retrieving the stored charge in a sequential way, reconstructing the image. In this paper we present recent work on the optoelectronic characterization of the PINPIN structure to be incorporated in the X-ray image sensor. The results from the optoelectronic characterization of the device and the dependence on scanning beam parameters are presented and discussed. Preliminary results of line scans are also presented.

Development of a spectro-electrochemical cell for soft X-ray photon-in photon-out spectroscopy

NASA Astrophysics Data System (ADS)

Ishihara, Tomoko; Tokushima, Takashi; Horikawa, Yuka; Kato, Masaru; Yagi, Ichizo

2017-10-01

We developed a spectro-electrochemical cell for X-ray absorption and X-ray emission spectroscopy, which are element-specific methods to study local electronic structures in the soft X-ray region. In the usual electrochemical measurement setup, the electrode is placed in solution, and the surface/interface region of the electrode is not normally accessible by soft X-rays that have low penetration depth in liquids. To realize soft X-ray observation of electrochemical reactions, a 15-nm-thick Pt layer was deposited on a 150-nm-thick film window with an adhesive 3-nm-thick Ti layer for use as both the working electrode and the separator window between vacuum and a sample liquid under atmospheric pressure. The designed three-electrode electrochemical cell consists of a Pt film on a SiC window, a platinized Pt wire, and a commercial Ag|AgCl electrode as the working, counter, and reference electrodes, respectively. The functionality of the cell was tested by cyclic voltammetry and X-ray absorption and emission spectroscopy. As a demonstration, the electroplating of Pb on the Pt/SiC membrane window was measured by X-ray absorption and real-time monitoring of fluorescence intensity at the O 1s excitation.

Diffracting aperture based differential phase contrast for scanning X-ray microscopy.

PubMed

Kaulich, Burkhard; Polack, Francois; Neuhaeusler, Ulrich; Susini, Jean; di Fabrizio, Enzo; Wilhein, Thomas

2002-10-07

It is demonstrated that in a zone plate based scanning X-ray microscope, used to image low absorbing, heterogeneous matter at a mesoscopic scale, differential phase contrast (DPC) can be implemented without adding any additional optical component to the normal scheme of the microscope. The DPC mode is simply generated by an appropriate positioning and alignment of microscope apertures. Diffraction from the apertures produces a wave front with a non-uniform intensity. The signal recorded by a pinhole photo diode located in the intensity gradient is highly sensitive to phase changes introduced by the specimen to be recorded. The feasibility of this novel DPC technique was proven with the scanning X-ray microscope at the ID21 beamline of the European Synchrotron Radiation facility (ESRF) operated at 6 keV photon energy. We observe a differential phase contrast, similar to Nomarski's differential interference contrast for the light microscope, which results in a tremendous increase in image contrast of up to 20 % when imaging low absorbing specimen.

Oxidant K edge x-ray emission spectroscopy of UF 4 and UO 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tobin, J. G.; Yu, S. -W.; Qiao, R.

The K-Edge (1s) x-ray emission spectroscopy of uranium tetrafluoride and uranium dioxide were compared to each other and to the results of a pair of earlier cluster calculations. Here, using a very simplified approach, it is possible to qualitatively reconstruct the main features of the x-ray emission spectra from the cluster calculation state energies and 2p percentages.

Oxidant K edge x-ray emission spectroscopy of UF 4 and UO 2

DOE PAGES

Tobin, J. G.; Yu, S. -W.; Qiao, R.; ...

2018-01-31

The K-Edge (1s) x-ray emission spectroscopy of uranium tetrafluoride and uranium dioxide were compared to each other and to the results of a pair of earlier cluster calculations. Here, using a very simplified approach, it is possible to qualitatively reconstruct the main features of the x-ray emission spectra from the cluster calculation state energies and 2p percentages.

X-ray Photoelectron Spectroscopy study of CaV1-xMoxO3-δ

NASA Astrophysics Data System (ADS)

Belyakov, S. A.; Kuznetsov, M. V.; Shkerin, S. N.

2018-06-01

An investigation was carried out on perovskite-based derivatives of CaV1-xMoxO3-δ using X-ray Photoelectron Spectroscopy (XPS). According to the XRD pattern, the area of homogeneity covers the region from x = 0 to x = 0.6. Wide XPS-peaks of Ca, V, Mo and O are observed, signalling that elements are presented in multiple states. A model for explaining the large chemical shifts of XPS peaks due to different charging effects on different parts of the sample surface is proposed.

Overview of nanoscale NEXAFS performed with soft X-ray microscopes.

PubMed

Guttmann, Peter; Bittencourt, Carla

2015-01-01

Today, in material science nanoscale structures are becoming more and more important. Not only for the further miniaturization of semiconductor devices like carbon nanotube based transistors, but also for newly developed efficient energy storage devices, gas sensors or catalytic systems nanoscale and functionalized materials have to be analysed. Therefore, analytical tools like near-edge X-ray absorption fine structure (NEXAFS) spectroscopy has to be applied on single nanostructures. Scanning transmission X-ray microscopes (STXM) as well as full-field transmission X-ray microscopes (TXM) allow the required spatial resolution to study individual nanostructures. In the soft X-ray energy range only STXM was used so far for NEXAFS studies. Due to its unique setup, the TXM operated by the Helmholtz-Zentrum Berlin (HZB) at the electron storage ring BESSY II is the first one in the soft X-ray range which can be used for NEXAFS spectroscopy studies which will be shown in this review. Here we will give an overview of the different microscopes used for NEXAFS studies and describe their advantages and disadvantages for different samples.

Crystallographic Characterization of Extraterrestrial Materials by Energy-Scanning X-ray Diffraction

NASA Technical Reports Server (NTRS)

Hagiya, Kenji; Mikouchi, Takashi; Ohsumi, Kazumasa; Terada, Yasuko; Yagi, Naoto; Komatsu, Mutsumi; Yamaguchi, Shoki; Hirata, Arashi; Kurokawa, Ayaka; Zolensky, Michael E. (Principal Investigator)

2016-01-01

We have continued our long-term project using X-ray diffraction to characterize a wide range of extraterrestrial samples. The stationary sample method with polychromatic X-rays is advantageous because the irradiated area of the sample is always same and fixed, meaning that all diffraction spots occur from the same area of the sample, however, unit cell parameters cannot be directly obtained by this method though they are very important for identification of mineral and for determination of crystal structures. In order to obtain the cell parameters even in the case of the sample stationary method, we apply energy scanning of a micro-beam of monochromatic SR at SPring-8.

Retrieving the Quantitative Chemical Information at Nanoscale from Scanning Electron Microscope Energy Dispersive X-ray Measurements by Machine Learning

NASA Astrophysics Data System (ADS)

Jany, B. R.; Janas, A.; Krok, F.

2017-11-01

The quantitative composition of metal alloy nanowires on InSb(001) semiconductor surface and gold nanostructures on germanium surface is determined by blind source separation (BSS) machine learning (ML) method using non negative matrix factorization (NMF) from energy dispersive X-ray spectroscopy (EDX) spectrum image maps measured in a scanning electron microscope (SEM). The BSS method blindly decomposes the collected EDX spectrum image into three source components, which correspond directly to the X-ray signals coming from the supported metal nanostructures, bulk semiconductor signal and carbon background. The recovered quantitative composition is validated by detailed Monte Carlo simulations and is confirmed by separate cross-sectional TEM EDX measurements of the nanostructures. This shows that SEM EDX measurements together with machine learning blind source separation processing could be successfully used for the nanostructures quantitative chemical composition determination.

The X-ray correlation spectroscopy instrument at the Linac Coherent Light Source

DOE PAGES

Alonso-Mori, Roberto; Caronna, Chiara; Chollet, Matthieu; ...

2015-03-03

The X-ray Correlation Spectroscopy instrument is dedicated to the study of dynamics in condensed matter systems using the unique coherence properties of free-electron lasers. It covers a photon energy range of 4–25 keV. The intrinsic temporal characteristics of the Linac Coherent Light Source, in particular the 120 Hz repetition rate, allow for the investigation of slow dynamics (milliseconds) by means of X-ray photon correlation spectroscopy. Double-pulse schemes could probe dynamics on the picosecond timescale. In addition, a description of the instrument capabilities and recent achievements is presented.

A high-temperature furnace for in situ synchrotron X-ray spectroscopy under controlled atmospheric conditions.

PubMed

Eeckhout, Sigrid Griet; Gorges, Bernard; Barthe, Laurent; Pelosi, Orietta; Safonova, Olga; Giuli, Gabriele

2008-09-01

A high-temperature furnace with an induction heater coil has been designed and constructed for in situ X-ray spectroscopic experiments under controlled atmospheric conditions and temperatures up to 3275 K. The multi-purpose chamber design allows working in backscattering and normal fluorescence mode for synchrotron X-ray absorption and emission spectroscopy. The use of the furnace is demonstrated in a study of the in situ formation of Cr oxide between 1823 K and 2023 K at logPO(2) values between -10.0 and -11.3 using X-ray absorption near-edge spectroscopy. The set-up is of particular interest for studying liquid metals, alloys and other electrically conductive materials under extreme conditions.

X-ray spectroscopy studies of nonradiative energy transfer processes in luminescent lanthanide materials

NASA Astrophysics Data System (ADS)

Pacold, Joseph I.

Luminescent materials play important roles in energy sciences, through solid state lighting and possible applications in solar energy utilization, and in biomedical research and applications, such as in immunoassays and fluorescence microscopy. The initial excitation of a luminescent material leads to a sequence of transitions between excited states, ideally ending with the emission of one or more optical-wavelength photons. It is essential to understand the microscopic physics of this excited state cascade in order to rationally design materials with high quantum efficiencies or with other fine-tuning of materials response. While optical-wavelength spectroscopies have unraveled many details of the energy transfer pathways in luminescent materials, significant questions remain open for many lanthanide-based luminescent materials. For organometallic dyes in particular, quantum yields remain limited in comparison with inorganic phosphors. This dissertation reports on a research program of synchrotron x-ray studies of the excited state electronic structure and energy-relaxation cascade in trivalent lanthanide phosphors and dyes. To this end, one of the primary results presented here is the first time-resolved x-ray absorption near edge spectroscopy studies of the transient 4f excited states in lanthanide-activated luminescent dyes and phosphors. This is a new application of time-resolved x-ray absorption spectroscopy that makes it possible to directly observe and, to some extent, quantify intramolecular nonradiative energy transfer processes. We find a transient increase in 4f spectral weight associated with an excited state confined to the 4f shell of trivalent Eu. This result implies that it is necessary to revise the current theoretical understanding of 4f excitation in trivalent lanthanide activators: either transient 4f-5d mixing effects are much stronger than previously considered, or else the lanthanide 4f excited state has an unexpectedly large contribution

Low Dose X-Ray Speckle Visibility Spectroscopy Reveals Nanoscale Dynamics in Radiation Sensitive Ionic Liquids

NASA Astrophysics Data System (ADS)

Verwohlt, Jan; Reiser, Mario; Randolph, Lisa; Matic, Aleksandar; Medina, Luis Aguilera; Madsen, Anders; Sprung, Michael; Zozulya, Alexey; Gutt, Christian

2018-04-01

X-ray radiation damage provides a serious bottleneck for investigating microsecond to second dynamics on nanometer length scales employing x-ray photon correlation spectroscopy. This limitation hinders the investigation of real time dynamics in most soft matter and biological materials which can tolerate only x-ray doses of kGy and below. Here, we show that this bottleneck can be overcome by low dose x-ray speckle visibility spectroscopy. Employing x-ray doses of 22-438 kGy and analyzing the sparse speckle pattern of count rates as low as 6.7 ×10-3 per pixel, we follow the slow nanoscale dynamics of an ionic liquid (IL) at the glass transition. At the prepeak of nanoscale order in the IL, we observe complex dynamics upon approaching the glass transition temperature TG with a freezing in of the alpha relaxation and a multitude of millisecond local relaxations existing well below TG . We identify this fast relaxation as being responsible for the increasing development of nanoscale order observed in ILs at temperatures below TG .

Pushing the Boundaries of X-ray Grating Spectroscopy in a Suborbital Rocket

NASA Technical Reports Server (NTRS)

McEntaffer, Randall L.; DeRoo, Casey; Schultz, Ted; Zhang, William W.; Murray, Neil J.; O'Dell, Stephen; Cash, Webster

2013-01-01

Developments in grating spectroscopy are paramount for meeting the soft X-ray science goals of future NASA X-ray Observatories. While developments in the laboratory setting have verified the technical feasibility of using off-plane reflection gratings to reach this goal, flight heritage is a key step in the development process toward large missions. To this end we have developed a design for a suborbital rocket payload employing an Off-Plane X-ray Grating Spectrometer. This spectrometer utilizes slumped glass Wolter-1 optics, an array of gratings, and a CCD camera. We discuss the unique capabilities of this design, the expected performance, the science return, and the perceived impact to future missions.

X-ray Spectroscopy of a TDE

NASA Astrophysics Data System (ADS)

Kochanek, Christopher

2017-09-01

Tidal disruption events (TDE), where supermassive black holes destroy stars to produce accretion flares, are of great current observational and theoretical interest. Here we propose a four epoch HRC/LETG X-ray spectroscopic ``movie'' of a TDE spread over the first 40 days of an X-ray bright TDE, including any discovered by our ASAS-SN survey, supported and extended by higher cadence Swift XRT/UVOT observations over the first 100 days. For this next X-ray bright TDE, we will measure the evolution of the X-ray emission (luminosity/temperature) from the hot accretion disk, the emission reprocessed by the debris into UV/optical, and use X-ray absorption (or emission) features to look at the abundances and the evolution of the kinematics and ionization parameter.

X-Ray Imaging System

NASA Technical Reports Server (NTRS)

1986-01-01

The FluoroScan Imaging System is a high resolution, low radiation device for viewing stationary or moving objects. It resulted from NASA technology developed for x-ray astronomy and Goddard application to a low intensity x-ray imaging scope. FlouroScan Imaging Systems, Inc, (formerly HealthMate, Inc.), a NASA licensee, further refined the FluoroScan System. It is used for examining fractures, placement of catheters, and in veterinary medicine. Its major components include an x-ray generator, scintillator, visible light image intensifier and video display. It is small, light and maneuverable.

Two-dimensional functional molecular nanoarchitectures - Complementary investigations with scanning tunneling microscopy and X-ray spectroscopy

NASA Astrophysics Data System (ADS)

Klappenberger, Florian

2014-02-01

Functional molecular nanoarchitectures (FMNs) are highly relevant for the development of future nanotechnology devices. Profound knowledge about the atomically controlled construction of such nanoscale assemblies is an indispensable requirement to render the implementation of such components into a real product successful. For exploiting their full potential the architectures’ functionalities have to be characterized in detail including the ways to tailor them. In recent years a plethora of sophisticated constructs were fabricated touching a wide range of research topics. The present review summarizes important achievements of bottom-up fabricated, molecular nanostructures created on single crystal metal surfaces under ultra-high vacuum conditions. This selection focuses on examples where self-assembly mechanisms played a central role for their construction. Such systems, though typically quite complex, can be comprehensively understood by the STM+XS approach combining scanning tunneling microscopy (STM) with X-ray spectroscopy (XS) and being aided in the atomic interpretation by the appropriate theoretic analysis, often from density functional theory. The symbiosis of the techniques is especially fruitful because of the complementary character of the information accessed by the local microscopy and the space-averaging spectroscopy tools. STM delivers sub-molecular spatial-resolution, but suffers from limited sensitivity for the chemical and conformational states of the building-blocks. XS compensates these weaknesses with element- and moiety-specific data, which in turn would be hard to interpret with respect to structure formation without the topographic details revealed by STM. The united merit of this methodology allows detailed geometric information to be obtained and addresses both the electronic and chemical state of the complex organic species constituting such architectures. Thus, possible changes induced by the various processes such as surface

Fast Atomic-Scale Elemental Mapping of Crystalline Materials by STEM Energy-Dispersive X-Ray Spectroscopy Achieved with Thin Specimens [Fast Atomic-Scale Chemical Imaging of Crystalline Materials by STEM Energy-Dispersive X-ray Spectroscopy Achieved with Thin Specimens].

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu, Ping; Yuan, Renliang; Zuo, Jian Min

Abstract Elemental mapping at the atomic-scale by scanning transmission electron microscopy (STEM) using energy-dispersive X-ray spectroscopy (EDS) provides a powerful real-space approach to chemical characterization of crystal structures. However, applications of this powerful technique have been limited by inefficient X-ray emission and collection, which require long acquisition times. Recently, using a lattice-vector translation method, we have shown that rapid atomic-scale elemental mapping using STEM-EDS can be achieved. This method provides atomic-scale elemental maps averaged over crystal areas of ~few 10 nm 2with the acquisition time of ~2 s or less. Here we report the details of this method, and, inmore » particular, investigate the experimental conditions necessary for achieving it. It shows, that in addition to usual conditions required for atomic-scale imaging, a thin specimen is essential for the technique to be successful. Phenomenological modeling shows that the localization of X-ray signals to atomic columns is a key reason. The effect of specimen thickness on the signal delocalization is studied by multislice image simulations. The results show that the X-ray localization can be achieved by choosing a thin specimen, and the thickness of less than about 22 nm is preferred for SrTiO 3in [001] projection for 200 keV electrons.« less

Fast Atomic-Scale Elemental Mapping of Crystalline Materials by STEM Energy-Dispersive X-Ray Spectroscopy Achieved with Thin Specimens [Fast Atomic-Scale Chemical Imaging of Crystalline Materials by STEM Energy-Dispersive X-ray Spectroscopy Achieved with Thin Specimens].

DOE PAGES

Lu, Ping; Yuan, Renliang; Zuo, Jian Min

2017-02-23

Abstract Elemental mapping at the atomic-scale by scanning transmission electron microscopy (STEM) using energy-dispersive X-ray spectroscopy (EDS) provides a powerful real-space approach to chemical characterization of crystal structures. However, applications of this powerful technique have been limited by inefficient X-ray emission and collection, which require long acquisition times. Recently, using a lattice-vector translation method, we have shown that rapid atomic-scale elemental mapping using STEM-EDS can be achieved. This method provides atomic-scale elemental maps averaged over crystal areas of ~few 10 nm 2with the acquisition time of ~2 s or less. Here we report the details of this method, and, inmore » particular, investigate the experimental conditions necessary for achieving it. It shows, that in addition to usual conditions required for atomic-scale imaging, a thin specimen is essential for the technique to be successful. Phenomenological modeling shows that the localization of X-ray signals to atomic columns is a key reason. The effect of specimen thickness on the signal delocalization is studied by multislice image simulations. The results show that the X-ray localization can be achieved by choosing a thin specimen, and the thickness of less than about 22 nm is preferred for SrTiO 3in [001] projection for 200 keV electrons.« less

Energy-discrimination x-ray computed tomography system utilizing a scanning cadmium-telluride detector

NASA Astrophysics Data System (ADS)

Sato, Eiichi; Abduraxit, Ablajan; Enomoto, Toshiyuki; Watanabe, Manabu; Hitomi, Keitaro; Takahashi, Kiyomi; Sato, Shigehiro; Ogawa, Akira; Onagawa, Jun

2010-04-01

An energy-discrimination K-edge x-ray computed tomography (CT) system is useful for controlling the image contrast of a target region by selecting both the photon energy and the energy width. The CT system has an oscillation-type linear cadmium telluride (CdTe) detectror. CT is performed by repeated linear scans and rotations of an object. Penetrating x-ray photons from the object are detected by a CdTe detector, and event signals of x-ray photons are produced using charge-sensitive and shaping amplifiers. Both photon energy and energy width are selected out using a multichannel analyzer, and the number of photons is counted by a counter card. In energy-discrimination CT, the tube voltage and tube current were 80 kV and 20 μA, respectively, and the x-ray intensity was 1.92 μGy/s at a distance of 1.0 m from the source and a tube voltage of 80 kV. The energy-discrimination CT was carried out by selecting x-ray photon energies.

Combined scanning transmission X-ray and electron microscopy for the characterization of bacterial endospores.

PubMed

Jamroskovic, Jan; Shao, Paul P; Suvorova, Elena; Barak, Imrich; Bernier-Latmani, Rizlan

2014-09-01

Endospores (also referred to as bacterial spores) are bacterial structures formed by several bacterial species of the phylum Firmicutes. Spores form as a response to environmental stress. These structures exhibit remarkable resistance to harsh environmental conditions such as exposure to heat, desiccation, and chemical oxidants. The spores include several layers of protein and peptidoglycan that surround a core harboring DNA as well as high concentrations of calcium and dipicolinic acid (DPA). A combination of scanning transmission X-ray microscopy, scanning transmission electron microscopy, and energy dispersive spectroscopy was used for the direct quantitative characterization of bacterial spores. The concentration and localization of DPA, Ca(2+) , and other elements were determined and compared for the core and cortex of spores from two distinct genera: Bacillus subtilis and Desulfotomaculum reducens. This micro-spectroscopic approach is uniquely suited for the direct study of individual bacterial spores, while classical molecular and biochemical methods access only bulk characteristics. © 2014 Federation of European Microbiological Societies. Published by John Wiley & Sons Ltd. All rights reserved.

Development of polycapillary x-ray optics for x-ray spectroscopy

NASA Astrophysics Data System (ADS)

Adams, Bernhard W.; Attenkofer, Klaus; Bond, Justin L.; Craven, Christopher A.; Cremer, Till; O'Mahony, Aileen; Minot, Michael J.; Popecki, Mark A.

2016-09-01

Bundles of hollow glass capillaries can be tapered to produce quasi-focusing x-ray optics. These optics are known as Kumakhov lenses. These optics are interesting for lab-based sources because they can be used to collimate and concentrate x-rays originating from a point, such as a laser focus or an electron-beam focus in a microtube.

Distinct charge dynamics in battery electrodes revealed by in situ and operando soft X-ray spectroscopy

PubMed Central

Liu, Xiaosong; Wang, Dongdong; Liu, Gao; Srinivasan, Venkat; Liu, Zhi; Hussain, Zahid; Yang, Wanli

2013-01-01

Developing high-performance batteries relies on material breakthroughs. During the past few years, various in situ characterization tools have been developed and have become indispensible in studying and the eventual optimization of battery materials. However, soft X-ray spectroscopy, one of the most sensitive probes of electronic states, has been mainly limited to ex situ experiments for battery research. Here we achieve in situ and operando soft X-ray absorption spectroscopy of lithium-ion battery cathodes. Taking advantage of the elemental, chemical and surface sensitivities of soft X-rays, we discover distinct lithium-ion and electron dynamics in Li(Co1/3Ni1/3Mn1/3)O2 and LiFePO4 cathodes in polymer electrolytes. The contrast between the two systems and the relaxation effect in LiFePO4 is attributed to a phase transformation mechanism, and the mesoscale morphology and charge conductivity of the electrodes. These discoveries demonstrate feasibility and power of in situ soft X-ray spectroscopy for studying integrated and dynamic effects in batteries. PMID:24100759

Electronic Structure of the Organic Semiconductor Alq3 (aluminum tris-8-hydroxyquinoline) from Soft X-ray Spectroscopies and Density Functional Theory Calculations

DOE Office of Scientific and Technical Information (OSTI.GOV)

DeMasi, A.; Piper, L; Zhang, Y

2008-01-01

The element-specific electronic structure of the organic semiconductor aluminum tris-8-hydroxyquinoline (Alq3) has been studied using a combination of resonant x-ray emission spectroscopy, x-ray photoelectron spectroscopy, x-ray absorption spectroscopy, and density functional theory (DFT) calculations. Resonant and nonresonant x-ray emission spectroscopy were used to measure directly the carbon, nitrogen and oxygen 2p partial densities of states in Alq3, and good agreement was found with the results of DFT calculations. Furthermore, resonant x-ray emission at the carbon K-edge is shown to be able to measure the partial density of states associated with individual C sites. Finally, comparison of previous x-ray emission studiesmore » and the present data reveal the presence of clear photon-induced damage in the former.« less

Electronic structure of the organic semiconductor Alq3 (aluminum tris-8-hydroxyquinoline) from soft x-ray spectroscopies and density functional theory calculations.

PubMed

DeMasi, A; Piper, L F J; Zhang, Y; Reid, I; Wang, S; Smith, K E; Downes, J E; Peltekis, N; McGuinness, C; Matsuura, A

2008-12-14

The element-specific electronic structure of the organic semiconductor aluminum tris-8-hydroxyquinoline (Alq(3)) has been studied using a combination of resonant x-ray emission spectroscopy, x-ray photoelectron spectroscopy, x-ray absorption spectroscopy, and density functional theory (DFT) calculations. Resonant and nonresonant x-ray emission spectroscopy were used to measure directly the carbon, nitrogen and oxygen 2p partial densities of states in Alq(3), and good agreement was found with the results of DFT calculations. Furthermore, resonant x-ray emission at the carbon K-edge is shown to be able to measure the partial density of states associated with individual C sites. Finally, comparison of previous x-ray emission studies and the present data reveal the presence of clear photon-induced damage in the former.

Local X-ray magnetic circular dichroism study of Fe/Cu(111) using a tunneling smart tip

PubMed Central

DiLullo, Andrew; Shirato, Nozomi; Cummings, Marvin; Kersell, Heath; Chang, Hao; Rosenmann, Daniel; Miller, Dean; Freeland, John W.; Hla, Saw-Wai; Rose, Volker

2016-01-01

Localized spectroscopy with simultaneous topographic, elemental and magnetic information is presented. A synchrotron X-ray scanning tunneling microscope has been employed for the local study of the X-ray magnetic circular dichroism at the Fe L 2,3-edges of a thin iron film grown on Cu(111). Polarization-dependent X-ray absorption spectra have been obtained through a tunneling smart tip that serves as a photoelectron detector. In contrast to conventional spin-polarized scanning tunneling microscopy, X-ray excitations provide magnetic contrast even with a non-magnetic tip. Intensity variations in the photoexcited tip current point to chemical variations within a single magnetic Fe domain. PMID:26917146

Local X-ray magnetic circular dichroism study of Fe/Cu(111) using a tunneling smart tip

DOE PAGES

DiLullo, Andrew; Shirato, Nozomi; Cummings, Marvin; ...

2016-01-28

Localized spectroscopy with simultaneous topographic, elemental and magnetic information is presented. A synchrotron X-ray scanning tunneling microscope has been employed for the local study of the X-ray magnetic circular dichroism at the FeL 2,3-edges of a thin iron film grown on Cu(111). Polarization-dependent X-ray absorption spectra have been obtained through a tunneling smart tip that serves as a photoelectron detector. In contrast to conventional spin-polarized scanning tunneling microscopy, X-ray excitations provide magnetic contrast even with a non-magnetic tip. Intensity variations in the photoexcited tip current point to chemical variations within a single magnetic Fe domain.

Local X-ray magnetic circular dichroism study of Fe/Cu(111) using a tunneling smart tip.

PubMed

DiLullo, Andrew; Shirato, Nozomi; Cummings, Marvin; Kersell, Heath; Chang, Hao; Rosenmann, Daniel; Miller, Dean; Freeland, John W; Hla, Saw-Wai; Rose, Volker

2016-03-01

Localized spectroscopy with simultaneous topographic, elemental and magnetic information is presented. A synchrotron X-ray scanning tunneling microscope has been employed for the local study of the X-ray magnetic circular dichroism at the Fe L2,3-edges of a thin iron film grown on Cu(111). Polarization-dependent X-ray absorption spectra have been obtained through a tunneling smart tip that serves as a photoelectron detector. In contrast to conventional spin-polarized scanning tunneling microscopy, X-ray excitations provide magnetic contrast even with a non-magnetic tip. Intensity variations in the photoexcited tip current point to chemical variations within a single magnetic Fe domain.

The Development of a Scanning Soft X-Ray Microscope.

NASA Astrophysics Data System (ADS)

Rarback, Harvey Miles

We have developed a scanning soft X-ray microscope, which can be used to image natural biological specimens at high resolution and with less damage than electron microscopy. The microscope focuses a monochromatic beam of synchrotron radiation to a nearly diffraction limited spot with the aid of a high resolution Fresnel zone plate, specially fabricated for us at the IBM Watson Research Center. The specimen at one atmosphere is mechanically scanned through the spot and the transmitted radiation is efficiently detected with a flow proportional counter. A computer forms a realtime transmission image of the specimen which is displayed on a color monitor. Our first generation optics have produced images of natural wet specimens at a resolution of 300 nm.

The X-ray Correlation Spectroscopy instrument at the Linac Coherent Light Source

PubMed Central

Alonso-Mori, Roberto; Caronna, Chiara; Chollet, Matthieu; Curtis, Robin; Damiani, Daniel S.; Defever, Jim; Feng, Yiping; Flath, Daniel L.; Glownia, James M.; Lee, Sooheyong; Lemke, Henrik T.; Nelson, Silke; Bong, Eric; Sikorski, Marcin; Song, Sanghoon; Srinivasan, Venkat; Stefanescu, Daniel; Zhu, Diling; Robert, Aymeric

2015-01-01

The X-ray Correlation Spectroscopy instrument is dedicated to the study of dynamics in condensed matter systems using the unique coherence properties of free-electron lasers. It covers a photon energy range of 4–25 keV. The intrinsic temporal characteristics of the Linac Coherent Light Source, in particular the 120 Hz repetition rate, allow for the investigation of slow dynamics (milli­seconds) by means of X-ray photon correlation spectroscopy. Double-pulse schemes could probe dynamics on the picosecond timescale. A description of the instrument capabilities and recent achievements is presented. PMID:25931061

Extended x-ray absorption fine structure spectroscopy and x-ray absorption near edge spectroscopy study of aliovalent doped ceria to correlate local structural changes with oxygen vacancies clustering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shirbhate, S. C.; Acharya, S. A., E-mail: saha275@yahoo.com; Yadav, A. K.

2016-04-04

This study provides atomic scale insight to understand the role of aliovalent dopants on oxygen vacancies clustering and dissociation mechanism in ceria system in order to enhance the performance of oxy-ion conductor. Dopants induced microscale changes in ceria are probed by extended X-ray absorption fine structure spectroscopy, X-ray absorption near edge spectra, and Raman spectroscopy. The results are explored to establish a correlation between atomic level structural changes (coordination number, interatomic spacing) → formation of dimer and trimer type cation-oxygen vacancies defect complex (intrinsic and extrinsic) → dissociation of oxygen vacancies from defect cluster → ionic conductivity temperature. It ismore » a strategic approach to understand key physics of ionic conductivity mechanism in order to reduce operating temperature of electrolytes for intermediate temperature (300–450 °C) electrochemical devices for the first time.« less

Time-resolved x-ray diffraction and calorimetric studies at low scan rates

PubMed Central

Yao, Haruhiko; Hatta, Ichiro; Koynova, Rumiana; Tenchov, Boris

1992-01-01

The phase transitions of dipalmitoylphosphatidylethanolamine (DPPE) in excess water have been examined by low-angle time-resolved x-ray diffraction and calorimetry at low scan rates. The lamellar subgel/lamellar liquid-crystalline (Lc → Lα), lamellar gel/lamellar liquid-crystalline (Lβ → Lα), and lamellar liquid-crystalline/lamellar gel (Lα → Lβ) phase transitions proceed via coexistence of the initial and final phases with no detectable intermediates at scan rates 0.1 and 0.5°C/min. At constant temperature within the region of the Lβ → Lα transition the ratio of the two coexisting phases was found to be stable for over 30 min. The state of stable phase coexistence was preceded by a 150-s relaxation taking place at constant temperature after termination of the heating scan in the transition region. While no intermediate structures were present in the coexistence region, a well reproducible multipeak pattern, with at least four prominent heat capacity peaks separated in temperature by 0.4-0.5°C, has been observed in the cooling transition (Lα → Lβ) by calorimetry. The multipeak pattern became distinct with an increase of incubation time in the liquid-crystalline phase. It was also clearly resolved in the x-ray diffraction intensity versus temperature plots recorded at slow cooling rates. These data suggest that the equilibrium state of the Lα phase of hydrated DPPE is represented by a mixture of domains that differ in thermal behavior, but cannot be distinguished structurally by x-ray scattering. Imagesp689-aFIGURE 9 PMID:19431820

A time-correlation function approach to nuclear dynamical effects in X-ray spectroscopy.

PubMed

Karsten, Sven; Bokarev, Sergey I; Aziz, Saadullah G; Ivanov, Sergei D; Kühn, Oliver

2017-06-14

Modern X-ray spectroscopy has proven itself as a robust tool for probing the electronic structure of atoms in complex environments. Despite working on energy scales that are much larger than those corresponding to nuclear motions, taking nuclear dynamics and the associated nuclear correlations into account may be of importance for X-ray spectroscopy. Recently, we have developed an efficient protocol to account for nuclear dynamics in X-ray absorption and resonant inelastic X-ray scattering spectra [Karsten et al., J. Phys. Chem. Lett. 8, 992 (2017)], based on ground state molecular dynamics accompanied with state-of-the-art calculations of electronic excitation energies and transition dipoles. Here, we present an alternative derivation of the formalism and elaborate on the developed simulation protocol using gas phase and bulk water as examples. The specific spectroscopic features stemming from the nuclear motions are analyzed and traced down to the dynamics of electronic energy gaps and transition dipole correlation functions. The observed tendencies are explained on the basis of a simple harmonic model, and the involved approximations are discussed. The method represents a step forward over the conventional approaches that treat the system in full complexity and provides a reasonable starting point for further improvements.

A time-correlation function approach to nuclear dynamical effects in X-ray spectroscopy

NASA Astrophysics Data System (ADS)

Karsten, Sven; Bokarev, Sergey I.; Aziz, Saadullah G.; Ivanov, Sergei D.; Kühn, Oliver

2017-06-01

Modern X-ray spectroscopy has proven itself as a robust tool for probing the electronic structure of atoms in complex environments. Despite working on energy scales that are much larger than those corresponding to nuclear motions, taking nuclear dynamics and the associated nuclear correlations into account may be of importance for X-ray spectroscopy. Recently, we have developed an efficient protocol to account for nuclear dynamics in X-ray absorption and resonant inelastic X-ray scattering spectra [Karsten et al., J. Phys. Chem. Lett. 8, 992 (2017)], based on ground state molecular dynamics accompanied with state-of-the-art calculations of electronic excitation energies and transition dipoles. Here, we present an alternative derivation of the formalism and elaborate on the developed simulation protocol using gas phase and bulk water as examples. The specific spectroscopic features stemming from the nuclear motions are analyzed and traced down to the dynamics of electronic energy gaps and transition dipole correlation functions. The observed tendencies are explained on the basis of a simple harmonic model, and the involved approximations are discussed. The method represents a step forward over the conventional approaches that treat the system in full complexity and provides a reasonable starting point for further improvements.

Spatial imaging and speciation of Cu in rice (Oryza sativa L.) roots using synchrotron-based X-ray microfluorescence and X-ray absorption spectroscopy.

PubMed

Lu, Lingli; Xie, Ruohan; Liu, Ting; Wang, Haixing; Hou, Dandi; Du, Yonghua; He, Zhenli; Yang, Xiaoe; Sun, Hui; Tian, Shengke

2017-05-01

Knowledge of elemental localization and speciation in rice (Oryza sativa L.) roots is crucial for elucidating the mechanisms of Cu accumulation so as to facilitate the development of strategies to inhibit Cu accumulation in rice grain grown in contaminated soils. Using synchrotron-based X-ray microfluorescence and X-ray absorption spectroscopy, we investigated the distribution patterns and speciation of Cu in rice roots treated with 50 μM Cu for 7 days. A clear preferential localization of Cu in the meristematic zone was observed in root tips as compared with the elongation zone. Investigation of Cu in the root cross sections revealed that the intensity of Cu in the vascular bundles was more than 10-fold higher than that in the other scanned sites (epidermis and cortex) in rice roots. The dominant chemical form of Cu (79.1%) in rice roots was similar to that in the Cu-cell wall compounds. These results suggest that although Cu can be easily transported into the vascular tissues in rice roots, most of the metal absorbed by plants is retained in the roots owing to its high binding to the cell wall compounds, thus preventing metal translocation to the aerial parts of the plants. Copyright © 2017 Elsevier Ltd. All rights reserved.

Application of Scanning Electron Microscopy/Energy-Dispersive X-Ray Spectroscopy for Characterization of Detrital Minerals in Karst Cave Speleothems.

PubMed

Zupančič, Nina; Miler, Miloš; Šebela, Stanka; Jarc, Simona

2016-02-01

Micro-scale observations in karst caves help to identify different processes that shaped local morphology. Scanning electron microscopy/energy-dispersive X-ray spectroscopy inspection of speleothems from two karst caves in Slovenia, Predjama and Črna Jama, confirmed the presence of sub-angular to sub-rounded detrital fragments of clay minerals, feldspars, quartz, Fe-oxides/hydroxides, rutile and Nb-rutile, xenotime, kassite, allanite, fluorapatite, epidote, ilmenite, monazite, sphene, and zircon, between 2 and 50 μm across. These occur in porous layers separating calcite laminae in the clayey coating on the layer below the surface of the speleothems, and are also incorporated within actual crystals. It is likely that they are derived from the weathered rocks of the Eocene flysch. Probably they were first transported into the caves by floodwaters forming cave sediments. Later, depending upon the climate conditions, they were moved by air currents or by water to the surface of active speleothems. They might also be redeposited from overlying soils enriched with wind-transported minerals from the flysch, or from higher passages filled with weathered flysch sediment, by drip water percolating through the fissured limestone. As some of the identified minerals are carriers of rare earth elements, Ti and Zr, their presence could affect any palaeoclimatic interpretations that are based upon the geochemical composition of the speleothems.

Detecting element specific electrons from a single cobalt nanocluster with synchrotron x-ray scanning tunneling microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kersell, Heath; Shirato, Nozomi; Cummings, Marvin

We use a nanofabricated scanning tunneling microscope tip as a detector to investigate local X-ray induced tunneling and electron emission from a single cobalt nanocluster on a Au(111) surface. The tip-detector is positioned a few angstroms above the nanocluster, and ramping the incident X-ray energy across the Co photoabsorption K-edge enables the detection of element specific electrons. Atomic-scale spatial dependent changes in the X-ray absorption cross section are directly measured by taking the X-ray induced current as a function of X-ray energy. From the measured sample and tip currents, element specific X-ray induced current components can be separated and therebymore » the corresponding yields for the X-ray induced processes of the single cobalt nanocluster can be determined. The detection of element specific synchrotron X-ray induced electrons of a single nanocluster opens a new avenue for materials characterization on a one particle at-a-time basis.« less

Detecting element specific electrons from a single cobalt nanocluster with synchrotron x-ray scanning tunneling microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kersell, Heath; Shirato, Nozomi; Cummings, Marvin

Here, we use a nanofabricated scanning tunneling microscope tip as a detector to investigate local X-ray induced tunneling and electron emission from a single cobalt nanocluster on a Au(111) surface. The tip-detector is positioned a few angstroms above the nanocluster, and ramping the incident X-ray energy across the Co photoabsorption K-edge enables the detection of element specific electrons. Atomic-scale spatial dependent changes in the X-ray absorption cross section are directly measured by taking the X-ray induced current as a function of X-ray energy. From the measured sample and tip currents, element specific X-ray induced current components can be separated andmore » thereby the corresponding yields for the X-ray induced processes of the single cobalt nanocluster can be determined. The detection of element specific synchrotron X-ray induced electrons of a single nanocluster opens a new avenue for materials characterization on a one particle at-a-time basis.« less

Detecting element specific electrons from a single cobalt nanocluster with synchrotron x-ray scanning tunneling microscopy

DOE PAGES

Kersell, Heath; Shirato, Nozomi; Cummings, Marvin; ...

2017-09-05

Here, we use a nanofabricated scanning tunneling microscope tip as a detector to investigate local X-ray induced tunneling and electron emission from a single cobalt nanocluster on a Au(111) surface. The tip-detector is positioned a few angstroms above the nanocluster, and ramping the incident X-ray energy across the Co photoabsorption K-edge enables the detection of element specific electrons. Atomic-scale spatial dependent changes in the X-ray absorption cross section are directly measured by taking the X-ray induced current as a function of X-ray energy. From the measured sample and tip currents, element specific X-ray induced current components can be separated andmore » thereby the corresponding yields for the X-ray induced processes of the single cobalt nanocluster can be determined. The detection of element specific synchrotron X-ray induced electrons of a single nanocluster opens a new avenue for materials characterization on a one particle at-a-time basis.« less

Tracking reaction dynamics in solution by pump-probe X-ray absorption spectroscopy and X-ray liquidography (solution scattering).

PubMed

Kim, Jeongho; Kim, Kyung Hwan; Oang, Key Young; Lee, Jae Hyuk; Hong, Kiryong; Cho, Hana; Huse, Nils; Schoenlein, Robert W; Kim, Tae Kyu; Ihee, Hyotcherl

2016-03-07

Characterization of transient molecular structures formed during chemical and biological processes is essential for understanding their mechanisms and functions. Over the last decade, time-resolved X-ray liquidography (TRXL) and time-resolved X-ray absorption spectroscopy (TRXAS) have emerged as powerful techniques for molecular and electronic structural analysis of photoinduced reactions in the solution phase. Both techniques make use of a pump-probe scheme that consists of (1) an optical pump pulse to initiate a photoinduced process and (2) an X-ray probe pulse to monitor changes in the molecular structure as a function of time delay between pump and probe pulses. TRXL is sensitive to changes in the global molecular structure and therefore can be used to elucidate structural changes of reacting solute molecules as well as the collective response of solvent molecules. On the other hand, TRXAS can be used to probe changes in both local geometrical and electronic structures of specific X-ray-absorbing atoms due to the element-specific nature of core-level transitions. These techniques are complementary to each other and a combination of the two methods will enhance the capability of accurately obtaining structural changes induced by photoexcitation. Here we review the principles of TRXL and TRXAS and present recent application examples of the two methods for studying chemical and biological processes in solution. Furthermore, we briefly discuss the prospect of using X-ray free electron lasers for the two techniques, which will allow us to keep track of structural dynamics on femtosecond time scales in various solution-phase molecular reactions.

Chemical Modification of Graphene Oxide by Nitrogenation: An X-ray Absorption and Emission Spectroscopy Study

NASA Astrophysics Data System (ADS)

Chuang, Cheng-Hao; Ray, Sekhar C.; Mazumder, Debarati; Sharma, Surbhi; Ganguly, Abhijit; Papakonstantinou, Pagona; Chiou, Jau-Wern; Tsai, Huang-Ming; Shiu, Hung-Wei; Chen, Chia-Hao; Lin, Hong-Ji; Guo, Jinghua; Pong, Way-Faung

2017-02-01

Nitrogen-doped graphene oxides (GO:Nx) were synthesized by a partial reduction of graphene oxide (GO) using urea [CO(NH2)2]. Their electronic/bonding structures were investigated using X-ray absorption near-edge structure (XANES), valence-band photoemission spectroscopy (VB-PES), X-ray emission spectroscopy (XES) and resonant inelastic X-ray scattering (RIXS). During GO:Nx synthesis, different nitrogen-bonding species, such as pyrrolic/graphitic-nitrogen, were formed by replacing of oxygen-containing functional groups. At lower N-content (2.7 at%), pyrrolic-N, owing to surface and subsurface diffusion of C, N and NH is deduced from various X-ray spectroscopies. In contrast, at higher N-content (5.0 at%) graphitic nitrogen was formed in which each N-atom trigonally bonds to three distinct sp2-hybridized carbons with substitution of the N-atoms for C atoms in the graphite layer. Upon nitrogen substitution, the total density of state close to Fermi level is increased to raise the valence-band maximum, as revealed by VB-PES spectra, indicating an electron donation from nitrogen, molecular bonding C/N/O coordination or/and lattice structure reorganization in GO:Nx. The well-ordered chemical environments induced by nitrogen dopant are revealed by XANES and RIXS measurements.

Mössbauer spectroscopy and X-ray diffraction analyses of clayey samples used as ceramic sourcing materials, in Peru

NASA Astrophysics Data System (ADS)

Quille, Rubén; Bustamante, Ángel; Palomino, Ybar

2011-11-01

The ceramic industry is an important area of economic activity in the Ayacucho Region, in particular in the District of Quinua. As a consequence, there is a huge demand for clay to produce ceramic pastes in that region. This paper reports on results concerning the mineralogical characterization of four clayey samples, which were collected MAA and SPQA from the area Pampa de La Quinua with geographic coordinates 13° 02' 49″ S 74° 08' 03″ W, CE1M and CE2M from the Quinua locality 13° 03' 07″ S 74° 08' 31″ W, both in the District of Quinua, Province of Huamanga, Ayacucho, Peru. The chemical and mineralogical characterization of these samples was carried out with powder X-ray diffraction detecting quartz, albite, montmorillonite, kaolinite and glauconite mineral phases, Mössbauer spectroscopy detected iron in kaolinite, glauconite and montmorillonite minerals. Chemical analysis was performed through scanning electron microscopy and energy dispersive X-ray spectroscopy. Data obtained from the combination of these techniques provided relevant information about the morphology, chemical composition, and the mineralogy of samples.

Near- and Extended-Edge X-Ray-Absorption Fine-Structure Spectroscopy Using Ultrafast Coherent High-Order Harmonic Supercontinua

NASA Astrophysics Data System (ADS)

Popmintchev, Dimitar; Galloway, Benjamin R.; Chen, Ming-Chang; Dollar, Franklin; Mancuso, Christopher A.; Hankla, Amelia; Miaja-Avila, Luis; O'Neil, Galen; Shaw, Justin M.; Fan, Guangyu; Ališauskas, Skirmantas; Andriukaitis, Giedrius; Balčiunas, Tadas; Mücke, Oliver D.; Pugzlys, Audrius; Baltuška, Andrius; Kapteyn, Henry C.; Popmintchev, Tenio; Murnane, Margaret M.

2018-03-01

Recent advances in high-order harmonic generation have made it possible to use a tabletop-scale setup to produce spatially and temporally coherent beams of light with bandwidth spanning 12 octaves, from the ultraviolet up to x-ray photon energies >1.6 keV . Here we demonstrate the use of this light for x-ray-absorption spectroscopy at the K - and L -absorption edges of solids at photon energies near 1 keV. We also report x-ray-absorption spectroscopy in the water window spectral region (284-543 eV) using a high flux high-order harmonic generation x-ray supercontinuum with 109 photons/s in 1% bandwidth, 3 orders of magnitude larger than has previously been possible using tabletop sources. Since this x-ray radiation emerges as a single attosecond-to-femtosecond pulse with peak brightness exceeding 1026 photons/s /mrad2/mm2/1 % bandwidth, these novel coherent x-ray sources are ideal for probing the fastest molecular and materials processes on femtosecond-to-attosecond time scales and picometer length scales.

Characterization of Colloidal Quantum Dot Ligand Exchange by X-ray Photoelectron Spectroscopy

NASA Astrophysics Data System (ADS)

Atewologun, Ayomide; Ge, Wangyao; Stiff-Roberts, Adrienne D.

2013-05-01

Colloidal quantum dots (CQDs) are chemically synthesized semiconductor nanoparticles with size-dependent wavelength tunability. Chemical synthesis of CQDs involves the attachment of long organic surface ligands to prevent aggregation; however, these ligands also impede charge transport. Therefore, it is beneficial to exchange longer surface ligands for shorter ones for optoelectronic devices. Typical characterization techniques used to analyze surface ligand exchange include Fourier-transform infrared spectroscopy, x-ray diffraction, transmission electron microscopy, and nuclear magnetic resonance spectroscopy, yet these techniques do not provide a simultaneously direct, quantitative, and sensitive method for evaluating surface ligands on CQDs. In contrast, x-ray photoelectron spectroscopy (XPS) can provide nanoscale sensitivity for quantitative analysis of CQD surface ligand exchange. A unique aspect of this work is that a fingerprint is identified for shorter surface ligands by resolving the regional XPS spectrum corresponding to different types of carbon bonds. In addition, a deposition technique known as resonant infrared matrix-assisted pulsed laser evaporation is used to improve the CQD film uniformity such that stronger XPS signals are obtained, enabling more accurate analysis of the ligand exchange process.

A structural study of bone changes in knee osteoarthritis by synchrotron-based X-ray fluorescence and X-ray absorption spectroscopy techniques

NASA Astrophysics Data System (ADS)

Sindhupakorn, Bura; Thienpratharn, Suwittaya; Kidkhunthod, Pinit

2017-10-01

Osteoarthritis (OA) is characterized by degeneration of articular cartilage and thickening of subchondral bone. The present study investigated the changing of biochemical components of cartilage and bone compared between normal and OA people. Using Synchrotron-based X-ray fluorescence (SR-XRF) and X-ray absorption spectroscopy (XAS) techniquesincluding X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) were employed for the bone changes in kneeosteoarthritisstudies. The bone samples were collected from various osteoarthritis patients with both male and female in the ages range between 20 and 74 years old. SR-XRF results excited at 4240 eV for Ca elements show a majority three main groups, based on their XRF intensities, 20-36 years, 40-60 years and over 70 years, respectively. By employing XAS techniques, XANES features can be used to clearly explain in term of electronic transitions occurring in bone samples which are affected from osteoarthritis symptoms. Moreover, a structural change around Ca ions in bone samples is obviously obtained by EXAFS results indicating an increase of Ca-amorphous phase when the ages increase.

Very high resolution UV and X-ray spectroscopy and imagery of solar active regions

NASA Technical Reports Server (NTRS)

Bruner, M.; Brown, W. A.; Haisch, B. M.

1987-01-01

A scientific investigation of the physics of the solar atmosphere, which uses the techniques of high resolution soft X-ray spectroscopy and high resolution UV imagery, is described. The experiments were conducted during a series of three sounding rocket flights. All three flights yielded excellent images in the UV range, showing unprecedented spatial resolution. The second flight recorded the X-ray spectrum of a solar flare, and the third that of an active region. A normal incidence multi-layer mirror was used during the third flight to make the first astronomical X-ray observations using this new technique.

X-ray Fluorescence Core Scanning of Oman Drilling Project Holes BT1B and GT3A Cores on D/V CHIKYU

NASA Astrophysics Data System (ADS)

Johnson, K. T. M.; Kelemen, P. B.; Michibayashi, K.; Greenberger, R. N.; Koepke, J.; Beinlich, A.; Morishita, T.; Jesus, A. P. M.; Lefay, R.

2017-12-01

The JEOL JSX-3600CA1 energy dispersive X-ray fluorescence core logger (XRF-CL) on the D/V Chikyu provides quantitative element concentrations of scanned cores. Scans of selected intervals are made on an x-y grid with point spacing of 5 mm. Element concentrations for Si, Al, Ti, Ca, Mg, Mn, Fe, Na, K, Cr, Ni, S and Zn are collected for each point on the grid. Accuracy of element concentrations provided by the instrument software is improved by applying empirical correction algorithms. Element concentrations were collected for 9,289 points from twenty-seven core intervals in Hole BT1B (basal thrust) and for 6,389 points from forty core intervals in Hole GT3A (sheeted dike-gabbro transition) of the Oman Drilling Project on the D/V Chikyu XRF-CL during Leg 2 of the Oman Drilling Project in August-September, 2017. The geochemical data are used for evaluating downhole compositional details associated with lithological changes, unit contacts and mineralogical variations and are particularly informative when plotted as concentration contour maps or downhole concentration diagrams. On Leg 2 additional core scans were made with X-ray Computed Tomography (X-ray CT) and infrared images from the visible-shortwave infrared imaging spectroscopy (IR) systems on board. XRF-CL, X-ray CT and IR imaging plots used together provide detailed information on rock compositions, textures and mineralogy that assist naked eye visual observations. Examples of some uses of XRF-CL geochemical maps and downhole data are shown. XRF-CL and IR scans of listvenite clearly show zones of magnesite, dolomite and the Cr-rich mica, fuchsite that are subdued in visual observation, and these scans can be used to calculate variations in proportions of these minerals in Hole BT1B cores. In Hole GT3A XRF-CL data can be used to distinguish compositional changes in different generations of sheeted dikes and gabbros and when combined with visual observations of intrusive relationships the detailed geochemical

CARNAÚBA: The Coherent X-Ray Nanoprobe Beamline for the Brazilian Synchrotron SIRIUS/LNLS

NASA Astrophysics Data System (ADS)

Tolentino, Hélio C. N.; Soares, Márcio M.; Perez, Carlos A.; Vicentin, Flávio C.; Abdala, Dalton B.; Galante, Douglas; Teixeira, Verônica de C.; de Araújo, Douglas H. C.; Westfahl, Harry, Jr.

2017-06-01

The CARNAÚBA beamline is the tender-to-hard X-ray (2 - 15 keV) scanning nanoprobe planned for the 4th generation storage ring SIRIUS at the LNLS. CARNAÚBA uses an undulator source with vertical linear polarization in a low-beta straight section and grazing incidence-focusing mirrors to create a nanoprobe at 143 m from the source. The beamline optic is based on KB mirrors and provides high brilliance at an achromatic focal spot down to the diffraction limit diameter of ˜30 nm with a working distance of ˜6 cm. These characteristics are crucial for studying nanometric samples in experiments involving complex stages and environments. The CARNAÚBA beamline aims to perform raster scans using x-ray fluorescence, x-ray absorption spectroscopy, x-ray diffraction and coherent x-ray imaging techniques. Computed tomography will extend these methods to three dimensions.

Fast Atomic-Scale Elemental Mapping of Crystalline Materials by STEM Energy-Dispersive X-Ray Spectroscopy Achieved with Thin Specimens.

PubMed

Lu, Ping; Yuan, Renliang; Zuo, Jian Min

2017-02-01

Elemental mapping at the atomic-scale by scanning transmission electron microscopy (STEM) using energy-dispersive X-ray spectroscopy (EDS) provides a powerful real-space approach to chemical characterization of crystal structures. However, applications of this powerful technique have been limited by inefficient X-ray emission and collection, which require long acquisition times. Recently, using a lattice-vector translation method, we have shown that rapid atomic-scale elemental mapping using STEM-EDS can be achieved. This method provides atomic-scale elemental maps averaged over crystal areas of ~few 10 nm2 with the acquisition time of ~2 s or less. Here we report the details of this method, and, in particular, investigate the experimental conditions necessary for achieving it. It shows, that in addition to usual conditions required for atomic-scale imaging, a thin specimen is essential for the technique to be successful. Phenomenological modeling shows that the localization of X-ray signals to atomic columns is a key reason. The effect of specimen thickness on the signal delocalization is studied by multislice image simulations. The results show that the X-ray localization can be achieved by choosing a thin specimen, and the thickness of less than about 22 nm is preferred for SrTiO3 in [001] projection for 200 keV electrons.

X-ray scanning of overhead aurorae from rockets

NASA Technical Reports Server (NTRS)

Barcus, J. R.; Goldberg, R. A.; Gesell, L. H.

1981-01-01

Two Nike Tomahawk rocket payloads were launched into energetic auroral events in September, 1976 to investigate the structure of these events, as well as their effects on the atmosphere. X-ray scintillation detectors with energy discrimination in four ranges were used to measure the deposition of bremsstrahlung produced X-rays within the stratosphere and mesosphere. Iterative computer techniques were used to reconstruct X-ray source maps at 100 km, taking atmospheric absorption effects into account. Payload 18.178 was launched on September 21st into an aurora having two distinct azimuthal regions of optical brightness. The X-ray scanner detected the same features, and overlays of the X-ray source maps on all-sky photographs showed spatial coincidence of the X-ray with optical features at the lower energies (below 40 keV). Payload 18.179 was launched September 23rd into an aurora with a more diffuse character. The optical structure did not coincide as well with the measured X-ray structure. There was also an indication of a two-component spectrum for each event, with the hard component originating in the more diffuse, optically faint regions.

Johann Spectrometer for High Resolution X-ray Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Machek, Pavel; Froeba, Michael; Welter, Edmund

2007-01-19

A newly designed vacuum Johann spectrometer with a large focusing analyzer crystal for inelastic x-ray scattering and high resolution fluorescence spectroscopy has been installed at the DORIS III storage ring. Spherically bent crystals with a maximum diameter of 125 mm, and cylindrically bent crystals are employed as dispersive optical elements. Standard radius of curvature of the crystals is 1000 mm, however, the design of the mechanical components also facilitates measurements with smaller and larger bending radii. Up to four crystals are mounted on a revolving crystal changer which enables crystal changes without breaking the vacuum. The spectrometer works at fixedmore » Bragg angle. It is preferably designed for the measurements in non-scanning mode with a broad beam spot, and offers a large flexibility to set the sample to the optimum position inside the Rowland circle. A deep depletion CCD camera is employed as a position sensitive detector to collect the energy-analyzed photons on the circumference of the Rowland circle. The vacuum in the spectrometer tank is typically 10-6 mbar. The sample chamber is separated from the tank either by 25 {mu}m thick Kapton windows, which allows samples to be measured under ambient conditions, or by two gate valves. The spectrometer is currently installed at wiggler beamline W1 whose working range is 4-10.5 keV with typical flux at the sample of 5x1010photons/s/mm2. The capabilities of the spectrometer are illustrated by resonant inelastic experiments on 3d transition metals and rare earth compounds, and by chemical shift measurements on chromium compounds.« less

Study of a chemically amplified resist for X-ray lithography by Fourier transform infrared spectroscopy.

PubMed

Tan, T L; Wong, D; Lee, P; Rawat, R S; Patran, A

2004-11-01

Future applications of microelectromechanical systems (MEMS) require lithographic performance of very high aspect ratio. Chemically amplified resists (CARs) such as the negative tone commercial SU-8 provide critical advantages in sensitivity, resolution, and process efficiency in deep ultraviolet, electron-beam, and X-ray lithographies (XRLs), which result in a very high aspect ratio. In this investigation, an SU-8 resist was characterized and optimized for X-ray lithographic applications by studying the cross-linking process of the resist under different conditions of resist thickness and X-ray exposure dose. The exposure dose of soft X-ray (SXR) irradiation at the average weighted wavelength of 1.20 nm from a plasma focus device ranges from 100 to 1600 mJ/cm(2) on the resist surface. Resist thickness varies from 3.5 to 15 mum. The cross-linking process of the resist during post-exposure bake (PEB) was accurately monitored using Fourier transform infrared (FT-IR) spectroscopy. The infrared absorption peaks at 862, 914, 972, and 1128 cm(-1) in the spectrum of the SU-8 resist were found to be useful indicators for the completion of cross-linking in the resist. Results of the experiments showed that the cross-linking of SU-8 was optimized at the exposure dose of 800 mJ/cm(2) for resist thicknesses of 3.5, 9.5, and 15 microm. PEB temperature was set at 95 degrees C and time at 3 min. The resist thickness was measured using interference patterns in the FT-IR spectra of the resist. Test structures with an aspect ratio 3:1 on 10 microm thick SU-8 resist film were obtained using scanning electron microscopy (SEM).

Monitoring the recrystallisation of amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering.

PubMed

Palomäki, Emmi; Ahvenainen, Patrik; Ehlers, Henrik; Svedström, Kirsi; Huotari, Simo; Yliruusi, Jouko

2016-07-11

In this paper we present a fast model system for monitoring the recrystallization of quench-cooled amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering. The use of these two methods enables comparison between surface and bulk crystallization. Non-ordered mesoporous silica micro-particles were added to the system in order to alter the rate of crystallization of the amorphous xylitol. Raman measurements showed that adding silica to the system increased the rate of surface crystallization, while X-ray measurements showed that the rate of bulk crystallization decreased. Using this model system it is possible to measure fast changes, which occur in minutes or within a few hours. Raman-spectroscopy and wide-angle X-ray scattering were found to be complementary techniques when assessing surface and bulk crystallization of amorphous xylitol. Copyright © 2016 Elsevier B.V. All rights reserved.

X-ray absorption fine structure and X-ray excited optical luminescence studies of II-VI semiconducting nanostructures

NASA Astrophysics Data System (ADS)

Murphy, Michael Wayne

2010-06-01

Various II-VI semiconducting nanomaterials such as ZnO-ZnS nanoribbons (NRs), CdSxSe1-x nanostructures, ZnS:Mn NRs, ZnS:Mn,Eu nanoprsims (NPs), ZnO:Mn nanopowders, and ZnO:Co nanopowders were synthesized for study. These materials were characterized by techniques such as scanning electron microscopy, transmission electron microscopy, element dispersive X-ray spectroscopy, selected area electron diffraction, and X-ray diffraction. The electronic and optical properties of these nanomaterials were studied by X-ray absorption fine structure (XAFS) spectroscopy and X-ray excited optical luminescence (XEOL) techniques, using tuneable soft X-rays from a synchrotron light source. The complementary nature ofthe XAFS and XEOL techniques give site, element and chemical specific measurements which allow a better understanding of the interplay and role of each element in the system. Chemical vapour deposition (CVD) of ZnS powder in a limited oxygen environment resulted in side-by-side biaxial ZnO-ZnS NR heterostructures. The resulting NRs contained distinct wurtzite ZnS and wurtzite ZnO components with widths of 10--100 nm and 20 --500 nm, respectively and a uniform interface region of 5-15 nm. XAFS and XEOL measurements revealed the luminescence of ZnO-ZnS NRs is from the ZnO component. The luminescence of CdSxSe1-x nanostructures is shown to be dependent on the S to Se ratio, with the band-gap emission being tunable between that of pure CdS and CdSe. Excitation of the CdSxSe 1-x nanostructures by X-ray in XEOL has revealed new de-excitation channels which show a defect emission band not seen by laser excitation. CVD of Mn2+ doped ZnS results in nanostructures with luminescence dominated by the yellow Mn2+ emission due to energy transfer from the ZnS host to the Mn dopant sites. The addition of EuCl3 to the reactants in the CVD process results in a change in morphology from NR to NP. Zn1-xMnxO and Zn1-xCOxO nanopowders were prepared by sol-gel methods at dopant concentrations

X-ray Fluorescence Spectroscopy of Pre-Federal American Currency

NASA Astrophysics Data System (ADS)

Raddell, Mark; Manukyan, Khachatur; Aprahamian, Ani; Wiescher, Michael; Jordan, Louis

2017-09-01

X-ray Fluorescence Spectroscopy (XRF) was used to study 17th and 18th century Mexican, Potosí, and Massachusetts silver colonial coins from the University of Notre Dame's Rare Books and Special Collections. Using different configurations and devices, we have learned more about the limitations and optimizations of the method. We have developed a moveable stand that may be used for XRF mapping of coin surfaces. We created standard silver alloy materials for quantification of the elemental composition of the coins. Inductively coupled plasma (ICP) spectroscopy was applied to determine the precise composition of the standards for accurate and non-destructive analyses of the colonial coins. XRF measurements were performed using two different XRF spectrometers, in both air and vacuum conditions, as well as an x-ray beam tube of varying diameters from 2 mm, 1 mm, and 0.03 mm. We quantified both the major elements and the bulk and surface impurities for 90 coins. We are using PCA to look at possible correlations between compositions of coinage from different geographical regions. Preliminary data analyses suggest that Massachusetts coins were minted using silver from Latin American sources. These results are of great interest to historians in tracing the origins of the currency. This work was made possible by the Notre Dame College of Science Summer Undergraduate Research Fellowships (COS-SURF).

New developments in fabrication of high-energy-resolution analyzers for inelastic x-ray spectroscopy.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Said, A. H.; Sinn, H.; Divan, R.

2011-05-01

In this work new improvements related to the fabrication of spherical bent analyzers for 1 meV energy-resolution inelastic X-ray scattering spectroscopy are presented. The new method includes the use of a two-dimensional bender to achieve the required radius of curvature for X-ray analyzers. The advantage of this method is the ability to monitor the focus during bending, which leads to higher-efficiency analyzers.

The CAT-ACT Beamline at ANKA: A new high energy X-ray spectroscopy facility for CATalysis and ACTinide research

NASA Astrophysics Data System (ADS)

Zimina, A.; Dardenne, K.; Denecke, M. A.; Grunwaldt, J. D.; Huttel, E.; Lichtenberg, H.; Mangold, S.; Pruessmann, T.; Rothe, J.; Steininger, R.; Vitova, T.

2016-05-01

A new hard X-ray beamline for CATalysis and ACTinide research has been built at the synchrotron radiation facility ANKA. The beamline design is dedicated to X-ray spectroscopy, including ‘flux hungry’ photon-in/photon-out and correlative techniques with a special infrastructure for radionuclide and catalysis research. The CAT-ACT beamline will help serve the growing need for high flux/hard X-ray spectroscopy in these communities. The design, the first spectra and the current status of this project are reported.

Slit-scanning differential x-ray phase-contrast mammography: proof-of-concept experimental studies.

PubMed

Koehler, Thomas; Daerr, Heiner; Martens, Gerhard; Kuhn, Norbert; Löscher, Stefan; van Stevendaal, Udo; Roessl, Ewald

2015-04-01

The purpose of this work is to investigate the feasibility of grating-based, differential phase-contrast, full-field digital mammography (FFDM) in terms of the requirements for field-of-view (FOV), mechanical stability, and scan time. A rigid, actuator-free Talbot interferometric unit was designed and integrated into a state-of-the-art x-ray slit-scanning mammography system, namely, the Philips MicroDose L30 FFDM system. A dedicated phase-acquisition and phase retrieval method was developed and implemented that exploits the redundancy of the data acquisition inherent to the slit-scanning approach to image generation of the system. No modifications to the scan arm motion control were implemented. The authors achieve a FOV of 160 × 196 mm consisting of two disjoint areas measuring 77 × 196 mm with a gap of 6 mm between them. Typical scanning times vary between 10 and 15 s and dose levels are lower than typical FFDM doses for conventional scans with identical acquisition parameters due to the presence of the source-grating G0. Only minor to moderate artifacts are observed in the three reconstructed images, indicating that mechanical vibrations induced by other system components do not prevent the use of the platform for phase contrast imaging. To the best of our knowledge, this is the first attempt to integrate x-ray gratings hardware into a clinical mammography unit. The results demonstrate that a scanning differential phase contrast FFDM system that meets the requirements of FOV, stability, scan time, and dose can be build.

Clocking Femtosecond Collisional Dynamics via Resonant X-Ray Spectroscopy

NASA Astrophysics Data System (ADS)

van den Berg, Q. Y.; Fernandez-Tello, E. V.; Burian, T.; Chalupský, J.; Chung, H.-K.; Ciricosta, O.; Dakovski, G. L.; Hájková, V.; Hollebon, P.; Juha, L.; Krzywinski, J.; Lee, R. W.; Minitti, M. P.; Preston, T. R.; de la Varga, A. G.; Vozda, V.; Zastrau, U.; Wark, J. S.; Velarde, P.; Vinko, S. M.

2018-02-01

Electron-ion collisional dynamics is of fundamental importance in determining plasma transport properties, nonequilibrium plasma evolution, and electron damage in diffraction imaging applications using bright x-ray free-electron lasers (FELs). Here we describe the first experimental measurements of ultrafast electron impact collisional ionization dynamics using resonant core-hole spectroscopy in a solid-density magnesium plasma, created and diagnosed with the Linac Coherent Light Source x-ray FEL. By resonantly pumping the 1 s →2 p transition in highly charged ions within an optically thin plasma, we have measured how off-resonance charge states are populated via collisional processes on femtosecond time scales. We present a collisional cross section model that matches our results and demonstrates how the cross sections are enhanced by dense-plasma effects including continuum lowering. Nonlocal thermodynamic equilibrium collisional radiative simulations show excellent agreement with the experimental results and provide new insight on collisional ionization and three-body-recombination processes in the dense-plasma regime.

Time-resolved x-ray absorption spectroscopy: Watching atoms dance

NASA Astrophysics Data System (ADS)

Milne, Chris J.; Pham, Van-Thai; Gawelda, Wojciech; van der Veen, Renske M.; El Nahhas, Amal; Johnson, Steven L.; Beaud, Paul; Ingold, Gerhard; Lima, Frederico; Vithanage, Dimali A.; Benfatto, Maurizio; Grolimund, Daniel; Borca, Camelia; Kaiser, Maik; Hauser, Andreas; Abela, Rafael; Bressler, Christian; Chergui, Majed

2009-11-01

The introduction of pump-probe techniques to the field of x-ray absorption spectroscopy (XAS) has allowed the monitoring of both structural and electronic dynamics of disordered systems in the condensed phase with unprecedented accuracy, both in time and in space. We present results on the electronically excited high-spin state structure of an Fe(II) molecular species, [FeII(bpy)3]2+, in aqueous solution, resolving the Fe-N bond distance elongation as 0.2 Å. In addition an analysis technique using the reduced χ2 goodness of fit between FEFF EXAFS simulations and the experimental transient absorption signal in energy space has been successfully tested as a function of excited state population and chemical shift, demonstrating its applicability in situations where the fractional excited state population cannot be determined through other measurements. Finally by using a novel ultrafast hard x-ray 'slicing' source the question of how the molecule relaxes after optical excitation has been successfully resolved using femtosecond XANES.

SUT-NANOTEC-SLRI beamline for X-ray absorption spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Klysubun, Wantana; Kidkhunthod, Pinit; Tarawarakarn, Pongjakr

2017-04-04

The SUT-NANOTEC-SLRI beamline was constructed in 2012 as the flagship of the SUT-NANOTEC-SLRI Joint Research Facility for Synchrotron Utilization, co-established by Suranaree University of Technology (SUT), National Nanotechnology Center (NANOTEC) and Synchrotron Light Research Institute (SLRI). It is an intermediate-energy X-ray absorption spectroscopy (XAS) beamline at SLRI. The beamline delivers an unfocused monochromatic X-ray beam of tunable photon energy (1.25–10 keV). The maximum normal incident beam size is 13 mm (width) × 1 mm (height) with a photon flux of 3 × 10 8to 2 × 10 10 photons s -1(100 mA) -1varying across photon energies. Details of the beamlinemore » and XAS instrumentation are described. To demonstrate the beamline performance,K-edge XANES spectra of MgO, Al 2O 3, S 8, FeS, FeSO 4, Cu, Cu 2O and CuO, and EXAFS spectra of Cu and CuO are presented.« less

Structural studies of homoisoflavonoids: NMR spectroscopy, X-ray diffraction, and theoretical calculations

NASA Astrophysics Data System (ADS)

Sievänen, Elina; Toušek, Jaromír; Lunerová, Kamila; Marek, Jaromír; Jankovská, Dagmar; Dvorská, Margita; Marek, Radek

2010-08-01

In this article we present a detailed structural investigation for five homoisoflavonoids, molecules important from the pharmacological point of view. For studying the electron distribution as well as its influence on the physicochemical properties, NMR spectroscopy, X-ray diffraction, and theoretical calculations have been used. Nuclear magnetic shieldings obtained by using DFT calculations for optimized molecular geometries are correlated with the experimentally determined chemical shifts. The theoretical data are well in agreement with the experimental values. The single crystal X-ray structures of homoisoflavonoid derivatives 1, 3, and 4 have been solved. The molecular geometries and crystal packing determined by X-ray diffraction are used for characterizing the intermolecular interactions. Electron distribution is crucial for the stability of radicals and hence the antioxidant efficiency of flavonoid structures. The hydrogen bonding governs the formation of complexes of homoisoflavonoids with biological targets.

X-Tip: a New Tool for Nanoscience or How to Combine X-Ray Spectroscopies to Local Probe Analysis

NASA Astrophysics Data System (ADS)

Olivier, Dhez; Mario, Rodrigues; Fabio, Comin; Roberto, Felici; Joel, Chevrier

2007-01-01

With the advent of nanoscale science, the need of tools able to image samples and bring the region of interest to the X-ray beam is essential. We show the possibility of using the high resolution imaging capability of a scanning probe microscope to image and align a sample relative to the X-ray beam, as well as the possibility to record the photoelectrons emitted by the sample.

Centaurus X-3. [early x-ray binary star spectroscopy

NASA Technical Reports Server (NTRS)

Hutchings, J. B.; Cowley, A. P.; Crampton, D.; Van Paradus, J.; White, N. E.

1979-01-01

Spectroscopic observations of Krzeminski's star at dispersions 25-60 A/mm are described. The primary is an evolved star of type O6-O8(f) with peculiarities, some of which are attributable to X-ray heating. Broad emission lines at 4640A (N III), 4686 A(He II) and H-alpha show self-absorption and do not originate entirely from the region near the X-ray star. The primary is not highly luminous (bolometric magnitude about -9) and does not show signs of an abnormally strong stellar wind. The X-ray source was 'on' at the time of optical observations. Orbital parameters are presented for the primary, which yield masses of 17 + or - 2 and 1.0 + or - 3 solar masses for the stars. The optical star is undermassive for its luminosity, as are other OB-star X-ray primaries. The rotation is probably synchronized with the orbital motion. The distance to Cen X-3 is estimated to be 10 + or - 1 kpc. Basic data for 12 early-type X-ray primaries are discussed briefly

Inter-diffusion of copper and hafnium as studied by x-ray photoelectron spectroscopy

NASA Astrophysics Data System (ADS)

Pearson, Justin; Chourasia, A. R.

The Cu/Hf interface has been characterized by x-ray photoelectron spectroscopy. Thin films (thicknesses ranging from 100 nm to 150 nm) of hafnium were deposited on a silicon substrate. About 80 nm of copper was then deposited on such samples. The e-beam method was used for the deposition. The samples were annealed for 30 min at temperatures of 100, 200, 300, 400, and 500°C. The inter-diffusion of copper and hafnium was investigated by sequential sputter depth profiling and x-ray photoelectron spectroscopy. The interdiffusion in each case was analyzed by the Matano-Boltzmann's procedure using the Fick's second law. The interdiffusion coefficients and the width of the interface as determined from the data have been correlated with the annealing temperature. Supported by Organized Research, TAMU-Commerce.

The Advanced X-ray Spectroscopy and Imaging Observatory (AXSIO)

NASA Technical Reports Server (NTRS)

White, Nicholas E.; Bookbinder, Jay; Petre, Robert; Smith, Randall; Ptak, Andrew; Tananbaum, Harvey; Garcia, Michael

2012-01-01

Following recommendations from the 2010 "New Worlds, New Horizons" (NWNH) report, the Advanced X-ray Spectroscopy and Imaging Observatory (AXSIO) concept streamlines the International X-ray Observatory (IXO) mission to concentrate on the science objectives that are enabled by high-resolution spectroscopic capabilities. AXSIO will trace orbits close to the event horizon of black holes, measure black hole spin for tens of supermassive black holes (SMBH), use spectroscopy to characterize outflows and the environment of AGN during their peak activity, observe 5MBH out to redshift z=6, map bulk motions and turbulence in galaxy clusters, find the missing baryons in the cosmic web using background quasars, and observe the process of cosmic feedback where black holes and supernovae inject energy on galactic and intergalactic scales. These measurements are enabled by a 0.9 sq m collecting area at 1.25 keV, a micro calorimeter array providing high-resolution spectroscopic imaging and a deployable high efficiency grating spectrometer. AXSIO delivers a 30-fold increase in effective area for high resolution spectroscopy. The key simplifications are guided by recommendations in the NWNH panel report include a reduction in focal length from 20m to 10m, eliminating the extendable optical bench, and a reduction in the instrument complement from six to two, avoiding a movable instrument platform. A focus on spectroscopic science allows the spatial resolution requirement to be relaxed to 10 arc sec (with a 5 arc sec goal). These simplifications decrease the total mission cost to under the $2B cost to NASA recommended by NWNH. AXSIO will be available to the entire astronomical community with observing allocations based on peer-review.

Design and performance of an X-ray scanning microscope at the Hard X-ray Nanoprobe beamline of NSLS-II

DOE PAGES

Nazaretski, E.; Yan, H.; Lauer, K.; ...

2017-10-05

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ~15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature ofmore » a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.« less

Design and performance of an X-ray scanning microscope at the Hard X-ray Nanoprobe beamline of NSLS-II

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nazaretski, E.; Yan, H.; Lauer, K.

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ~15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature ofmore » a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.« less

Photon-in photon-out hard X-ray spectroscopy at the Linac Coherent Light Source

DOE PAGES

Alonso-Mori, Roberto; Sokaras, Dimosthenis; Zhu, Diling; ...

2015-04-15

X-ray free-electron lasers (FELs) have opened unprecedented possibilities to study the structure and dynamics of matter at an atomic level and ultra-fast timescale. Many of the techniques routinely used at storage ring facilities are being adapted for experiments conducted at FELs. In order to take full advantage of these new sources several challenges have to be overcome. They are related to the very different source characteristics and its resulting impact on sample delivery, X-ray optics, X-ray detection and data acquisition. Here it is described how photon-in photon-out hard X-ray spectroscopy techniques can be applied to study the electronic structure andmore » its dynamics of transition metal systems with ultra-bright and ultra-short FEL X-ray pulses. In particular, some of the experimental details that are different compared with synchrotron-based setups are discussed and illustrated by recent measurements performed at the Linac Coherent Light Source.« less

Scanning three-dimensional x-ray diffraction microscopy using a high-energy microbeam

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hayashi, Y., E-mail: y-hayashi@mosk.tytlabs.co.jp; Hirose, Y.; Seno, Y.

2016-07-27

A scanning three-dimensional X-ray diffraction (3DXRD) microscope apparatus with a high-energy microbeam was installed at the BL33XU Toyota beamline at SPring-8. The size of the 50 keV beam focused using Kirkpatrick-Baez mirrors was 1.3 μm wide and 1.6 μm high in full width at half maximum. The scanning 3DXRD method was tested for a cold-rolled carbon steel sheet sample. A three-dimensional orientation map with 37 {sup 3} voxels was obtained.

Quantitative X-ray dark-field and phase tomography using single directional speckle scanning technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Hongchang, E-mail: hongchang.wang@diamond.ac.uk; Kashyap, Yogesh; Sawhney, Kawal

2016-03-21

X-ray dark-field contrast tomography can provide important supplementary information inside a sample to the conventional absorption tomography. Recently, the X-ray speckle based technique has been proposed to provide qualitative two-dimensional dark-field imaging with a simple experimental arrangement. In this letter, we deduce a relationship between the second moment of scattering angle distribution and cross-correlation degradation of speckle and establish a quantitative basis of X-ray dark-field tomography using single directional speckle scanning technique. In addition, the phase contrast images can be simultaneously retrieved permitting tomographic reconstruction, which yields enhanced contrast in weakly absorbing materials. Such complementary tomography technique can allow systematicmore » investigation of complex samples containing both soft and hard materials.« less

Hydrothermal Diamond Anvil Cell (HDAC): From Visual Observation to X-ray Absorption Spectroscopy

NASA Astrophysics Data System (ADS)

Bassett, W. A.; Mibe, K.

2006-05-01

A fluid sample contained in a Re gasket between two diamond anvils can be subjected to pressures up to 2.5 GPa and temperatures up to 1200°C in a resistively heated hydrothermal diamond anvil cell (HDAC). Thermocouples are used to measure temperature. The constant-volume sample chamber permits isochoric measurements that can be used to determine pressure from the equation of state of H2O and to map phases and properties in P-T space. A movie of reactions between K-feldspar and water up to 2.5 GPa and 880°C illustrates the use of visual observations for mapping coexisting solution, melt, and solid phases. X-ray absorption spectroscopy of ZnBr2 in solution up to 500°C and 500 MPa shows hydrogen bond breaking in the hydration shells of the ZnBr42- and Br- ions with increasing temperature. In other studies the stability field of ikaite (CaCO3·6H2O) has been mapped by visual observation and Raman spectroscopy; the phases of montmorillonite have been mapped by X-ray diffraction; and the leaching of Pb from zircon has been measured by X-ray microprobe.

Wavefront metrology for coherent hard X-rays by scanning a microsphere.

PubMed

Skjønsfjell, Eirik Torbjørn Bakken; Chushkin, Yuriy; Zontone, Federico; Patil, Nilesh; Gibaud, Alain; Breiby, Dag W

2016-05-16

Characterization of the wavefront of an X-ray beam is of primary importance for all applications where coherence plays a major role. Imaging techniques based on numerically retrieving the phase from interference patterns are often relying on an a-priori assumption of the wavefront shape. In Coherent X-ray Diffraction Imaging (CXDI) a planar incoming wave field is often assumed for the inversion of the measured diffraction pattern, which allows retrieving the real space image via simple Fourier transformation. It is therefore important to know how reliable the plane wave approximation is to describe the real wavefront. Here, we demonstrate that the quantitative wavefront shape and flux distribution of an X-ray beam used for CXDI can be measured by using a micrometer size metal-coated polymer sphere serving in a similar way as the hole array in a Hartmann wavefront sensor. The method relies on monitoring the shape and center of the scattered intensity distribution in the far field using a 2D area detector while raster-scanning the microsphere with respect to the incoming beam. The reconstructed X-ray wavefront was found to have a well-defined central region of approximately 16 µm diameter and a weaker, asymmetric, intensity distribution extending 30 µm from the beam center. The phase front distortion was primarily spherical with an effective radius of 0.55 m which matches the distance to the last upstream beam-defining slit, and could be accurately represented by Zernike polynomials.

Characterization of aluminum nitride based films with high resolution X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Anagnostopoulos, D. F.; Siozios, A.; Patsalas, P.

2018-02-01

X-ray fluorescence spectra of Al based films are measured, using a lab-scale wavelength dispersive flat crystal spectrometer. Various structures of AlN films were studied, like single layered, capped, stratified, nanostructured, crystalline, or amorphous. By optimizing the set-up for enhanced energy resolution and detection efficiency, the measured line shapes of Κα, Kβ, and KLL radiative Auger transitions are shown to be adequately detailed to allow chemical characterization. The chemistry identification is based on the pattern comparison of the emitted line shape from the chemically unknown film and the reference line shapes from standard materials, recorded under identical experimental conditions. The ultimate strength of lab-scale high resolution X-ray fluorescence spectroscopy on film analysis is verified, in cases that ordinary applied techniques like X-ray photoelectron and X-ray diffraction fail, while the characterization refers to the non-destructive determination of the bulk properties of the film and not to its surface, as the probed depth is in the micrometer range.

Nanoscopium: a Scanning Hard X-ray Nanoprobe Beamline at Synchrotron Soleil

NASA Astrophysics Data System (ADS)

Somogyi, A.; Polack, F.; Moreno, T.

2010-06-01

Nanoscopium is the single scanning hard X-ray nano-probe beamline planned at SOLEIL. This ˜155 m long beamline will fully exploit the high brilliance and coherence characteristics of the X-ray beam both for diffraction limited focusing and for contrast formation. It will offer the most advanced imaging techniques in multimodal mode and will be a research tool for a wide user community working in the fields of earth-, environmental-, and life-sciences. The different μ-μnano-probe techniques offered by the beamline will permit elemental mapping at trace (ppm) levels (scanning XRF), speciation mapping (XANES), phase gradient mapping (scanning differential phase contrast), and density-contrast based imaging of internal structures (coherent diffraction imaging) in the 30 nm to 1 μm spatial resolution range, also in "in situ conditions". Nanoscopium will cover the 5-20 keV energy range. The stability of the nanobeam will be ensured by horizontally reflecting beamline optics (a sagitally and a tangentially pre-focusing mirror, horizontally reflecting monochromators) in front of the overfilled secondary source. Trade-off between high energy resolution (ΔE/E˜10-4) and high flux (1011 ph/s with ΔE/E˜10-2) will be achieved by two interchangeable monochromators (a double crystal and a double multilayer one). KB mirror and FZP lenses will be used as focusing devices. The beamline is in the design and construction phase. It is foreseen to be open for users at the beginning of 2013.

X-ray ptychography

NASA Astrophysics Data System (ADS)

Pfeiffer, Franz

2018-01-01

X-ray ptychographic microscopy combines the advantages of raster scanning X-ray microscopy with the more recently developed techniques of coherent diffraction imaging. It is limited neither by the fabricational challenges associated with X-ray optics nor by the requirements of isolated specimen preparation, and offers in principle wavelength-limited resolution, as well as stable access and solution to the phase problem. In this Review, we discuss the basic principles of X-ray ptychography and summarize the main milestones in the evolution of X-ray ptychographic microscopy and tomography over the past ten years, since its first demonstration with X-rays. We also highlight the potential for applications in the life and materials sciences, and discuss the latest advanced concepts and probable future developments.

Dual crystal x-ray spectrometer at 1.8 keV for high repetition-rate single-photon counting spectroscopy experiments

DOE PAGES

Gamboa, E. J.; Bachmann, B.; Kraus, D.; ...

2016-08-01

The recent development of high-repetition rate x-ray free electron lasers (FEL), makes it possible to perform x-ray scattering and emission spectroscopy measurements from thin foils or gasses heated to high-energy density conditions by integrating over many experimental shots. Since the expected signal may be weaker than the typical CCD readout noise over the region-of-interest, it is critical to the success of this approach to use a detector with high-energy resolution so that single x-ray photons may be isolated. We describe a dual channel x-ray spectrometer developed for the Atomic and Molecular Optics endstation at the Linac Coherent Light Source (LCLS)more » for x-ray spectroscopy near the K-edge of aluminum. The spectrometer is based on a pair of curved PET (002) crystals coupled to a single pnCCD detector which simultaneously measures x-ray scattering and emission in the forward and backward directions. Furthermore, the signals from single x-ray photons are accumulated permitting continuous single-shot acquisition at 120 Hz.« less

X-ray ptychographic and fluorescence microscopy of frozen-hydrated cells using continuous scanning

DOE PAGES

Deng, Junjing; Vine, David J.; Chen, Si; ...

2017-03-27

X-ray microscopy can be used to image whole, unsectioned cells in their native hydrated state. It complements the higher resolution of electron microscopy for submicrometer thick specimens, and the molecule-specific imaging capabilites of fluorescence light microscopy. We describe here the first use of fast, continuous x-ray scanning of frozen hydrated cells for simultaneous sub-20 nm resolution ptychographic transmission imaging with high contrast, and sub-100 nm resolution deconvolved x-ray fluorescence imaging of diffusible and bound ions at native concentrations, without the need to add specific labels. Here, by working with cells that have been rapidly frozen without the use of chemicalmore » fixatives, and imaging them under cryogenic conditions, we are able to obtain images with well preserved structural and chemical composition, and sufficient stability against radiation damage to allow for multiple images to be obtained with no observable change.« less

Composition Analysis of III-Nitrides at the Nanometer Scale: Comparison of Energy Dispersive X-ray Spectroscopy and Atom Probe Tomography.

PubMed

Bonef, Bastien; Lopez-Haro, Miguel; Amichi, Lynda; Beeler, Mark; Grenier, Adeline; Robin, Eric; Jouneau, Pierre-Henri; Mollard, Nicolas; Mouton, Isabelle; Monroy, Eva; Bougerol, Catherine

2016-12-01

The enhancement of the performance of advanced nitride-based optoelectronic devices requires the fine tuning of their composition, which has to be determined with a high accuracy and at the nanometer scale. For that purpose, we have evaluated and compared energy dispersive X-ray spectroscopy (EDX) in a scanning transmission electron microscope (STEM) and atom probe tomography (APT) in terms of composition analysis of AlGaN/GaN multilayers. Both techniques give comparable results with a composition accuracy better than 0.6 % even for layers as thin as 3 nm. In case of EDX, we show the relevance of correcting the X-ray absorption by simultaneous determination of the mass thickness and chemical composition at each point of the analysis. Limitations of both techniques are discussed when applied to specimens with different geometries or compositions.

High resolution X- and gamma-ray spectroscopy of cosmic X-ray sources

NASA Technical Reports Server (NTRS)

Lin, R. P.

1983-01-01

A high resolution X-ray spectrometer and large area phoswich detector were designed and co-aligned in a common elevation mounting in order to measure solar and cosmic X-ray and gamma ray emission in the 13 to 600 KeV energy range from a balloon. The instrument is described and results obtained for the Crab Nebula, the supernova remnant Cas A, and the Sun are discussed and analyzed.

X-ray diffraction, IR spectroscopy and thermal characterization of partially hydrolyzed guar gum.

PubMed

Mudgil, Deepak; Barak, Sheweta; Khatkar, B S

2012-05-01

Guar gum was hydrolyzed using cellulase from Aspergillus niger at 5.6 pH and 50°C temperature. Hydrolyzed guar gum sample was characterized using Fourier transform infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis, X-ray diffraction, dilute solution viscometry and rotational viscometry. Viscometry analysis of native guar gum showed a molecular weight of 889742.06, whereas, after enzymatic hydrolysis, the resultant product had a molecular weight of 7936.5. IR spectral analysis suggests that after enzymatic hydrolysis of guar gum there was no major transformation of functional group. Thermal analysis revealed no major change in thermal behavior of hydrolyzed guar gum. It was shown that partial hydrolysis of guar gum could be achieved by inexpensive and food grade cellulase (Aspergillus niger) having commercial importance and utilization as a functional soluble dietary fiber for food industry. Copyright © 2012 Elsevier B.V. All rights reserved.

Near-edge x-ray absorption fine structure spectroscopy at atmospheric pressure with a table-top laser-induced soft x-ray source

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kühl, Frank-Christian, E-mail: Frank-christian.kuehl@mail.de; Müller, Matthias, E-mail: matthias.mueller@llg-ev.de; Schellhorn, Meike

2016-07-15

The authors present a table-top soft x-ray absorption spectrometer, accomplishing investigations of the near-edge x-ray absorption fine structure (NEXAFS) in a laboratory environment. The system is based on a low debris plasma ignited by a picosecond laser in a pulsed krypton gas jet, emitting soft x-ray radiation in the range from 1 to 5 nm. For absorption spectroscopy in and around the “water window” (2.3–4.4 nm), a compact helium purged sample compartment for experiments at atmospheric pressure has been constructed and tested. NEXAFS measurements on CaCl{sub 2} and KMnO{sub 4} samples were conducted at the calcium and manganese L-edges, as well asmore » at the oxygen K-edge in air, atmospheric helium, and under vacuum, respectively. The results indicate the importance of atmospheric conditions for an investigation of sample hydration processes.« less

Annealing induced atomic rearrangements on (Ga,In) (N,As) probed by hard X-ray photoelectron spectroscopy and X-ray absorption fine structure.

PubMed

Ishikawa, Fumitaro; Higashi, Kotaro; Fuyuno, Satoshi; Morifuji, Masato; Kondow, Masahiko; Trampert, Achim

2018-04-13

We study the effects of annealing on (Ga 0.64 ,In 0.36 ) (N 0.045 ,As 0.955 ) using hard X-ray photoelectron spectroscopy and X-ray absorption fine structure measurements. We observed surface oxidation and termination of the N-As bond defects caused by the annealing process. Specifically, we observed a characteristic chemical shift towards lower binding energies in the photoelectron spectra related to In. This phenomenon appears to be caused by the atomic arrangement, which produces increased In-N bond configurations within the matrix, as indicated by the X-ray absorption fine structure measurements. The reduction in the binding energies of group-III In, which occurs concomitantly with the atomic rearrangements of the matrix, causes the differences in the electronic properties of the system before and after annealing.

X-Ray Absorption near Edge Structure Spectroscopy of Nanodiamonds from the Allende Meteorite

NASA Technical Reports Server (NTRS)

Flynn, G. J.; Keller, L. P.; Hill, H.; Jacobsen, C.; Wirick, S.

2000-01-01

Carbon X-ray Absorption Near Edge Structure Spectroscopy shows Allende DM nanodiamonds have two pre-edge peaks, consistent with other small diamonds, but fail to show a diamond exciton which is seen in 3.6 nm diamond thin films.

What can be Learned from X-ray Spectroscopy Concerning Hot Gas in Local Bubble and Charge Exchange Processes?

NASA Technical Reports Server (NTRS)

Snowden, Steve

2007-01-01

What can be learned from x-ray spectroscopy in observing hot gas in local bubble and charge exchange processes depends on spectral resolution, instrumental grasp, instrumental energy band, signal-to-nose, field of view, angular resolution and observatory location. Early attempts at x-ray spectroscopy include ROSAT; more recently, astronomers have used diffuse x-ray spectrometers, XMM Newton, sounding rocket calorimeters, and Suzaku. Future observations are expected with calorimeters on the Spectrum Roentgen Gamma mission, and the Solar Wind Charge Exchange (SWCX). The Geospheric SWCX may provide remote sensing of the solar wind and magnetosheath and remote observations of solar CMEs moving outward from the sun.

Diagnosis of electrocution: The application of scanning electron microscope and energy-dispersive X-ray spectroscopy in five cases.

PubMed

Visonà, S D; Chen, Y; Bernardi, P; Andrello, L; Osculati, A

2018-03-01

Deaths from electricity, generally, do not have specific findings at the autopsy. The diagnosis is commonly based on the circumstances of the death and the morphologic findings, above all the current mark. Yet, the skin injury due to an electrocution and other kinds of thermal injuries often cannot be differentiated with certainty. Therefore, there is a great interest in finding specific markers of electrocution. The search for the metallization of the skin through Scanning Electron Microscope equipped with Energy Dispersive X-Ray Spectroscopy (EDS) probe is of special importance in order to achieve a definite diagnosis in case of suspected electrocution. We selected five cases in which the electrocution was extremely likely considering the circumstances of the death. In each case a forensic autopsy was performed. Then, the skin specimens were stained with Hematoxylin Eosin and Perls. On the other hand, the skin lesions were examined with a scanning electron microscope equipped with EDS probe in order to evaluate the morphological ultrastructural features and the presence of deposits on the surface of the skin. The typical skin injury of the electrocution (current mark) were macroscopically detected in all of the cases. The microscopic examination of the skin lesions revealed the typical spherical vacuoles in the horny layer and, in the epidermis, the elongation of the cell nuclei as well as necrosis. Perls staining was negative in 4 out 6 cases. Ultrastructural morphology revealed the evident vacuolization of the horny layer, elongation of epidermic cells, coagulation of the elastic fibers. In the specimens collected from the site of contact with the conductor of case 1 and 2, the presence of the Kα peaks of iron was detected. In the corresponding specimens taken from cases 2, 4, 5 the microanalysis showed the Kα peaks of titanium. In case 3, titanium and carbon were found. In the suspicion of electrocution, the integrated use of different tools is recommended

Optical Metrology for the Segmented Optics on the Constellation-X Spectroscopy X-Ray Telescope

NASA Technical Reports Server (NTRS)

Content, David; Colella, David; Fleetwood, Charles; Hadjimichael, Theo; Lehan, John; McMann, Joseph; Reid, Paul; Saha, Timo; Wright, Geraldine; Zhang, William

2004-01-01

We present the metrology requirements and metrology implementation necessary to prove out the reflector technology for the Constellation X(C-X) spectroscopy X-ray telescope (SXT). This segmented, 1.6m diameter highly nested Wolter-1 telescope presents many metrology and alignment challenges. In particular, these mirrors have a stringent imaging error budget as compared to their intrinsic stiffness; This is required for Constellation-X to have sufficient effective area with the weight requirement. This has implications for the metrology that can be used. A variety of contract and noncontact optical profiling and interferometric methods are combined to test the formed glass substrates before replication and the replicated reflector segments.The reflectors are tested both stand-alone and in-situ in an alignment tower.Some of these methods have not been used on prior X-ray telescopes and some are feasible only because of the segmented approach used on the SXT. Methods discussed include high precision coordinate measurement machines using very low force or optical probe axial interferometric profiling azimuthal circularity profiling and use of advanced null optics such as conical computer generated hologram (CGHs).

Grid-enhanced X-ray coded aperture microscopy with polycapillary optics

PubMed Central

Sowa, Katarzyna M.; Last, Arndt; Korecki, Paweł

2017-01-01

Polycapillary devices focus X-rays by means of multiple reflections of X-rays in arrays of bent glass capillaries. The size of the focal spot (typically 10–100 μm) limits the resolution of scanning, absorption and phase-contrast X-ray imaging using these devices. At the expense of a moderate resolution, polycapillary elements provide high intensity and are frequently used for X-ray micro-imaging with both synchrotrons and X-ray tubes. Recent studies have shown that the internal microstructure of such an optics can be used as a coded aperture that encodes high-resolution information about objects located inside the focal spot. However, further improvements to this variant of X-ray microscopy will require the challenging fabrication of tailored devices with a well-defined capillary microstructure. Here, we show that submicron coded aperture microscopy can be realized using a periodic grid that is placed at the output surface of a polycapillary optics. Grid-enhanced X-ray coded aperture microscopy with polycapillary optics does not rely on the specific microstructure of the optics but rather takes advantage only of its focusing properties. Hence, submicron X-ray imaging can be realized with standard polycapillary devices and existing set-ups for micro X-ray fluorescence spectroscopy. PMID:28322316

Grid-enhanced X-ray coded aperture microscopy with polycapillary optics.

PubMed

Sowa, Katarzyna M; Last, Arndt; Korecki, Paweł

2017-03-21

Polycapillary devices focus X-rays by means of multiple reflections of X-rays in arrays of bent glass capillaries. The size of the focal spot (typically 10-100 μm) limits the resolution of scanning, absorption and phase-contrast X-ray imaging using these devices. At the expense of a moderate resolution, polycapillary elements provide high intensity and are frequently used for X-ray micro-imaging with both synchrotrons and X-ray tubes. Recent studies have shown that the internal microstructure of such an optics can be used as a coded aperture that encodes high-resolution information about objects located inside the focal spot. However, further improvements to this variant of X-ray microscopy will require the challenging fabrication of tailored devices with a well-defined capillary microstructure. Here, we show that submicron coded aperture microscopy can be realized using a periodic grid that is placed at the output surface of a polycapillary optics. Grid-enhanced X-ray coded aperture microscopy with polycapillary optics does not rely on the specific microstructure of the optics but rather takes advantage only of its focusing properties. Hence, submicron X-ray imaging can be realized with standard polycapillary devices and existing set-ups for micro X-ray fluorescence spectroscopy.

Quantitative Phase Composition of TiO 2-Coated Nanoporous-Au Monoliths by X-ray Absorption Spectroscopy and Correlations to Catalytic

DOE PAGES

Bagge-Hansen, Michael; Wichmann, Andre; Wittstock, Arne; ...

2014-02-03

Porous titania/metal composite materials have many potential applications in the fields of green catalysis, energy harvesting, and storage in which both the overall morphology of the nanoporous host material and the crystallographic phase of the titania (TiO 2) guest determine the material’s performance. New insights into the structure–function relationships of these materials were obtained by near-edge X-ray absorption fine structure (NEXAFS) spectroscopy that, for example, provides quantitative crystallographic phase composition from ultrathin, nanostructured titania films, including sensitivity to amorphous components. We demonstrate that crystallographic phase, morphology, and catalytic activity of TiO 2-functionalized nanoporous gold (np-Au) can be controlled by amore » simple annealing procedure (T < 1300 K). The material was prepared by atomic layer deposition of ~2 nm thick TiO 2 on millimeter-sized samples of np-Au (40–50 nm mean ligament size) and catalytically investigated with respect to aerobic CO oxidation. Moreover, the annealing-induced changes in catalytic activity are correlated with concurrent morphology and phase changes as provided by cross-sectional scanning electron microscopy, transmission electron microscopy, and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy.« less

X-ray Emission Spectroscopy of Biomimetic Mn Coordination Complexes.

PubMed

Jensen, Scott C; Davis, Katherine M; Sullivan, Brendan; Hartzler, Daniel A; Seidler, Gerald T; Casa, Diego M; Kasman, Elina; Colmer, Hannah E; Massie, Allyssa A; Jackson, Timothy A; Pushkar, Yulia

2017-06-15

Understanding the function of Mn ions in biological and chemical redox catalysis requires precise knowledge of their electronic structure. X-ray emission spectroscopy (XES) is an emerging technique with a growing application to biological and biomimetic systems. Here, we report an improved, cost-effective spectrometer used to analyze two biomimetic coordination compounds, [Mn IV (OH) 2 (Me 2 EBC)] 2+ and [Mn IV (O)(OH)(Me 2 EBC)] + , the second of which contains a key Mn IV ═O structural fragment. Despite having the same formal oxidation state (Mn IV ) and tetradentate ligands, XES spectra from these two compounds demonstrate different electronic structures. Experimental measurements and DFT calculations yield different localized spin densities for the two complexes resulting from Mn IV -OH conversion to Mn IV ═O. The relevance of the observed spectroscopic changes is discussed for applications in analyzing complex biological systems such as photosystem II. A model of the S 3 intermediate state of photosystem II containing a Mn IV ═O fragment is compared to recent time-resolved X-ray diffraction data of the same state.

Clocking Femtosecond Collisional Dynamics via Resonant X-Ray Spectroscopy

DOE PAGES

van den Berg, Q. Y.; Fernandez-Tello, E. V.; Burian, T.; ...

2018-02-01

Electron-ion collisional dynamics is of fundamental importance in determining plasma transport properties, nonequilibrium plasma evolution, and electron damage in diffraction imaging applications using bright x-ray free-electron lasers (FELs). Here in this paper, we describe the first experimental measurements of ultrafast electron impact collisional ionization dynamics using resonant core-hole spectroscopy in a solid-density magnesium plasma, created and diagnosed with the Linac Coherent Light Source x-ray FEL. By resonantly pumping the 1s → 2p transition in highly charged ions within an optically thin plasma, we have measured how off-resonance charge states are populated via collisional processes on femtosecond time scales. We presentmore » a collisional cross section model that matches our results and demonstrates how the cross sections are enhanced by dense-plasma effects including continuum lowering. Nonlocal thermodynamic equilibrium collisional radiative simulations show excellent agreement with the experimental results and provide new insight on collisional ionization and three-body-recombination processes in the dense-plasma regime.« less

Prediction of Ba, Co and Ni for tropical soils using diffuse reflectance spectroscopy and X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Arantes Camargo, Livia; Marques Júnior, José; Reynaldo Ferracciú Alleoni, Luís; Tadeu Pereira, Gener; De Bortoli Teixeira, Daniel; Santos Rabelo de Souza Bahia, Angélica

2017-04-01

Environmental impact assessments may be assisted by spatial characterization of potentially toxic elements (PTEs). Diffuse reflectance spectroscopy (DRS) and X-ray fluorescence spectroscopy (XRF) are rapid, non-destructive, low-cost, prediction tools for a simultaneous characterization of different soil attributes. Although low concentrations of PTEs might preclude the observation of spectral features, their contents can be predicted using spectroscopy by exploring the existing relationship between the PTEs and soil attributes with spectral features. This study aimed to evaluate, in three geomorphic surfaces of Oxisols, the capacity for predicting PTEs (Ba, Co, and Ni) and their spatial variability by means of diffuse reflectance spectroscopy (DRS) and X-ray fluorescence spectroscopy (XRF). For that, soil samples were collected from three geomorphic surfaces and analyzed for chemical, physical, and mineralogical properties, and then analyzed in DRS (visible + near infrared - VIS+NIR and medium infrared - MIR) and XRF equipment. PTE prediction models were calibrated using partial least squares regression (PLSR). PTE spatial distribution maps were built using the values calculated by the calibrated models that reached the best accuracy using geostatistics. PTE prediction models were satisfactorily calibrated using MIR DRS for Ba, and Co (residual prediction deviation - RPD > 3.0), Vis DRS for Ni (RPD > 2.0) and FRX for all the studied PTEs (RPD > 1.8). DRS- and XRF-predicted values allowed the characterization and the understanding of spatial variability of the studied PTEs.

X-ray absorption spectroscopy investigations on oxidized Ni/Au contacts to p-GaN.

PubMed

Jan, J C; Asokan, K; Chiou, J W; Pong, W F; Tseng, P K; Chen, L C; Chen, F R; Lee, J F; Wu, J S; Lin, H J; Chen, C T

2001-03-01

X-ray absorption spectroscopy was used to investigate the electronic structure of as-deposited and oxidized Ni/Au contacts to p-GaN and to elucidate the mechanism responsible for low impedance. X-ray absorption near edge spectra of Ni K- and L3,2-edges clearly indicate formation of NiO on the sample surface after annealing. The reason for low impedance may be attributed to increase in hole concentration and existence of p-NiO layer on the surface.

Diagnosis of a two wire X-pinch by X-ray absorption spectroscopy utilizing a doubly curved ellipsoidal crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cahill, A. D., E-mail: adc87@cornell.edu; Hoyt, C. L., E-mail: adc87@cornell.edu; Shelkovenko, T. A., E-mail: adc87@cornell.edu

2014-12-15

X-ray absorption spectroscopy is a powerful tool for the diagnosis of plasmas over a wide range of both temperature and density. However, such a measurement is often limited to probing plasmas with temperatures well below that of the x-ray source in order to avoid object plasma emission lines from obscuring important features of the absorption spectrum. This has excluded many plasmas from being investigated by this technique. We have developed an x-ray spectrometer that provides the ability to record absorption spectra from higher temperature plasmas than the usual approach allows without the risk of data contamination by line radiation emittedmore » by the plasma under study. This is accomplished using a doubly curved mica crystal which is bent both elliptically and cylindrically. We present here initial absorption spectra obtained from an aluminum x-pinch plasma.« less

Ultrafast X-Ray Absorption Spectroscopy of Isochorically Heated Warm Dense Matter

NASA Astrophysics Data System (ADS)

Engelhorn, Kyle Craig

This dissertation will present a series of new tools, together with new techniques, focused on the understanding of warm and dense matter. We report on the development of a high time resolution and high detection efficiency x-ray camera. The camera is integrated with a short pulse laser and an x-ray beamline at the Advanced Light Source synchrotron. This provides an instrument for single shot, broadband x-ray absorption spectroscopy of warm and dense matter with 2 picosecond time resolution. Warm and dense matter is created by isochorically heating samples of known density with an ultrafast optical laser pulse, and X-ray absorption spectroscopy probes the unoccupied electronic density of states before the onset of hydrodynamic expansion and electron-ion equilibrium is reached. Measured spectra from a variety of materials are compared with first principle molecular dynamics and density functional theory calculations. In heated silicon dioxide spectra, two novel pre-edge features are observed, a peak below the band gap and absorption within the band gap, while a reduction was observed in the features above the edge. From consideration of the calculated spectra, the peak below the gap is attributed to valence electrons that have been promoted to the conduction band, the absorption within the gap is attributed to broken Si-O bonds, and the reduction above the edge is attributed to an elevated ionic temperature. In heated copper spectra, a time-dependent shift and broadening of the absorption edge are observed, consistent with and elevated electron temperature. The temporal evolution of the electronic temperature is accurately determined by fitting the measured spectra with calculated spectra. The electron-ion equilibration is studied with a two-temperature model. In heated nickel spectra, a shift of the absorption edge is observed. This shift is found to be inconsistent with calculated spectra and independent of incident laser fluence. A shift of the chemical potential

The X-ray Astronomy Recovery Mission

NASA Astrophysics Data System (ADS)

Tashiro, M.; Kelley, R.

2017-10-01

On 25 March 2016, the Japanese 6th X-ray astronomical satellite ASTRO-H (Hitomi), launched on February 17, lost communication after a series of mishap in its attitude control system. In response to the mishap the X-ray astronomy community and JAXA analyzed the direct and root cause of the mishap and investigated possibility of a recovery mission with the international collaborator NASA and ESA. Thanks to great effort of scientists, agencies, and governments, the X-ray Astronomy Recovery Mission (XARM) are proposed. The recovery mission is planned to resume high resolution X-ray spectroscopy with imaging realized by Hitomi under the international collaboration in the shortest time possible, simply by focusing one of the main science goals of Hitomi Resolving astrophysical problems by precise high-resolution X-ray spectroscopy'. XARM will carry a 6 x 6 pixelized X-ray micro-calorimeter on the focal plane of an X-ray mirror assembly, and an aligned X-ray CCD camera covering the same energy band and wider field of view, but no hard X-ray or soft gamma-ray instruments are onboard. In this paper, we introduce the science objectives, mission concept, and schedule of XARM.

Revealing hole trapping in zinc oxide nanoparticles by time-resolved X-ray spectroscopy

DOE PAGES

Penfold, Thomas J.; Szlachetko, Jakub; Santomauro, Fabio G.; ...

2018-02-02

Nanostructures of transition metal oxides (TMO), such as ZnO, have attracted considerable interest for solar-energy conversion and photocatalysis. For the latter, trapping of charge carriers has an essential role. The probing of electron trapping in the conduction band of room temperature photoexcited TMOs has recently become possible owing to the emergence of time-resolved element-sensitive methods, such as X-ray spectroscopy. However, because the valence band of TMOs is dominated by the oxygen 2p orbitals,holes have so far escaped observation. Herein we use a novel dispersive X-ray emission spectrometer combined with X-ray absorption spectroscopy to directly probe the charge carrier relaxation andmore » trapping pro-cesses in ZnO nanoparticles after above band-gap photoexcitation. Here, our results, supported by simulations, demonstrate that within our temporal resolution of 80 ps, photo-excited holes are trapped at singly charged oxygen vacancies, turning them into doubly charged vacancies, which causes an outward displacement by approximately 15% of the four surrounding Zn atoms away from the central vacancy. These traps recombine radiatively with the delocalised electrons of the conduction band yielding the commonly observed green luminescence. This identification of the hole traps and their evolution provides new insight for future developments of TMO-based nanodevices.« less

Revealing hole trapping in zinc oxide nanoparticles by time-resolved X-ray spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Penfold, Thomas J.; Szlachetko, Jakub; Santomauro, Fabio G.

Nanostructures of transition metal oxides (TMO), such as ZnO, have attracted considerable interest for solar-energy conversion and photocatalysis. For the latter, trapping of charge carriers has an essential role. The probing of electron trapping in the conduction band of room temperature photoexcited TMOs has recently become possible owing to the emergence of time-resolved element-sensitive methods, such as X-ray spectroscopy. However, because the valence band of TMOs is dominated by the oxygen 2p orbitals,holes have so far escaped observation. Herein we use a novel dispersive X-ray emission spectrometer combined with X-ray absorption spectroscopy to directly probe the charge carrier relaxation andmore » trapping pro-cesses in ZnO nanoparticles after above band-gap photoexcitation. Here, our results, supported by simulations, demonstrate that within our temporal resolution of 80 ps, photo-excited holes are trapped at singly charged oxygen vacancies, turning them into doubly charged vacancies, which causes an outward displacement by approximately 15% of the four surrounding Zn atoms away from the central vacancy. These traps recombine radiatively with the delocalised electrons of the conduction band yielding the commonly observed green luminescence. This identification of the hole traps and their evolution provides new insight for future developments of TMO-based nanodevices.« less

New Optimizations of Microcalorimeter Arrays for High-Resolution Imaging X-ray Spectroscopy

NASA Astrophysics Data System (ADS)

Kilbourne, Caroline

We propose to continue our successful research program in developing arrays of superconducting transition-edge sensors (TES) for x-ray astrophysics. Our standard 0.3 mm TES pixel achieves better than 2.5-eV resolution, and we now make 32x32 arrays of such pixels. We have also achieved better than 1-eV resolution in smaller pixels, and promising performance in a range of position-sensitive designs. We propose to continue to advance the designs of both the single-pixel and position-sensitive microcalorimeters so that we can produce arrays suitable for several x-ray spectroscopy observatories presently in formulation. We will also investigate various array and pixel optimizations such as would be needed for large arrays for surveys, large- pixel arrays for diffuse soft x-ray measurements, or sub-arrays of fast pixels optimized for neutron-star burst spectroscopy. In addition, we will develop fabrication processes for integrating sub-arrays with very different pixel designs into a monolithic focal-plane array to simplify the design of the focal-plane assembly and make feasible new detector configurations such as the one currently baselined for AXSIO. Through a series of measurements on test devices, we have improved our understanding of the weak-link physics governing the observed resistive transitions in TES detectors. We propose to build on that work and ultimately use the results to improve the immunity of the detector to environmental magnetic fields, as well as its fundamental performance, in each of the targeted optimizations we are developing.

Scanning transmission X-ray, laser scanning, and transmission electron microscopy mapping of the exopolymeric matrix of microbial biofilms.

PubMed

Lawrence, J R; Swerhone, G D W; Leppard, G G; Araki, T; Zhang, X; West, M M; Hitchcock, A P

2003-09-01

Confocal laser scanning microscopy (CLSM), transmission electron microscopy (TEM), and soft X-ray scanning transmission X-ray microscopy (STXM) were used to map the distribution of macromolecular subcomponents (e.g., polysaccharides, proteins, lipids, and nucleic acids) of biofilm cells and matrix. The biofilms were developed from river water supplemented with methanol, and although they comprised a complex microbial community, the biofilms were dominated by heterotrophic bacteria. TEM provided the highest-resolution structural imaging, CLSM provided detailed compositional information when used in conjunction with molecular probes, and STXM provided compositional mapping of macromolecule distributions without the addition of probes. By examining exactly the same region of a sample with combinations of these techniques (STXM with CLSM and STXM with TEM), we demonstrate that this combination of multimicroscopy analysis can be used to create a detailed correlative map of biofilm structure and composition. We are using these correlative techniques to improve our understanding of the biochemical basis for biofilm organization and to assist studies intended to investigate and optimize biofilms for environmental remediation applications.

Effects of X-Ray Dose On Rhizosphere Studies Using X-Ray Computed Tomography

PubMed Central

Zappala, Susan; Helliwell, Jonathan R.; Tracy, Saoirse R.; Mairhofer, Stefan; Sturrock, Craig J.; Pridmore, Tony; Bennett, Malcolm; Mooney, Sacha J.

2013-01-01

X-ray Computed Tomography (CT) is a non-destructive imaging technique originally designed for diagnostic medicine, which was adopted for rhizosphere and soil science applications in the early 1980s. X-ray CT enables researchers to simultaneously visualise and quantify the heterogeneous soil matrix of mineral grains, organic matter, air-filled pores and water-filled pores. Additionally, X-ray CT allows visualisation of plant roots in situ without the need for traditional invasive methods such as root washing. However, one routinely unreported aspect of X-ray CT is the potential effect of X-ray dose on the soil-borne microorganisms and plants in rhizosphere investigations. Here we aimed to i) highlight the need for more consistent reporting of X-ray CT parameters for dose to sample, ii) to provide an overview of previously reported impacts of X-rays on soil microorganisms and plant roots and iii) present new data investigating the response of plant roots and microbial communities to X-ray exposure. Fewer than 5% of the 126 publications included in the literature review contained sufficient information to calculate dose and only 2.4% of the publications explicitly state an estimate of dose received by each sample. We conducted a study involving rice roots growing in soil, observing no significant difference between the numbers of root tips, root volume and total root length in scanned versus unscanned samples. In parallel, a soil microbe experiment scanning samples over a total of 24 weeks observed no significant difference between the scanned and unscanned microbial biomass values. We conclude from the literature review and our own experiments that X-ray CT does not impact plant growth or soil microbial populations when employing a low level of dose (<30 Gy). However, the call for higher throughput X-ray CT means that doses that biological samples receive are likely to increase and thus should be closely monitored. PMID:23840640

Hard x-ray spectroscopy and imaging by a reflection zone plate in the presence of astigmatism

DOE PAGES

Braig, Christoph; Lochel, Heike; Firsov, Alexander; ...

2015-12-17

Here, the feasibility of an off-axis x-ray reflection zone plate to perform wavelength-dispersive spectroscopy, on-axis point focusing, and two-dimensional imaging is demonstrated by means of one and the same diffractive optical element (DOE) at a synchrotron radiation facility. The resolving power varies between 3 × 10 1 and 4 × 10 2 in the range of 7.6 keV to 9.0 keV, with its maximum at the design energy of 8.3 keV. This result is verified using an adjustable entrance slit, by which horizontal (H) and vertical (V) focusing to 0.85 μm(H) and 1.29 μm(V) is obtained near the sagittal focalmore » plane of the astigmatic configuration. An angular and axial scan proves an accessible field of view of at least 0.6 arcmin × 0.8 arcmin and a focal depth of ±0.86 mm. Supported by the grating efficiency of around 17.5% and a very short pulse elongation, future precision x-ray fluorescence and absorption studies of transition metals at their K-edge on an ultrashort timescale could benefit from our findings.« less

Identification of two hard X-ray emitting Be stars using the HEAO 1 scanning modulation collimator

NASA Technical Reports Server (NTRS)

Steiner, J. E.; Ferrara, A.; Garcia, M.; Patterson, J.; Schwartz, D. A.; Warwick, R. S.; Watson, M. G.; Mcclintock, J. E.

1984-01-01

Using precise positions from the HEAO 1 Scanning Modulation Collimator experiment, two hard X-ray sources, 4U 0728 - 25 = 3A 0726 - 260 and 4U 2206 + 54 = 3A 2206 + 543, are identified with early-type stars. In both cases broad (10 A FWHM) H-alpha emission is detected. The UBV colors suggest that the optical counterparts are main-sequence B0-B2 stars at 2-6 kpc, implying a mean X-ray luminosity of order 10 to the 35th ergs/sq cm s (2-10 keV). The X-ray emission in both cases is highly variable, and it is suggested that they belong to the class of X-ray emitting Be stars, containing a neutron star in a widely separated binary system.

In situ/Operando studies of electrocatalysts using hard X-ray spectroscopy

DOE PAGES

Lassalle-Kaiser, Benedikt; Gul, Sheraz; Kern, Jan; ...

2017-05-02

This review focuses on the use of X-ray absorption and emission spectroscopy techniques using hard X-rays to study electrocatalysts under in situ/operando conditions. The importance and the versatility of methods in the study of electrodes in contact with the electrolytes are described, when they are being cycled through the catalytic potentials during the progress of the oxygen-evolution, oxygen reduction and hydrogen evolution reactions. The catalytic oxygen evolution reaction is illustrated with examples using three oxides, Co, Ni and Mn, and two sulfides, Mo and Co. These are used as examples for the hydrogen evolution reaction. A bimetallic, bifunctional oxygen evolvingmore » and oxygen reducing Ni/Mn oxide is also presented. The various advantages and constraints in the use of these techniques and the future outlook are discussed.« less

Quantitative 3D comparison of biofilm imaged by X-ray micro-tomography and two-photon laser scanning microscopy.

PubMed

Larue, A E; Swider, P; Duru, P; Daviaud, D; Quintard, M; Davit, Y

2018-06-21

Optical imaging techniques for biofilm observation, like laser scanning microscopy, are not applicable when investigating biofilm formation in opaque porous media. X-ray micro-tomography (X-ray CMT) might be an alternative but it finds limitations in similarity of X-ray absorption coefficients for the biofilm and aqueous phases. To overcome this difficulty, barium sulphate was used in Davit et al. (2011) to enable high-resolution 3D imaging of biofilm via X-ray CMT. However, this approach lacks comparison with well-established imaging methods, which are known to capture the fine structures of biofilms, as well as uncertainty quantification. Here, we compare two-photon laser scanning microscopy (TPLSM) images of Pseudomonas Aeruginosa biofilm grown in glass capillaries against X-ray CMT using an improved protocol where barium sulphate is combined with low-gelling temperature agarose to avoid sedimentation. Calibrated phantoms consisting of mono-dispersed fluorescent and X-ray absorbent beads were used to evaluate the uncertainty associated with our protocol along with three different segmentation techniques, namely hysteresis, watershed and region growing, to determine the bias relative to image binarization. Metrics such as volume, 3D surface area and thickness were measured and comparison of both imaging modalities shows that X-ray CMT of biofilm using our protocol yields an accuracy that is comparable and even better in certain respects than TPLSM, even in a nonporous system that is largely favourable to TPLSM. © 2018 The Authors Journal of Microscopy © 2018 Royal Microscopical Society.

Simultaneous Femtosecond X-ray Spectroscopy and Diffraction of Photosystem II at Room Temperature

PubMed Central

Kern, Jan; Alonso-Mori, Roberto; Tran, Rosalie; Hattne, Johan; Gildea, Richard J.; Echols, Nathaniel; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G.; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; DiFiore, Dörte; Milathianaki, Despina; Fry, Alan R.; Miahnahri, Alan; Schafer, Donald W.; Messerschmidt, Marc; Seibert, M. Marvin; Koglin, Jason E.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J.; Grosse-Kunstleve, Ralf W.; Zwart, Petrus H.; White, William E.; Glatzel, Pieter; Adams, Paul D.; Bogan, Michael J.; Williams, Garth J.; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Sauter, Nicholas K.; Yachandra, Vittal K.; Bergmann, Uwe; Yano, Junko

2013-01-01

Intense femtosecond X-ray pulses produced at the Linac Coherent Light Source (LCLS) were used for simultaneous X-ray diffraction (XRD) and X-ray emission spectroscopy (XES) of microcrystals of Photosystem II (PS II) at room temperature. This method probes the overall protein structure and the electronic structure of the Mn4CaO5 cluster in the oxygen-evolving complex of PS II. XRD data are presented from both the dark state (S1) and the first illuminated state (S2) of PS II. Our simultaneous XRD/XES study shows that the PS II crystals are intact during our measurements at the LCLS, not only with respect to the structure of PS II, but also with regard to the electronic structure of the highly radiation sensitive Mn4CaO5 cluster, opening new directions for future dynamics studies. PMID:23413188

Simultaneous femtosecond X-ray spectroscopy and diffraction of photosystem II at room temperature.

PubMed

Kern, Jan; Alonso-Mori, Roberto; Tran, Rosalie; Hattne, Johan; Gildea, Richard J; Echols, Nathaniel; Glöckner, Carina; Hellmich, Julia; Laksmono, Hartawan; Sierra, Raymond G; Lassalle-Kaiser, Benedikt; Koroidov, Sergey; Lampe, Alyssa; Han, Guangye; Gul, Sheraz; Difiore, Dörte; Milathianaki, Despina; Fry, Alan R; Miahnahri, Alan; Schafer, Donald W; Messerschmidt, Marc; Seibert, M Marvin; Koglin, Jason E; Sokaras, Dimosthenis; Weng, Tsu-Chien; Sellberg, Jonas; Latimer, Matthew J; Grosse-Kunstleve, Ralf W; Zwart, Petrus H; White, William E; Glatzel, Pieter; Adams, Paul D; Bogan, Michael J; Williams, Garth J; Boutet, Sébastien; Messinger, Johannes; Zouni, Athina; Sauter, Nicholas K; Yachandra, Vittal K; Bergmann, Uwe; Yano, Junko

2013-04-26

Intense femtosecond x-ray pulses produced at the Linac Coherent Light Source (LCLS) were used for simultaneous x-ray diffraction (XRD) and x-ray emission spectroscopy (XES) of microcrystals of photosystem II (PS II) at room temperature. This method probes the overall protein structure and the electronic structure of the Mn4CaO5 cluster in the oxygen-evolving complex of PS II. XRD data are presented from both the dark state (S1) and the first illuminated state (S2) of PS II. Our simultaneous XRD-XES study shows that the PS II crystals are intact during our measurements at the LCLS, not only with respect to the structure of PS II, but also with regard to the electronic structure of the highly radiation-sensitive Mn4CaO5 cluster, opening new directions for future dynamics studies.

Measurement Error in Atomic-Scale Scanning Transmission Electron Microscopy-Energy-Dispersive X-Ray Spectroscopy (STEM-EDS) Mapping of a Model Oxide Interface.

PubMed

Spurgeon, Steven R; Du, Yingge; Chambers, Scott A

2017-06-01

With the development of affordable aberration correctors, analytical scanning transmission electron microscopy (STEM) studies of complex interfaces can now be conducted at high spatial resolution at laboratories worldwide. Energy-dispersive X-ray spectroscopy (EDS) in particular has grown in popularity, as it enables elemental mapping over a wide range of ionization energies. However, the interpretation of atomically resolved data is greatly complicated by beam-sample interactions that are often overlooked by novice users. Here we describe the practical factors-namely, sample thickness and the choice of ionization edge-that affect the quantification of a model perovskite oxide interface. Our measurements of the same sample, in regions of different thickness, indicate that interface profiles can vary by as much as 2-5 unit cells, depending on the spectral feature. This finding is supported by multislice simulations, which reveal that on-axis maps of even perfectly abrupt interfaces exhibit significant delocalization. Quantification of thicker samples is further complicated by channeling to heavier sites across the interface, as well as an increased signal background. We show that extreme care must be taken to prepare samples to minimize channeling effects and argue that it may not be possible to extract atomically resolved information from many chemical maps.

Measurement Error in Atomic-Scale Scanning Transmission Electron Microscopy—Energy-Dispersive X-Ray Spectroscopy (STEM-EDS) Mapping of a Model Oxide Interface

DOE Office of Scientific and Technical Information (OSTI.GOV)

Spurgeon, Steven R.; Du, Yingge; Chambers, Scott A.

Abstract With the development of affordable aberration correctors, analytical scanning transmission electron microscopy (STEM) studies of complex interfaces can now be conducted at high spatial resolution at laboratories worldwide. Energy-dispersive X-ray spectroscopy (EDS) in particular has grown in popularity, as it enables elemental mapping over a wide range of ionization energies. However, the interpretation of atomically resolved data is greatly complicated by beam–sample interactions that are often overlooked by novice users. Here we describe the practical factors—namely, sample thickness and the choice of ionization edge—that affect the quantification of a model perovskite oxide interface. Our measurements of the same sample,more » in regions of different thickness, indicate that interface profiles can vary by as much as 2–5 unit cells, depending on the spectral feature. This finding is supported by multislice simulations, which reveal that on-axis maps of even perfectly abrupt interfaces exhibit significant delocalization. Quantification of thicker samples is further complicated by channeling to heavier sites across the interface, as well as an increased signal background. We show that extreme care must be taken to prepare samples to minimize channeling effects and argue that it may not be possible to extract atomically resolved information from many chemical maps.« less

Measurement Error in Atomic-Scale Scanning Transmission Electron Microscopy—Energy-Dispersive X-Ray Spectroscopy (STEM-EDS) Mapping of a Model Oxide Interface

DOE PAGES

Spurgeon, Steven R.; Du, Yingge; Chambers, Scott A.

2017-04-05

Abstract With the development of affordable aberration correctors, analytical scanning transmission electron microscopy (STEM) studies of complex interfaces can now be conducted at high spatial resolution at laboratories worldwide. Energy-dispersive X-ray spectroscopy (EDS) in particular has grown in popularity, as it enables elemental mapping over a wide range of ionization energies. However, the interpretation of atomically resolved data is greatly complicated by beam–sample interactions that are often overlooked by novice users. Here we describe the practical factors—namely, sample thickness and the choice of ionization edge—that affect the quantification of a model perovskite oxide interface. Our measurements of the same sample,more » in regions of different thickness, indicate that interface profiles can vary by as much as 2–5 unit cells, depending on the spectral feature. This finding is supported by multislice simulations, which reveal that on-axis maps of even perfectly abrupt interfaces exhibit significant delocalization. Quantification of thicker samples is further complicated by channeling to heavier sites across the interface, as well as an increased signal background. We show that extreme care must be taken to prepare samples to minimize channeling effects and argue that it may not be possible to extract atomically resolved information from many chemical maps.« less

Instrumentation for in situ flow electrochemical Scanning Transmission X-ray Microscopy (STXM)

NASA Astrophysics Data System (ADS)

Prabu, Vinod; Obst, Martin; Hosseinkhannazer, Hooman; Reynolds, Matthew; Rosendahl, Scott; Wang, Jian; Hitchcock, Adam P.

2018-06-01

We report the design and performance of a 3-electrode device for real time in situ scanning transmission X-ray microscopy studies of electrochemical processes under both static (sealed, non-flow) conditions and with a continuous flow of electrolytes. The device was made using a combination of silicon microfabrication and 3D printing technologies. The performance is illustrated by results of a study of copper deposition and stripping at a gold working electrode. X-ray absorption spectromicroscopy at the Cu 2p edge was used to follow the evolution as a function of potential and time of the spatial distributions of Cu(0) and Cu(i) species electro-deposited from an aqueous solution of copper sulphate. The results are interpreted in terms of competing mechanisms for the reduction of Cu(ii).

Phonon spectroscopy with sub-meV resolution by femtosecond x-ray diffuse scattering

DOE PAGES

Zhu, Diling; Robert, Aymeric; Henighan, Tom; ...

2015-08-10

We present a reconstruction of the transverse acoustic phonon dispersion of germanium from femtosecond time-resolved x-ray diffuse scattering measurements at the Linac Coherent Light Source. We demonstrate an energy resolution of 0.3 meV with a momentum resolution of 0.01 nm -1 using 10-keV x rays with a bandwidth of ~ 1 eV. This high resolution was achieved simultaneously for a large section of reciprocal space including regions closely following three of the principal symmetry directions. The phonon dispersion was reconstructed with less than 3 h of measurement time, during which neither the x-ray energy, the sample orientation, nor the detectormore » position were scanned. In conclusion, these results demonstrate how time-domain measurements can complement conventional frequency domain inelastic-scattering techniques.« less

Component analyses of urinary nanocrystallites of uric acid stone formers by combination of high-resolution transmission electron microscopy, fast Fourier transformation, energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared spectroscopy.

PubMed

Sun, Xin-Yuan; Xue, Jun-Fa; Xia, Zhi-Yue; Ouyang, Jian-Ming

2015-06-01

This study aimed to analyse the components of nanocrystallites in urines of patients with uric acid (UA) stones. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, high-resolution transmission electron microscopy (HRTEM), fast Fourier transformation (FFT) of HRTEM, and energy dispersive X-ray spectroscopy (EDS) were performed to analyse the components of these nanocrystallites. XRD and FFT showed that the main component of urinary nanocrystallites was UA, which contains a small amount of calcium oxalate monohydrate and phosphates. EDS showed the characteristic absorption peaks of C, O, Ca and P. The formation of UA stones was closely related to a large number of UA nanocrystallites in urine. A combination of HRTEM, FFT, EDS and XRD analyses could be performed accurately to analyse the components of urinary nanocrystallites.

Bone age assessment by dual-energy X-ray absorptiometry in children: an alternative for X-ray?

PubMed

Heppe, D H M; Taal, H R; Ernst, G D S; Van Den Akker, E L T; Lequin, M M H; Hokken-Koelega, A C S; Geelhoed, J J M; Jaddoe, V W V

2012-02-01

The aim of the study was to validate dual-energy X-ray absorptiometry (DXA) as a method to assess bone age in children. Paired dual-energy X-ray absorptiometry (DXA) scans and X-rays of the left hand were performed in 95 children who attended the paediatric endocrinology outpatient clinic of University Hospital Rotterdam, the Netherlands. We compared bone age assessments by DXA scan with those performed by X-ray. Bone age assessment was performed by two blinded observers according to the reference method of Greulich and Pyle. Intra-observer and interobserver reproducibility were investigated using the intraclass correlation coefficient (ICC), and agreement was tested using Bland and Altman plots. The intra-observer ICCs for both observers were 0.997 and 0.991 for X-ray and 0.993 and 0.987 for DXA assessments. The interobserver ICC was 0.993 and 0.991 for X-ray and DXA assessments, respectively. The mean difference between bone age assessed by X-ray and DXA was 0.11 years. The limits of agreement ranged from -0.82 to 1.05 years, which means that 95% of all differences between the methods were covered by this range. Results of bone age assessment by DXA scan are similar to those obtained by X-ray. The DXA method seems to be an alternative for assessing bone age in a paediatric hospital-based population.

"Un-annealed and Annealed Pd Ultra-Thin Film on SiC Characterized by Scanning Probe Microscopy and X-ray Photoelectron Spectroscopy"

NASA Technical Reports Server (NTRS)

Lu, W. J.; Shi, D. T.; Elshot, K.; Bryant, E.; Lafate, K.; Chen, H.; Burger, A.; Collins, W. E.

1998-01-01

Pd/SiC has been used as a hydrogen and a hydrocarbon gas sensor operated at high temperature. UHV (Ultra High Vacuum)-Scanning Tunneling Microscopy (STM), Atomic Force Microscopy (AFM) and X-ray Photoelectron Spectroscopy (XPS) techniques were applied to study the relationship between the morphology and chemical compositions for Pd ultra-thin films on SiC (less than 30 angstroms) at different annealing temperatures. Pd ultra-thin film on 6H-SiC was prepared by the RF sputtering method. The morphology from UHV-STM and AFM shows that the Pd thin film was well deposited on SiC substrate, and the Pd was partially aggregated to round shaped participates at an annealing temperature of 300 C. At 400 C, the amount of surface participates decreases, and some strap shape participates appear. From XPS, Pd2Si was formed on the surface after annealing at 300 C, and all Pd reacted with SiC to form Pd2Si after annealing at 400 C. The intensity of the XPS Pd peak decreases enormously at 400 C. The Pd film diffused into SiC, and the Schottky barrier height has almost no changes. The work shows the Pd sicilides/SiC have the same electronic properties with Pd/SiC, and explains why the Pd/SiC sensor still responds to hydrogen at high operating temperatures.

X-ray diagnostics of massive star winds

NASA Astrophysics Data System (ADS)

Oskinova, L. M.; Ignace, R.; Huenemoerder, D. P.

2017-11-01

Observations with powerful X-ray telescopes, such as XMM-Newton and Chandra, significantly advance our understanding of massive stars. Nearly all early-type stars are X-ray sources. Studies of their X-ray emission provide important diagnostics of stellar winds. High-resolution X-ray spectra of O-type stars are well explained when stellar wind clumping is taking into account, providing further support to a modern picture of stellar winds as non-stationary, inhomogeneous outflows. X-ray variability is detected from such winds, on time scales likely associated with stellar rotation. High-resolution X-ray spectroscopy indicates that the winds of late O-type stars are predominantly in a hot phase. Consequently, X-rays provide the best observational window to study these winds. X-ray spectroscopy of evolved, Wolf-Rayet type, stars allows to probe their powerful metal enhanced winds, while the mechanisms responsible for the X-ray emission of these stars are not yet understood.

Origin of Pressure-induced Superconducting Phase in K xFe 2-ySe 2 studied by Synchrotron X-ray Diffraction and Spectroscopy

DOE PAGES

Yamamoto, Yoshiya; Yamaoka, Hitoshi; Tanaka, Masashi; ...

2016-08-08

Pressure dependence of the electronic and crystal structures of K xFe 2–ySe 2, which has pressure-induced two superconducting domes of SC I and SC II, was investigated by x-ray emission spectroscopy and diffraction. X-ray diffraction data show that compressibility along the c-axis changes around 12 GPa, where a new superconducting phase of SC II appears. This suggests a possible tetragonal to collapsed tetragonal phase transition. X-ray emission spectroscopy data also shows the change in the electronic structure around 12 GPa. These results can be explained by the scenario that the two SC domes under pressure originate from the change ofmore » Fermi surface topology. Lastly, our results here show the pronounced increase of the density of states near the Fermi surface under pressure with a structural phase transition, which can help address our fundamental understanding for the appearance of the SC II phase.« less

High-rate x-ray spectroscopy in mammography with a CdTe detector: a digital pulse processing approach.

PubMed

Abbene, L; Gerardi, G; Principato, F; Del Sordo, S; Ienzi, R; Raso, G

2010-12-01

Direct measurement of mammographic x-ray spectra under clinical conditions is a difficult task due to the high fluence rate of the x-ray beams as well as the limits in the development of high resolution detection systems in a high counting rate environment. In this work we present a detection system, based on a CdTe detector and an innovative digital pulse processing (DPP) system, for high-rate x-ray spectroscopy in mammography. The DPP system performs a digital pile-up inspection and a digital pulse height analysis of the detector signals, digitized through a 14-bit, 100 MHz digitizer, for x-ray spectroscopy even at high photon counting rates. We investigated on the response of the digital detection system both at low (150 cps) and at high photon counting rates (up to 500 kcps) by using monoenergetic x-ray sources and a nonclinical molybdenum anode x-ray tube. Clinical molybdenum x-ray spectrum measurements were also performed by using a pinhole collimator and a custom alignment device. The detection system shows excellent performance up to 512 kcps with an energy resolution of 4.08% FWHM at 22.1 keV. Despite the high photon counting rate (up to 453 kcps), the molybdenum x-ray spectra, measured under clinical conditions, are characterized by a low number of pile-up events. The agreement between the attenuation curves and the half value layer values, obtained from the measured spectra, simulated spectra, and from the exposure values directly measured with an ionization chamber, also shows the accuracy of the measurements. These results make the proposed detection system a very attractive tool for both laboratory research and advanced quality controls in mammography.

X-ray photoelectron spectroscopy for characterization of wood surfaces in adhesion studies

Treesearch

James F. Beecher; Charles R. Frihart

2005-01-01

X-ray photoelectron spectroscopy (XPS) is one of a set of tools that have been used to characterize wood surfaces. Among the advantages of XPS are surface sensitivity, identification of nearly all elements, and frequently, discrimination of bonding states. For these reasons, XPS seemed to be an appropriate tool to help explain the differences in bond strength under wet...

CONTIN XPCS: Software for Inverse Transform Analysis of X-Ray Photon Correlation Spectroscopy Dynamics

PubMed Central

Narayanan, Suresh; Zhang, Fan; Kuzmenko, Ivan; Ilavsky, Jan

2018-01-01

X-ray photon correlation spectroscopy (XPCS) and dynamic light scattering (DLS) both reveal dynamics using coherent scattering, but X-rays permit investigating of dynamics in a much more diverse array of materials. Heterogeneous dynamics occur in many such materials, and we showed how classic tools employed in analysis of heterogeneous DLS dynamics extend to XPCS, revealing additional information that conventional Kohlrausch exponential fitting obscures. This work presents the software implementation of inverse transform analysis of XPCS data called CONTIN XPCS, an extension of traditional CONTIN that accommodates dynamics encountered in equilibrium XPCS measurements. PMID:29875507

CONTIN XPCS: Software for Inverse Transform Analysis of X-Ray Photon Correlation Spectroscopy Dynamics.

PubMed

Andrews, Ross N; Narayanan, Suresh; Zhang, Fan; Kuzmenko, Ivan; Ilavsky, Jan

2018-02-01

X-ray photon correlation spectroscopy (XPCS) and dynamic light scattering (DLS) both reveal dynamics using coherent scattering, but X-rays permit investigating of dynamics in a much more diverse array of materials. Heterogeneous dynamics occur in many such materials, and we showed how classic tools employed in analysis of heterogeneous DLS dynamics extend to XPCS, revealing additional information that conventional Kohlrausch exponential fitting obscures. This work presents the software implementation of inverse transform analysis of XPCS data called CONTIN XPCS, an extension of traditional CONTIN that accommodates dynamics encountered in equilibrium XPCS measurements.

Sodium Chloride Diffusion during Muscle Salting Evidenced by Energy-Dispersive X-ray Spectroscopy Imaging.

PubMed

Filgueras, Rénata; Peyrin, Frédéric; Vénien, Annie; Hénot, Jean Marc; Astruc, Thierry

2016-01-27

To better understand the relationship between the muscle structure and NaCl transfers in meat, we used energy-dispersive X-ray spectroscopy (EDS) coupled with scanning electron microscopy (SEM) to analyze brined and dry-salted rat muscles. The muscles were freeze-dried to avoid the delocalization of soluble ions that happens in regular dehydration through a graded series of ethanol. Na and Cl maps were superimposed on SEM images to combine the muscle structure and NaCl diffusion. Brining causes rapid diffusion of NaCl through the tissue. Most brine diffuses in a linear front from the muscle surface, but a small proportion enters through the perimysium network. The muscle area penetrated by brine shows heterogeneous patterns of NaCl retention, with some connective tissue islets containing more NaCl than other parts of perimysium. NaCl penetration is considerably slower after dry salting than after brining.

Fluorescence imaging of reactive oxygen species by confocal laser scanning microscopy for track analysis of synchrotron X-ray photoelectric nanoradiator dose: X-ray pump-optical probe.

PubMed

Jeon, Jae Kun; Han, Sung Mi; Kim, Jong Ki

2016-09-01

Bursts of emissions of low-energy electrons, including interatomic Coulomb decay electrons and Auger electrons (0-1000 eV), as well as X-ray fluorescence produced by irradiation of large-Z element nanoparticles by either X-ray photons or high-energy ion beams, is referred to as the nanoradiator effect. In therapeutic applications, this effect can damage pathological tissues that selectively take up the nanoparticles. Herein, a new nanoradiator dosimetry method is presented that uses probes for reactive oxygen species (ROS) incorporated into three-dimensional gels, on which macrophages containing iron oxide nanoparticles (IONs) are attached. This method, together with site-specific irradiation of the intracellular nanoparticles from a microbeam of polychromatic synchrotron X-rays (5-14 keV), measures the range and distribution of OH radicals produced by X-ray emission or superoxide anions ({\\rm{O}}_2^-) produced by low-energy electrons. The measurements are based on confocal laser scanning of the fluorescence of the hydroxyl radical probe 2-[6-(4'-amino)phenoxy-3H-xanthen-3-on-9-yl] benzoic acid (APF) or the superoxide probe hydroethidine-dihydroethidium (DHE) that was oxidized by each ROS, enabling tracking of the radiation dose emitted by the nanoradiator. In the range 70 µm below the irradiated cell, ^\\bullet{\\rm{OH}} radicals derived mostly from either incident X-ray or X-ray fluorescence of ION nanoradiators are distributed along the line of depth direction in ROS gel. In contrast, {\\rm{O}}_2^- derived from secondary electron or low-energy electron emission by ION nanoradiators are scattered over the ROS gel. ROS fluorescence due to the ION nanoradiators was observed continuously to a depth of 1.5 mm for both oxidized APF and oxidized DHE with relatively large intensity compared with the fluorescence caused by the ROS produced solely by incident primary X-rays, which was limited to a depth of 600 µm, suggesting dose enhancement as well as more

Scanning Kirkpatrick-Baez X-ray telescope to maximize effective area and eliminate spurious images - Design

NASA Technical Reports Server (NTRS)

Kast, J. W.

1975-01-01

We consider the design of a Kirkpatrick-Baez grazing-incidence X-ray telescope to be used in a scan of the sky and analyze the distribution of both properly reflected rays and spurious images over the field of view. To obtain maximum effective area over the field of view, it is necessary to increase the spacing between plates for a scanning telescope as compared to a pointing telescope. Spurious images are necessarily present in this type of lens, but they can be eliminated from the field of view by adding properly located baffles or collimators. Results of a computer design are presented.

Proposed new accelerator design for homeland security x-ray applications

DOE PAGES

Clayton, James; Shedlock, Daniel; Langeveld, Willem G.J.; ...

2015-01-01

Two goals for security scanning of cargo and freight are the ability to determine the type of material that is being imaged, and to do so at low radiation dose. One commonly used technique to determine the effective Z of the cargo is dual-energy imaging, i.e. imaging with different x-ray energy spectra. Another technique uses the fact that the transmitted x-ray spectrum itself also depends on the effective Z. Spectroscopy is difficult because the energy of individual x rays needs to be measured in a very high count-rate environment. Typical accelerators for security applications offer large but short bursts ofmore » x-rays, suitable for current-mode integrated imaging. In order to perform x-ray spectroscopy, a new accelerator design is desired that has the following features: 1) increased duty factor in order to spread out the arrival of x-rays at the detector array over time; 2) x-ray intensity modulation from one delivered pulse to the next by adjusting the accelerator electron beam instantaneous current so as to deliver adequate signal without saturating the spectroscopic detector; and 3) the capability to direct the (forward peaked) x-ray intensity towards high-attenuation areas in the cargo (“fan-beam-steering”). Current sources are capable of 0.1% duty factor, although usually they are operated at significantly lower duty factors (~0.04%), but duty factors in the range 0.4-1.0% are desired. The higher duty factor can be accomplished, e.g., by moving from 300 pulses per second (pps) to 1000 pps and/or increasing the pulse duration from a typical 4 μs to 10 μs. This paper describes initial R&D to examine cost effective modifications that could be performed on a typical accelerator for these purposes, as well as R&D for fan-beam steering.« less

Charge and Spin-State Characterization of Cobalt Bis( o-dioxolene) Valence Tautomers Using Co Kβ X-ray Emission and L-Edge X-ray Absorption Spectroscopies

DOE PAGES

Liang, H. Winnie; Kroll, Thomas; Nordlund, Dennis; ...

2016-12-30

The valence tautomeric states of Co(phen)(3,5-DBQ) 2 and Co(tmeda)(3,5-DBQ) 2, where 3,5-DBQ is either the semiquinone (SQ –) or catecholate (Cat 2–) form of 3,5-di- tert-butyl-1,2-benzoquinone, have been examined by a series of cobalt-specific X-ray spectroscopies. In this work, we have utilized the sensitivity of 1s3p X-ray emission spectroscopy (Kβ XES) to the oxidation and spin states of 3d transition-metal ions to determine the cobalt-specific electronic structure of valence tautomers. A comparison of their Kβ XES spectra with the spectra of cobalt coordination complexes with known oxidation and spin states demonstrates that the low-temperature valence tautomer can be described asmore » a low-spin Co III configuration and the high-temperature valence tautomer as a high-spin Co II configuration. This conclusion is further supported by Co L-edge X-ray absorption spectroscopy (L-edge XAS) of the high-temperature valence tautomers and ligand-field atomic-multiplet calculations of the Kβ XES and L-edge XAS spectra. In conclusion, the nature and strength of the magnetic exchange interaction between the cobalt center and SQ – in cobalt valence tautomers is discussed in view of the effective spin at the Co site from Kβ XES and the molecular spin moment from magnetic susceptibility measurements.« less

Charge and Spin-State Characterization of Cobalt Bis( o-dioxolene) Valence Tautomers Using Co Kβ X-ray Emission and L-Edge X-ray Absorption Spectroscopies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liang, H. Winnie; Kroll, Thomas; Nordlund, Dennis

The valence tautomeric states of Co(phen)(3,5-DBQ) 2 and Co(tmeda)(3,5-DBQ) 2, where 3,5-DBQ is either the semiquinone (SQ –) or catecholate (Cat 2–) form of 3,5-di- tert-butyl-1,2-benzoquinone, have been examined by a series of cobalt-specific X-ray spectroscopies. In this work, we have utilized the sensitivity of 1s3p X-ray emission spectroscopy (Kβ XES) to the oxidation and spin states of 3d transition-metal ions to determine the cobalt-specific electronic structure of valence tautomers. A comparison of their Kβ XES spectra with the spectra of cobalt coordination complexes with known oxidation and spin states demonstrates that the low-temperature valence tautomer can be described asmore » a low-spin Co III configuration and the high-temperature valence tautomer as a high-spin Co II configuration. This conclusion is further supported by Co L-edge X-ray absorption spectroscopy (L-edge XAS) of the high-temperature valence tautomers and ligand-field atomic-multiplet calculations of the Kβ XES and L-edge XAS spectra. In conclusion, the nature and strength of the magnetic exchange interaction between the cobalt center and SQ – in cobalt valence tautomers is discussed in view of the effective spin at the Co site from Kβ XES and the molecular spin moment from magnetic susceptibility measurements.« less

Phosphor Scanner For Imaging X-Ray Diffraction

NASA Technical Reports Server (NTRS)

Carter, Daniel C.; Hecht, Diana L.; Witherow, William K.

1992-01-01

Improved optoelectronic scanning apparatus generates digitized image of x-ray image recorded in phosphor. Scanning fiber-optic probe supplies laser light stimulating luminescence in areas of phosphor exposed to x rays. Luminescence passes through probe and fiber to integrating sphere and photomultiplier. Sensitivity and resolution exceed previously available scanners. Intended for use in x-ray crystallography, medical radiography, and molecular biology.

X-ray microanalysis in the scanning electron microscope.

PubMed

Roomans, Godfried M; Dragomir, Anca

2014-01-01

X-ray microanalysis conducted using the scanning electron microscope is a technique that allows the determination of chemical elements in bulk or semi-thick specimens. The lowest concentration of an element that can be detected is in the order of a few mmol/kg or a few hundred parts per million, and the smallest amount is in the order of 10(-18) g. The spatial resolution of the analysis depends on the thickness of the specimen. For biological specimen analysis, care must be taken to prevent displacement/loss of the element of interest (usually ions). Protocols are presented for the processing of frozen-hydrated and freeze-dried specimens, as well as for the analysis of small volumes of fluid, cell cultures, and other specimens. Aspects of qualitative and quantitative analysis are covered, including limitations of the technique.

X-ray microanalysis in the scanning electron microscope.

PubMed

Roomans, Godfried M; Dragomir, Anca

2007-01-01

X-ray microanalysis conducted using the scanning electron microscope is a technique that allows the determination of chemical elements in bulk or semithick specimens. The lowest concentration of an element that can be detected is in the order of a few mmol/kg or a few hundred parts per million, and the smallest amount is in the order of 10(-18) g. The spatial resolution of the analysis depends on the thickness of the specimen. For biological specimen analysis, care must be taken to prevent displacement/loss of the element of interest (usually ions). Protocols are presented for the processing of frozen-hydrated and freeze-dried specimens, as well as for the analysis of small volumes of fluid, cell cultures and other specimens. Aspects of qualitative and quantitative analysis are covered, including limitations of the technique.

Specimen charging in X-ray absorption spectroscopy: correction of total electron yield data from stabilized zirconia in the energy range 250-915 eV.

PubMed

Vlachos, Dimitrios; Craven, Alan J; McComb, David W

2005-03-01

The effects of specimen charging on X-ray absorption spectroscopy using total electron yield have been investigated using powder samples of zirconia stabilized by a range of oxides. The stabilized zirconia powder was mixed with graphite to minimize the charging but significant modifications of the intensities of features in the X-ray absorption near-edge fine structure (XANES) still occurred. The time dependence of the charging was measured experimentally using a time scan, and an algorithm was developed to use this measured time dependence to correct the effects of the charging. The algorithm assumes that the system approaches the equilibrium state by an exponential decay. The corrected XANES show improved agreement with the electron energy-loss near-edge fine structure obtained from the same samples.

a High-Density Electron Beam and Quad-Scan Measurements at Pleiades Thomson X-Ray Source

NASA Astrophysics Data System (ADS)

Lim, J. K.; Rosenzweig, J. B.; Anderson, S. G.; Tremaine, A. M.

2007-09-01

A recent development of the photo-cathode injector technology has greatly enhanced the beam quality necessary for the creation of high density/high brightness electron beam sources. In the Thomson backscattering x-ray experiment, there is an immense need for under 20 micron electron beam spot at the interaction point with a high-intensity laser in order to produce a large x-ray flux. This has been demonstrated successfully at PLEIADES in Lawrence Livermore National Laboratory. For this Thomson backscattering experiment, we employed an asymmetric triplet, high remanence permanent-magnet quads to produce smaller electron beams. Utilizing highly efficient optical transition radiation (OTR) beam spot imaging technique and varying electron focal spot sizes enabled a quadrupole scan at the interaction zone. Comparisons between Twiss parameters obtained upstream to those parameter values deduced from PMQ scan will be presented in this report.

a High-Density Electron Beam and Quad-Scan Measurements at Pleiades Thomson X-Ray Source

NASA Astrophysics Data System (ADS)

Lim, J. K.; Rosenzweig, J. B.; Anderson, S. G.; Tremaine, A. M.

A recent development of the photo-cathode injector technology has greatly enhanced the beam quality necessary for the creation of high density/high brightness electron beam sources. In the Thomson backscattering x-ray experiment, there is an immense need for under 20 micron electron beam spot at the interaction point with a high-intensity laser in order to produce a large x-ray flux. This has been demonstrated successfully at PLEIADES in Lawrence Livermore National Laboratory. For this Thomson backscattering experiment, we employed an asymmetric triplet, high remanence permanent-magnet quads to produce smaller electron beams. Utilizing highly efficient optical transition radiation (OTR) beam spot imaging technique and varying electron focal spot sizes enabled a quadrupole scan at the interaction zone. Comparisons between Twiss parameters obtained upstream to those parameter values deduced from PMQ scan will be presented in this report.

Counting-loss correction for X-ray spectroscopy using unit impulse pulse shaping.

PubMed

Hong, Xu; Zhou, Jianbin; Ni, Shijun; Ma, Yingjie; Yao, Jianfeng; Zhou, Wei; Liu, Yi; Wang, Min

2018-03-01

High-precision measurement of X-ray spectra is affected by the statistical fluctuation of the X-ray beam under low-counting-rate conditions. It is also limited by counting loss resulting from the dead-time of the system and pile-up pulse effects, especially in a high-counting-rate environment. In this paper a detection system based on a FAST-SDD detector and a new kind of unit impulse pulse-shaping method is presented, for counting-loss correction in X-ray spectroscopy. The unit impulse pulse-shaping method is evolved by inverse deviation of the pulse from a reset-type preamplifier and a C-R shaper. It is applied to obtain the true incoming rate of the system based on a general fast-slow channel processing model. The pulses in the fast channel are shaped to unit impulse pulse shape which possesses small width and no undershoot. The counting rate in the fast channel is corrected by evaluating the dead-time of the fast channel before it is used to correct the counting loss in the slow channel.

Reactor for tracking catalyst nanoparticles in liquid at high temperature under a high-pressure gas phase with X-ray absorption spectroscopy.

PubMed

Nguyen, Luan; Tao, Franklin Feng

2018-02-01

Structure of catalyst nanoparticles dispersed in liquid phase at high temperature under gas phase of reactant(s) at higher pressure (≥5 bars) is important for fundamental understanding of catalytic reactions performed on these catalyst nanoparticles. Most structural characterizations of a catalyst performing catalysis in liquid at high temperature under gas phase at high pressure were performed in an ex situ condition in terms of characterizations before or after catalysis since, from technical point of view, access to the catalyst nanoparticles during catalysis in liquid phase at high temperature under high pressure reactant gas is challenging. Here we designed a reactor which allows us to perform structural characterization using X-ray absorption spectroscopy including X-ray absorption near edge structure spectroscopy and extended X-ray absorption fine structure spectroscopy to study catalyst nanoparticles under harsh catalysis conditions in terms of liquid up to 350 °C under gas phase with a pressure up to 50 bars. This reactor remains nanoparticles of a catalyst homogeneously dispersed in liquid during catalysis and X-ray absorption spectroscopy characterization.

X-ray emission spectroscopy of biomimetic Mn coordination complexes

DOE PAGES

Jensen, Scott C.; Davis, Katherine M.; Sullivan,

2017-05-19

Understanding the function of Mn ions in biological and chemical redox catalysis requires precise knowledge of their electronic structure. X-ray emission spectroscopy (XES) is an emerging technique with a growing application to biological and biomimetic systems. Here, we report an improved, cost-effective spectrometer used to analyze two biomimetic coordination compounds, [Mn IV(OH) 2(Me 2EBC)] 2+ and [Mn IV(O)(OH)(Me 2EBC)] +, the second of which contains a key Mn IV=O structural fragment. Despite having the same formal oxidation state (Mn IV) and tetradentate ligands, XES spectra from these two compounds demonstrate different electronic structures. Experimental measurements and DFT calculations yield differentmore » localized spin densities for the two complexes resulting from Mn IV–OH conversion to Mn IV=O. The relevance of the observed spectroscopic changes is discussed for applications in analyzing complex biological systems such as photosystem II. In conclusion, a model of the S 3 intermediate state of photosystem II containing a Mn IV=O fragment is compared to recent time-resolved X-ray diffraction data of the same state.« less

The Application of Scanning Electron Microscopy with Energy-Dispersive X-Ray Spectroscopy (SEM-EDX) in Ancient Dental Calculus for the Reconstruction of Human Habits.

PubMed

Fialová, Dana; Skoupý, Radim; Drozdová, Eva; Paták, Aleš; Piňos, Jakub; Šín, Lukáš; Beňuš, Radoslav; Klíma, Bohuslav

2017-12-01

The great potential of scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX) is in detection of unusual chemical elements included in ancient human dental calculus to verify hypotheses about life and burial habits of historic populations and individuals. Elemental spectra were performed from archeological samples of three chosen individuals from different time periods. The unusual presence of magnesium, aluminum, and silicon in the first sample could confirm the hypothesis of high degree of dental abrasion caused by particles from grinding stones in flour. In the second sample, presence of copper could confirm that bronze jewelery could lie near the buried body. The elemental composition of the third sample with the presence of lead and copper confirms the origin of individual to Napoleonic Wars because the damage to his teeth could be explained by the systematic utilization of the teeth for the opening of paper cartridges (a charge with a dose of gunpowder and a bullet), which were used during the 18th and the 19th century AD. All these results contribute to the reconstruction of life (first and third individual) and burial (second individual) habits of historic populations and individuals.

Development of a scanning transmission x-ray microscope for the beamline P04 at PETRA III DESY

DOE Office of Scientific and Technical Information (OSTI.GOV)

Andrianov, Konstantin; Ewald, Johannes; Nisius, Thomas

We present a scanning transmission x-ray microscope (STXM) built on top of our existing modular platform for high resolution imaging experiments. This platform consists of up to three separate vacuum chambers and custom designed piezo stages. These piezo stages are able to move precisely in x-, y- and z-direction, this makes it possible to adjust the components for different imaging modes. During recent experiments the endstation was operated mainly as a transmission x-ray microscope (TXM) [1, 2].

Quantitative phase tomography by using x-ray microscope with Foucault knife-edge scanning filter

DOE Office of Scientific and Technical Information (OSTI.GOV)

Watanabe, Norio; Tsuburaya, Yuji; Shimada, Akihiro

2016-01-28

Quantitative phase tomography was evaluated by using a differential phase microscope with a Foucault knife-edge scanning filter. A 3D x-ray phase image of polystyrene beads was obtained at 5.4 keV. The reconstructed refractive index was fairly good agreement with the Henke’s tabulated data.

Single- and double-core-hole ion emission spectroscopy of transient neon plasmas produced by ultraintense x-ray laser pulses

NASA Astrophysics Data System (ADS)

Gao, Cheng; Zeng, Jiaolong; Yuan, Jianmin

2016-02-01

Single-core-hole (SCH) and double-core-hole (DCH) spectroscopy is investigated systematically for neon gas in the interaction with ultraintense x-ray pulses with photon energy from 937 eV to 2000 eV. A time-dependent rate equation, implemented in detailed level accounting approximation, is utilized to study the dynamical evolution of the level population and emission properties of the laser-produced highly transient plasmas. The plasma-density effects on level populations and charge-state distribution are demonstrated with an x-ray photon energy of 2000 eV. It is shown that atomic number density of relevant experiment is about 1 × 1018 cm-3, which is comparable to a recent experiment. At this density, we systematically investigate the emissivity of the transient neon plasmas. For laser photon energy in the range 937-1360 eV, resonant absorptions (RA) of 1s\\to {np} (n≥slant 2) transitions play important roles in time evolution of the population and DCH emission spectroscopy. The RA effects are illustrated in detail for an x-ray pulse of 944 eV photon energy, which creates the 1s\\to 2p RA from the SCH states (1s2{s}22{p}4, 1s2s2p5, and 1s2p6) of Ne3+. After averaging over the space and time distribution of x-ray pulse, DCH emission spectroscopy is studied at x-ray photon energies of 937, 944, 955, 968, 980, and 990 eV, where there exist 1s\\to 2p resonances from SCH states of Ne2+-Ne7+. The processes with producing DCH states are discussed. For x-ray photon energy larger than 1360 eV, no RA exist and transient plasmas show different features in the DCH spectroscopy.

Monte Carlo simulation of X-ray imaging and spectroscopy experiments using quadric geometry and variance reduction techniques

NASA Astrophysics Data System (ADS)

Golosio, Bruno; Schoonjans, Tom; Brunetti, Antonio; Oliva, Piernicola; Masala, Giovanni Luca

2014-03-01

The simulation of X-ray imaging experiments is often performed using deterministic codes, which can be relatively fast and easy to use. However, such codes are generally not suitable for the simulation of even slightly more complex experimental conditions, involving, for instance, first-order or higher-order scattering, X-ray fluorescence emissions, or more complex geometries, particularly for experiments that combine spatial resolution with spectral information. In such cases, simulations are often performed using codes based on the Monte Carlo method. In a simple Monte Carlo approach, the interaction position of an X-ray photon and the state of the photon after an interaction are obtained simply according to the theoretical probability distributions. This approach may be quite inefficient because the final channels of interest may include only a limited region of space or photons produced by a rare interaction, e.g., fluorescent emission from elements with very low concentrations. In the field of X-ray fluorescence spectroscopy, this problem has been solved by combining the Monte Carlo method with variance reduction techniques, which can reduce the computation time by several orders of magnitude. In this work, we present a C++ code for the general simulation of X-ray imaging and spectroscopy experiments, based on the application of the Monte Carlo method in combination with variance reduction techniques, with a description of sample geometry based on quadric surfaces. We describe the benefits of the object-oriented approach in terms of code maintenance, the flexibility of the program for the simulation of different experimental conditions and the possibility of easily adding new modules. Sample applications in the fields of X-ray imaging and X-ray spectroscopy are discussed. Catalogue identifier: AERO_v1_0 Program summary URL:http://cpc.cs.qub.ac.uk/summaries/AERO_v1_0.html Program obtainable from: CPC Program Library, Queen’s University, Belfast, N. Ireland

Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

PubMed Central

Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

2016-01-01

We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions. PMID:27324109

Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

NASA Astrophysics Data System (ADS)

Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

2016-06-01

We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions.

Insights into electron and ion acceleration and transport from x-ray and gamma-ray imaging spectroscopy

NASA Astrophysics Data System (ADS)

Hurford, Gordon J.; Krucker, Samuel

The previous solar maximum has featured high resolution imaging/spectroscopy observations at hard x-ray and gamma-ray energies by the Reuven Ramaty High Energy Solar/Spectroscopic Imager (RHESSI). Highlights of these observations will be reviewed, along with their impli-cations for our understanding of ion and electron acceleration and transport processes. The results to date have included new insights into the location of the acceleration region and the thick target model, a new appreciation of the significance of x-ray albedo, observation of coronal gamma-ray sources and their implications for electron trapping, and indications of differences in the acceleration and transport between electrons and ions. The role of RHESSI's observational strengths and weaknesses in determining the character of its scientific results will also be discussed and used to identify what aspects of the acceleration and transport processes must await the next generation of instrumentation. The extent to which new instrumentation now under development, such as Solar Orbiter/STIX, GRIPS, and FOXSI, can address these open issues will be outlined.

Investigating the local structure of B-site cations in (1-x)BaTiO3-xBiScO3 and (1-x)PbTiO3-xBiScO3 using X-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Blanchard, Peter E. R.; Grosvenor, Andrew P.

2018-05-01

The structural properties of (1-x)BaTiO3-xBiScO3 and (1-x)PbTiO3-xBiScO3 were investigated using powder X-ray diffraction and X-ray absorption spectroscopy. Diffraction measurements confirmed that substituting small amounts of BiScO3 into BaTiO3 initially stabilizes a cubic phase at x = 0.2 before impurity phases begin to form at x = 0.5. BiScO3 substitution also resulted in noticeable changes in the local coordination environment of Ti4+. X-ray absorption near-edge spectroscopy (XANES) analysis showed that replacing Ti4+ with Sc3+ results in an increase in the off-centre displacement of Ti4+ cations. Surprisingly, BiScO3 substitution has no effect on the displacement of the Ti4+ cation in the (1-x)PbTiO3-xBiScO3 solid solution.

Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers

DOE PAGES

Kern, Jan; Yachandra, Vittal K.; Yano, Junko

2015-09-02

We have studied the structure of enzymes and the chemistry at the catalytic sites, intensively and have acquired an understanding of the atomic-scale chemistry which requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the samplemore » is destroyed. Our review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.« less

Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kern, Jan; Yachandra, Vittal K.; Yano, Junko

We have studied the structure of enzymes and the chemistry at the catalytic sites, intensively and have acquired an understanding of the atomic-scale chemistry which requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the samplemore » is destroyed. Our review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.« less

X ray spectra of X Per. [oso-8 observations

NASA Technical Reports Server (NTRS)

Becker, R. H.; Boldt, E. A.; Holt, S. S.; Pravdo, S. H.; Robinson-Saba, J.; Serlemitsos, P. J.; Swank, J. H.

1978-01-01

The cosmic X-ray spectroscopy experiment on OSO-8 observed X Per for twenty days during two observations in Feb. 1976 and Feb. 1977. The spectrum of X Per varies in phase with its 13.9 min period, hardening significantly at X-ray minimum. Unlike other X-ray binary pulsar spectra, X Per's spectra do not exhibit iron line emission or strong absorption features. The data show no evidence for a 22 hour periodicity in the X-ray intensity of X Per. These results indicate that the X-ray emission from X Per may be originating from a neutron star in a low density region far from the optically identified Be star.

Single and double core-hole ion emission spectroscopy of transient neon plasmas produced by ultraintense x-ray laser pulses

NASA Astrophysics Data System (ADS)

Gao, Cheng; Zeng, Jiaolong; Yuan, Jianmin

2016-05-01

Single core-hole (SCH) and double core-hole (DCH) spectroscopy is investigated systematically for neon gas in the interaction with ultraintense x-ray pulses with photon energy from 937 eV to 2000 eV. A time-dependent rate equation, implemented in the detailed level accounting approximation, is utilized to study the dynamical evolution of the level population and emission properties of the laser-produced highly transient plasmas. The plasma density effects on level populations are demonstrated with an x-ray photon energy of 2000 eV. For laser photon energy in the range of 937 - 1360 eV, resonant absorptions (RA) of 1s-np (n> = 2) transitions play important roles in time evolution of the population and DCH emission spectroscopy. For x-ray photon energy larger than 1360 eV, no RA exist and transient plasmas show different features in the DCH spectroscopy.

REDSoX: Monte-Carlo ray-tracing for a soft x-ray spectroscopy polarimeter

NASA Astrophysics Data System (ADS)

Günther, Hans M.; Egan, Mark; Heilmann, Ralf K.; Heine, Sarah N. T.; Hellickson, Tim; Frost, Jason; Marshall, Herman L.; Schulz, Norbert S.; Theriault-Shay, Adam

2017-08-01

X-ray polarimetry offers a new window into the high-energy universe, yet there has been no instrument so far that could measure the polarization of soft X-rays (about 17-80 Å) from astrophysical sources. The Rocket Experiment Demonstration of a Soft X-ray Polarimeter (REDSoX Polarimeter) is a proposed sounding rocket experiment that uses a focusing optic and splits the beam into three channels. Each channel has a set of criticalangle transmission (CAT) gratings that disperse the x-rays onto a laterally graded multilayer (LGML) mirror, which preferentially reflects photons with a specific polarization angle. The three channels are oriented at 120 deg to each other and thus measure the three Stokes parameters: I, Q, and U. The period of the LGML changes with position. The main design challenge is to arrange the gratings so that they disperse the spectrum in such a way that all rays are dispersed onto the position on the multi-layer mirror where they satisfy the local Bragg condition despite arriving on the mirror at different angles due to the converging beam from the focusing optics. We present a polarimeteric Monte-Carlo ray-trace of this design to assess non-ideal effects from e.g. mirror scattering or the finite size of the grating facets. With mirror properties both simulated and measured in the lab for LGML mirrors of 80-200 layers we show that the reflectivity and the width of the Bragg-peak are sufficient to make this design work when non-ideal effects are included in the simulation. Our simulations give us an effective area curve, the modulation factor and the figure of merit for the REDSoX polarimeter. As an example, we simulate an observation of Mk 421 and show that we could easily detect a 20% linear polarization.

Is scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) quantitative?

PubMed

Newbury, Dale E; Ritchie, Nicholas W M

2013-01-01

Scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) is a widely applied elemental microanalysis method capable of identifying and quantifying all elements in the periodic table except H, He, and Li. By following the "k-ratio" (unknown/standard) measurement protocol development for electron-excited wavelength dispersive spectrometry (WDS), SEM/EDS can achieve accuracy and precision equivalent to WDS and at substantially lower electron dose, even when severe X-ray peak overlaps occur, provided sufficient counts are recorded. Achieving this level of performance is now much more practical with the advent of the high-throughput silicon drift detector energy dispersive X-ray spectrometer (SDD-EDS). However, three measurement issues continue to diminish the impact of SEM/EDS: (1) In the qualitative analysis (i.e., element identification) that must precede quantitative analysis, at least some current and many legacy software systems are vulnerable to occasional misidentification of major constituent peaks, with the frequency of misidentifications rising significantly for minor and trace constituents. (2) The use of standardless analysis, which is subject to much broader systematic errors, leads to quantitative results that, while useful, do not have sufficient accuracy to solve critical problems, e.g. determining the formula of a compound. (3) EDS spectrometers have such a large volume of acceptance that apparently credible spectra can be obtained from specimens with complex topography that introduce uncontrolled geometric factors that modify X-ray generation and propagation, resulting in very large systematic errors, often a factor of ten or more. © Wiley Periodicals, Inc.

Gamma ray spectroscopy in astrophysics. [conferences

NASA Technical Reports Server (NTRS)

Cline, T. L. (Editor); Ramaty, R. (Editor)

1978-01-01

Experimental and theoretical aspects of gamma ray spectroscopy in high energy astrophysics are discussed. Line spectra from solar, stellar, planetary, and cosmic gamma rays are examined as well as HEAO investigations, the prospects of a gamma ray observatory, and follow-on X-ray experiments in space.

Scanning electron microscope/energy dispersive x ray analysis of impact residues in LDEF tray clamps

NASA Technical Reports Server (NTRS)

Bernhard, Ronald P.; Durin, Christian; Zolensky, Michael E.

1993-01-01

Detailed optical scanning of tray clamps is being conducted in the Facility for the Optical Inspection of Large Surfaces at JSC to locate and document impacts as small as 40 microns in diameter. Residues from selected impacts are then being characterized by Scanning Electron Microscopy/Energy Dispersive X-ray Analysis at CNES. Results from this analysis will be the initial step to classifying projectile residues into specific sources.

Direct observation of X-ray induced atomic motion using scanning tunneling microscope combined with synchrotron radiation.

PubMed

Saito, Akira; Tanaka, Takehiro; Takagi, Yasumasa; Hosokawa, Hiromasa; Notsu, Hiroshi; Ohzeki, Gozo; Tanaka, Yoshihito; Kohmura, Yoshiki; Akai-Kasaya, Megumi; Ishikawa, Tetsuya; Kuwahara, Yuji; Kikuta, Seishi; Aono, Masakazu

2011-04-01

X-ray induced atomic motion on a Ge(111)-c(2 x 8) clean surface at room temperature was directly observed with atomic resolution using a synchrotron radiation (SR)-based scanning tunneling microscope (STM) system under ultra high vacuum condition. The atomic motion was visualized as a tracking image by developing a method to merge the STM images before and after X-ray irradiation. Using the tracking image, the atomic mobility was found to be strongly affected by defects on the surface, but was not dependent on the incident X-ray energy, although it was clearly dependent on the photon density. The atomic motion can be attributed to surface diffusion, which might not be due to core-excitation accompanied with electronic transition, but a thermal effect by X-ray irradiation. The crystal surface structure was possible to break even at a lower photon density than the conventionally known barrier. These results can alert X-ray studies in the near future about sample damage during measurements, while suggesting the possibility of new applications. Also the obtained results show a new availability of the in-situ SR-STM system.

Characterization of Gas Hydrate Samples from IODP 311 using High Resolution Raman Spectroscopy, X-ray Diffraction and Differential Scanning Calorimetry

NASA Astrophysics Data System (ADS)

Schicks, J. M.; Ziemann, M. A.; Naumann, R.; Erzinger, J.

2006-12-01

Investigations on hydrate bearing sediments taken from different locations (Gulf of Mexico, Sea of Okhotsk, etc.) lead to the conclusion that the coexistence of gas hydrates with different structures and compositions in nature is possible (Sassen et al. 2000, Takeya et al 2006). The aim of this study is to get more information about the variation in local composition of gas hydrates in samples from IODP Leg 311 (Hole 1328) using Raman spectroscopy. Therefore, in addition to investigations performed at the same samples by Lu et al., experiments in this study have been carried out with a confocal Raman microprobe in high lateral and spectral resolution mode. The samples have been analysed at 153 K and at atmospheric pressure (single spots, line scans, area mapping). The specified structure I hydrates contain methane and H2S. The Raman bands at 2569 cm-1 and 2593 cm-1 indicate H2S in large and small cages, respectively. Further information is provided about the variation of the CH4-H2S- composition and the cage occupancy of the sample. The samples have also been investigated with X-ray diffraction and differential scanning calorimetry (DSC). DSC measurements hint at the coexistence of two different gas hydrates with significantly different decomposition temperatures at atmospheric pressure (206 K and 247 K). This could be caused by variable amounts of H2S incorporated in the hydrate lattice. The results from the investigation on the IODP Leg 311 samples are compared and discussed with results of similar investigations on samples of structure I hydrate from Mallik 5L-38 drill hole in the permafrost of NW Canada. References: R. Sassen, S.T. Sweet, D.A. DeFreitas, A.V. Milkov, 2000. Organic Geochemistry, 31, 1257-1262. S. Takeya, M. Kida, H. Minami, H. Sakagami, A. Hachikubo, N. Takahashi, H. Shoji, V. Soloviev, K. Wallmann, N. Biebow, A. Obzhirov, A Salomatin, J. Poort, 2006. Chemical Engineering Science, 61, 2670- 2674.

Imaging of intracellular fatty acids by scanning X-ray fluorescence microscopy

PubMed Central

Shimura, Mari; Shindou, Hideo; Szyrwiel, Lukasz; Tokuoka, Suzumi M.; Hamano, Fumie; Matsuyama, Satoshi; Okamoto, Mayumi; Matsunaga, Akihiro; Kita, Yoshihiro; Ishizaka, Yukihito; Yamauchi, Kazuto; Kohmura, Yoshiki; Lobinski, Ryszard; Shimizu, Isao; Shimizu, Takao

2016-01-01

Fatty acids are taken up by cells and incorporated into complex lipids such as neutral lipids and glycerophospholipids. Glycerophospholipids are major constituents of cellular membranes. More than 1000 molecular species of glycerophospholipids differ in their polar head groups and fatty acid compositions. They are related to cellular functions and diseases and have been well analyzed by mass spectrometry. However, intracellular imaging of fatty acids and glycerophospholipids has not been successful due to insufficient resolution using conventional methods. Here, we developed a method for labeling fatty acids with bromine (Br) and applied scanning X-ray fluorescence microscopy (SXFM) to obtain intracellular Br mapping data with submicrometer resolution. Mass spectrometry showed that cells took up Br-labeled fatty acids and metabolized them mainly into glycerophospholipids in CHO cells. Most Br signals observed by SXFM were in the perinuclear region. Higher resolution revealed a spot-like distribution of Br in the cytoplasm. The current method enabled successful visualization of intracellular Br-labeled fatty acids. Single-element labeling combined with SXFM technology facilitates the intracellular imaging of fatty acids, which provides a new tool to determine dynamic changes in fatty acids and their derivatives at the single-cell level.—Shimura, M., Shindou, H., Szyrwiel, L., Tokuoka, S. M., Hamano, F., Matsuyama, S., Okamoto, M., Matsunaga, A., Kita, Y., Ishizaka, Y., Yamauchi, K., Kohmura, Y., Lobinski, R., Shimizu, I., Shimizu, T. Imaging of intracellular fatty acids by scanning X-ray fluorescence microscopy. PMID:27601443

High-Resolution Spectroscopy with the Chandra X-ray Observatory

ScienceCinema

Canizares, Claude R. [MIT, Cambridge, Massachusetts, United States

2017-12-09

The capabilities of the Chandra X-ray Observatory and XMM-Newton for high-resolution spectroscopy have brought tradition plasma diagnostic techniques to the study of cosmic plasma. Observations have probed nearly every class of astronomical object, from young proto-starts through massive O starts and black hole binaries, supernova remnants, active galactic nuclei, and the intergalactic medium. Many of these sources show remarkable rich spectra that reveal new physical information, such as emission measure distributions, elemental abundances, accretion disk and wind signatures, and time variability. This talk will present an overview of the Chandra instrumentaton and selected examples of spectral observations of astrophysical and cosmological importance.

X-ray spectroscopy of the mixed morphology supernova remnant W 28 with XMM-Newton

NASA Astrophysics Data System (ADS)

Nakamura, Ryoko; Bamba, Aya; Ishida, Manabu; Yamazaki, Ryo; Tatematsu, Ken'ichi; Kohri, Kazunori; Pühlhofer, Gerd; Wagner, Stefan J.; Sawada, Makoto

2014-06-01

We report on spatially resolved X-ray spectroscopy of the north-eastern part of the mixed morphology supernova remnant (SNR) W 28 with XMM-Newton. The observed field of view includes a prominent and twisted shell emission forming the edge of this SNR as well as part of the center-filled X-ray emission brightening toward the south-west edge of the field of view. The shell region spectra are in general represented by an optically thin thermal plasma emission in collisional ionization equilibrium with a temperature of ˜ 0.3 keV and a density of ˜ 10 cm-3, which is much higher than the density obtained for inner parts. In contrast, we detected no significant X-ray flux from one of the TeV γ-ray peaks with an upper-limit flux of 2.1 × 10-14 erg cm-2 s-1 in the 2-10 keV band. The large flux ratio of TeV to X-ray, larger than 16, and the spatial coincidence of the molecular cloud and the TeV γ-ray emission site indicate that the TeV γ-ray of W 28 is π0-decay emission originating from collisions between accelerated protons and molecular cloud protons. Comparing the spectrum in the TeV band and the X-ray upper limit, we obtained a weak upper limit on the magnetic field strength B ≲ 1500 μG.

Data reduction and analysis for the graphite crystal X-ray spectrometer and polarimeter experiment flown aboard OSO-8 spacecraft

NASA Technical Reports Server (NTRS)

Novick, R.

1980-01-01

The documentation and software programs developed for the reception, initial processing (quickbook), and production analysis of data obtained by solar X-ray spectroscopy, stellar spectroscopy, and X-ray polarimetry experiments on OSO-8 are listed. The effectiveness and sensitivity of the Bragg crystal scattering instruments used are assessed. The polarization data polarimetric data obtained shows that some X-ray sources are polarized and that a larger polarimeter of this type is required to perform the measurements necessary to fully understand the physics of X-ray sources. The scanning Bragg crystal spectrometer was ideally suited for studying rapidly changing solar conditions. Observations of the Crab Nebula and pulsar, Cyg X-1, Cyg X-2, Cyg X-3, Sco X-1, Cen X-3, and Her X-1 are discussed as well as of 4U1656-53 and 4U1820-30. Evidence was obtained for iron line emission from Cyg X-3.

Dual energy scanning beam laminographic x-radiography

DOEpatents

Majewski, Stanislaw; Wojcik, Randolph F.

1998-01-01

A multiple x-ray energy level imaging system includes a scanning x-ray beam and two detector design having a first low x-ray energy sensitive detector and a second high x-ray energy sensitive detector. The low x-ray energy detector is placed next to or in front of the high x-ray energy detector. The low energy sensitive detector has small stopping power for x-rays. The lower energy x-rays are absorbed and converted into electrical signals while the majority of the higher energy x-rays pass through undetected. The high energy sensitive detector has a large stopping power for x-rays as well as it having a filter placed between it and the object to absorb the lower energy x-rays. In a second embodiment; a single energy sensitive detector is provided which provides an output signal proportional to the amount of energy in each individual x-ray it absorbed. It can then have an electronic threshold or thresholds set to select two or more energy ranges for the images. By having multiple detectors located at different positions, a dual energy laminography system is possible.

Dual energy scanning beam laminographic x-radiography

DOEpatents

Majewski, S.; Wojcik, R.F.

1998-04-21

A multiple x-ray energy level imaging system includes a scanning x-ray beam and two detector design having a first low x-ray energy sensitive detector and a second high x-ray energy sensitive detector. The low x-ray energy detector is placed next to or in front of the high x-ray energy detector. The low energy sensitive detector has small stopping power for x-rays. The lower energy x-rays are absorbed and converted into electrical signals while the majority of the higher energy x-rays pass through undetected. The high energy sensitive detector has a large stopping power for x-rays as well as it having a filter placed between it and the object to absorb the lower energy x-rays. In a second embodiment; a single energy sensitive detector is provided which provides an output signal proportional to the amount of energy in each individual x-ray it absorbed. It can then have an electronic threshold or thresholds set to select two or more energy ranges for the images. By having multiple detectors located at different positions, a dual energy laminography system is possible. 6 figs.

Continuous motion scan ptychography: characterization for increased speed in coherent x-ray imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deng, Junjing; Nashed, Youssef S. G.; Chen, Si

2015-01-01

Ptychography is a coherent diffraction imaging (CDI) method for extended objects in which diffraction patterns are acquired sequentially from overlapping coherent illumination spots. The object's complex transmission function can be reconstructed from those diffraction patterns at a spatial resolution limited only by the scattering strength of the object and the detector geometry. Most experiments to date have positioned the illumination spots on the sample using a move-settle-measure sequence in which the move and settle steps can take longer to complete than the measure step. We describe here the use of a continuous "fly-scan" mode for ptychographic data collection in whichmore » the sample is moved continuously, so that the experiment resembles one of integrating the diffraction patterns from multiple probe positions. This allows one to use multiple probe mode reconstruction methods to obtain an image of the object and also of the illumination function. We show in simulations, and in x-ray imaging experiments, some of the characteristics of fly-scan ptychography, including a factor of 25 reduction in the data acquisition time. This approach will become increasingly important as brighter x-ray sources are developed, such as diffraction limited storage rings.« less

Continuous motion scan ptychography: characterization for increased speed in coherent x-ray imaging.

PubMed

Deng, Junjing; Nashed, Youssef S G; Chen, Si; Phillips, Nicholas W; Peterka, Tom; Ross, Rob; Vogt, Stefan; Jacobsen, Chris; Vine, David J

2015-03-09

Ptychography is a coherent diffraction imaging (CDI) method for extended objects in which diffraction patterns are acquired sequentially from overlapping coherent illumination spots. The object's complex transmission function can be reconstructed from those diffraction patterns at a spatial resolution limited only by the scattering strength of the object and the detector geometry. Most experiments to date have positioned the illumination spots on the sample using a move-settle-measure sequence in which the move and settle steps can take longer to complete than the measure step. We describe here the use of a continuous "fly-scan" mode for ptychographic data collection in which the sample is moved continuously, so that the experiment resembles one of integrating the diffraction patterns from multiple probe positions. This allows one to use multiple probe mode reconstruction methods to obtain an image of the object and also of the illumination function. We show in simulations, and in x-ray imaging experiments, some of the characteristics of fly-scan ptychography, including a factor of 25 reduction in the data acquisition time. This approach will become increasingly important as brighter x-ray sources are developed, such as diffraction limited storage rings.

Revealing the electronic structure of LiC 6 by soft X-ray spectroscopy

DOE PAGES

Zhang, L.; Li, X.; Augustsson, A.; ...

2017-03-09

The electronic structure of LiC 6 has been investigated in this paper by soft X-ray absorption and emission spectroscopies. The results reveal that upon full lithiation of graphite, the Li 2s electrons are transferred into the carbon π* states in a near rigid-band behavior, resulting in the increased density of states near E F and the shift of σ* states to lower energies. Finally, in addition, the resonant inelastic X-ray scattering spectra of LiC 6 do not show strong dispersive features as that of graphite, indicating that the crystal momentum is not conserved during the scattering process due to themore » delocalization of electrons in the intermediate state.« less

PtyNAMi: ptychographic nano-analytical microscope at PETRA III: interferometrically tracking positions for 3D x-ray scanning microscopy using a ball-lens retroreflector

NASA Astrophysics Data System (ADS)

Schroer, Christian G.; Seyrich, Martin; Kahnt, Maik; Botta, Stephan; Döhrmann, Ralph; Falkenberg, Gerald; Garrevoet, Jan; Lyubomirskiy, Mikhail; Scholz, Maria; Schropp, Andreas; Wittwer, Felix

2017-09-01

In recent years, ptychography has revolutionized x-ray microscopy in that it is able to overcome the diffraction limit of x-ray optics, pushing the spatial resolution limit down to a few nanometers. However, due to the weak interaction of x rays with matter, the detection of small features inside a sample requires a high coherent fluence on the sample, a high degree of mechanical stability, and a low background signal from the x-ray microscope. The x-ray scanning microscope PtyNAMi at PETRA III is designed for high-spatial-resolution 3D imaging with high sensitivity. The design concept is presented with a special focus on real-time metrology of the sample position during tomographic scanning microscopy.

Methods development for diffraction and spectroscopy studies of metalloenzymes at X-ray free-electron lasers

PubMed Central

Kern, Jan; Hattne, Johan; Tran, Rosalie; Alonso-Mori, Roberto; Laksmono, Hartawan; Gul, Sheraz; Sierra, Raymond G.; Rehanek, Jens; Erko, Alexei; Mitzner, Rolf; Wernet, Phillip; Bergmann, Uwe; Sauter, Nicholas K.; Yachandra, Vittal; Yano, Junko

2014-01-01

X-ray free-electron lasers (XFELs) open up new possibilities for X-ray crystallographic and spectroscopic studies of radiation-sensitive biological samples under close to physiological conditions. To facilitate these new X-ray sources, tailored experimental methods and data-processing protocols have to be developed. The highly radiation-sensitive photosystem II (PSII) protein complex is a prime target for XFEL experiments aiming to study the mechanism of light-induced water oxidation taking place at a Mn cluster in this complex. We developed a set of tools for the study of PSII at XFELs, including a new liquid jet based on electrofocusing, an energy dispersive von Hamos X-ray emission spectrometer for the hard X-ray range and a high-throughput soft X-ray spectrometer based on a reflection zone plate. While our immediate focus is on PSII, the methods we describe here are applicable to a wide range of metalloenzymes. These experimental developments were complemented by a new software suite, cctbx.xfel. This software suite allows for near-real-time monitoring of the experimental parameters and detector signals and the detailed analysis of the diffraction and spectroscopy data collected by us at the Linac Coherent Light Source, taking into account the specific characteristics of data measured at an XFEL. PMID:24914169

The use of C-near edge X-ray absorption fine structure spectroscopy for the elaboration of chemistry in lignocellulosics

Treesearch

Lucian A. Lucia; Hiroki Nanko; Alan W. Rudie; Doug G. Mancosky; Sue Wirick

2006-01-01

The research presented elucidates the oxidation chemistry occurring in hydrogen peroxide bleached kraft pulp fibers by employing carbon near edge x-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft x-ray technique that selectively interrogates atomic moieties using photoelectrons (Xrays) of variable energies. The X1A beam line at the National...

Novel visualization studies of lignocellulosic oxidation chemistry by application of C-near edge X-ray absorption fine structure spectroscopy

Treesearch

Douglas G. Mancosky; Lucian A. Lucia; Hiroki Nanko; Sue Wirick; Alan W. Rudie; Robert Braun

2005-01-01

The research presented herein is the first attempt to probe the chemical nature of lignocellulosic samples by the application of carbon near edge X-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft X-ray technique that principally provides selective interrogation of discrete atomic moieties using photoelectrons of variable energies. The X1A beam...

Femtosecond time-resolved X-ray absorption spectroscopy of anatase TiO2 nanoparticles using XFEL

PubMed Central

Obara, Yuki; Ito, Hironori; Ito, Terumasa; Kurahashi, Naoya; Thürmer, Stephan; Tanaka, Hiroki; Katayama, Tetsuo; Togashi, Tadashi; Owada, Shigeki; Yamamoto, Yo-ichi; Karashima, Shutaro; Nishitani, Junichi; Yabashi, Makina; Suzuki, Toshinori; Misawa, Kazuhiko

2017-01-01

The charge-carrier dynamics of anatase TiO2 nanoparticles in an aqueous solution were studied by femtosecond time-resolved X-ray absorption spectroscopy using an X-ray free electron laser in combination with a synchronized ultraviolet femtosecond laser (268 nm). Using an arrival time monitor for the X-ray pulses, we obtained a temporal resolution of 170 fs. The transient X-ray absorption spectra revealed an ultrafast Ti K-edge shift and a subsequent growth of a pre-edge structure. The edge shift occurred in ca. 100 fs and is ascribed to reduction of Ti by localization of generated conduction band electrons into shallow traps of self-trapped polarons or deep traps at penta-coordinate Ti sites. Growth of the pre-edge feature and reduction of the above-edge peak intensity occur with similar time constants of 300–400 fs, which we assign to the structural distortion dynamics near the surface. PMID:28713842

Micromorphology of sialoliths in submandibular salivary gland: a scanning electron microscope and X-ray diffraction analysis.

PubMed

Kasaboğlu, Oğuzcan; Er, Nuray; Tümer, Celal; Akkocaoğlu, Murat

2004-10-01

Sialoliths are common in the submandibular gland and its duct system. The exact cause of formation of a sialolith is still a matter of debate. The aim of this study was to analyze 6 sialoliths ultrastructurally to determine their development mechanism in the submandibular salivary glands. Six sialoliths retrieved from the hilus and duct of the submandibular salivary glands of 6 patients with sialadenitis were analyzed ultrastructurally by scanning electron microscope and x-ray diffractometer. Scanning electron microscope revealed mainly irregular, partly rudely hexagonal, needle-like and plate-shaped crystals. The cross-section from the surface to the inner part of the sialoliths showed no organic material. X-ray diffraction showed that the sialoliths were composed of hydroxyapatite crystals. Energy dispersive x-ray microanalysis showed that all of the samples contained high levels of Ca and P, and small amounts of Mg, Na, Cl, Si, Fe, and K. The main structures of the submandibular sialoliths were found to be hydroxyapatite crystals. No organic cores were observed in the central parts of the sialoliths. In accordance with these preliminary results, sialoliths in the submandibular salivary glands may arise secondary to sialadenitis, but not via a luminal organic nidus.

Scanning X-ray diffraction on cardiac tissue: automatized data analysis and processing.

PubMed

Nicolas, Jan David; Bernhardt, Marten; Markus, Andrea; Alves, Frauke; Burghammer, Manfred; Salditt, Tim

2017-11-01

A scanning X-ray diffraction study of cardiac tissue has been performed, covering the entire cross section of a mouse heart slice. To this end, moderate focusing by compound refractive lenses to micrometer spot size, continuous scanning, data acquisition by a fast single-photon-counting pixel detector, and fully automated analysis scripts have been combined. It was shown that a surprising amount of structural data can be harvested from such a scan, evaluating the local scattering intensity, interfilament spacing of the muscle tissue, the filament orientation, and the degree of anisotropy. The workflow of data analysis is described and a data analysis toolbox with example data for general use is provided. Since many cardiomyopathies rely on the structural integrity of the sarcomere, the contractile unit of cardiac muscle cells, the present study can be easily extended to characterize tissue from a diseased heart.

High resolution x-ray absorption and emission spectroscopy of Li x CoO2 single crystals as a function delithiation

NASA Astrophysics Data System (ADS)

Simonelli, L.; Paris, E.; Iwai, C.; Miyoshi, K.; Takeuchi, J.; Mizokawa, T.; Saini, N. L.

2017-03-01

The effect of delithiation in Li x CoO2 is studied by high resolution Co K-edge x-ray absorption and x-ray emission spectroscopy. Polarization dependence of the x-ray absorption spectra on single crystal samples is exploited to reveal information on the anisotropic electronic structure. We find that the electronic structure of Li x CoO2 is significantly affected by delithiation in which the Co ions oxidation state tending to change from 3+  to 4+. The Co intersite (intrasite) 4p-3d hybridization suffers a decrease (increase) by delithiation. The unoccupied 3d t 2g orbitals with a 1g symmetry, containing substantial O 2p character, hybridize isotropically with Co 4p orbitals and likely to have itinerant character unlike anisotropically hybridized 3d e g orbitals. Such a peculiar electronic structure could have significant effect on the mobility of Li in Li x CoO2 cathode and hence the battery characteristics.

Spectra of cosmic X-ray sources

NASA Technical Reports Server (NTRS)

Holt, S. S.; Mccray, R.

1982-01-01

X-ray measurements provide the most direct probes of astrophysical environments with temperatures exceeding one million K. Progress in experimental research utilizing dispersive techniques (e.g., Bragg and grating spectroscopy) is considerably slower than that in areas utilizing photometric techniques, because of the relative inefficiency of the former for the weak X-ray signals from celestial sources. As a result, the term "spectroscopy" as applied to X-ray astronomy has traditionally satisfied a much less restrictive definition (in terms of resolving power) than it has in other wavebands. Until quite recently, resolving powers of order unity were perfectly respectable, and still provide (in most cases) the most useful spectroscopic data. In the broadest sense, X-ray photometric measurements are spectroscopic, insofar as they represent samples of the overall electromagnetic continua of celestial objects.

EUV Spectroscopy of High-redshift X-ray Objects

NASA Astrophysics Data System (ADS)

Kowalski, Michael Paul; Wolff, M. T.; Wood, K. S.; Barbee, T. W., Jr.

2010-03-01

As astronomical observations are pushed to cosmological distances (z>3) the spectral energy distributions of X-ray objects, AGNs for example, will have their maxima redshifted into the EUV waveband ( 90-912 Å/0.1-0.01 keV). Consequently, a wealth of spectral diagnostics, provided by, for example, the Fe L-shell complex ( 60-6 Å/0.2-2.0 keV) and the O VII/VIII lines ( 20 Å/0.5 keV), will be lost to X-ray instruments operating at traditional ( 0.5-10 keV) and higher X-ray energies. There are precedents in other wavebands. For example, HST evolutionary studies will become largely the province of JWST. Despite the successes of EUVE, the ROSAT WFC, and the Chandra LETG, the EUV continues to be unappreciated and under-utilized, partly because of a preconception that absorption by neutral galactic Hydrogen in the ISM prevents any useful extragalactic measurements at all EUV wavelengths and, until recently, by a lack of a suitable enabling technology. Thus, if future planned X-ray missions (e.g., IXO, Gen-X) are optimized again for traditional X-ray energies, their performance (effective area, resolving power) will be cut off at ultrasoft X-ray energies or at best be radically reduced in the EUV. This opens up a critical gap in performance located right at short EUV wavelengths, where the critical X-ray spectral transitions occur in high-z objects. However, normal-incidence multilayer-grating technology, which performs best precisely at such wavelengths, together with advanced nano-laminate fabrication techniques have been developed and are now mature to the point where advanced EUV instrument designs with performance complementary to IXO and Gen-X are practical. Such EUV instruments could be flown either independently or as secondary instruments on these X-ray missions. We present here a critical examination of the limits placed on extragalactic EUV measurements by ISM absorption, the range where high-z measurements are practical, and the requirements this imposes on

A flexible gas flow reaction cell for in situ x-ray absorption spectroscopy studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kroner, Anna B., E-mail: anna.kroner@diamond.ac.uk; Gilbert, Martin; Duller, Graham

2016-07-27

A capillary-based sample environment with hot air blower and integrated gas system was developed at Diamond to conduct X-ray absorption spectroscopy (XAS) studies of materials under time-resolved, in situ conditions. The use of a hot air blower, operating in the temperature range of 298-1173 K, allows introduction of other techniques e.g. X-ray diffraction (XRD), Raman spectroscopy for combined techniques studies. The flexibility to use either quartz or Kapton capillaries allows users to perform XAS measurement at energies as low as 5600 eV. To demonstrate performance, time-resolved, in situ XAS results of Rh catalysts during the process of activation (Rh K-edge,more » Ce L{sub 3}-edge and Cr K-edge) and the study of mixed oxide membrane (La{sub 0.6}Sr{sub 0.4}Co{sub 0.2}Fe{sub 0.8}O{sub 3−δ}) under various partial oxygen pressure conditions are described.« less

Combining X-ray and neutron crystallography with spectroscopy.

PubMed

Kwon, Hanna; Smith, Oliver; Raven, Emma Lloyd; Moody, Peter C E

2017-02-01

X-ray protein crystallography has, through the determination of the three-dimensional structures of enzymes and their complexes, been essential to the understanding of biological chemistry. However, as X-rays are scattered by electrons, the technique has difficulty locating the presence and position of H atoms (and cannot locate H + ions), knowledge of which is often crucially important for the understanding of enzyme mechanism. Furthermore, X-ray irradiation, through photoelectronic effects, will perturb the redox state in the crystal. By using single-crystal spectrophotometry, reactions taking place in the crystal can be monitored, either to trap intermediates or follow photoreduction during X-ray data collection. By using neutron crystallography, the positions of H atoms can be located, as it is the nuclei rather than the electrons that scatter neutrons, and the scattering length is not determined by the atomic number. Combining the two techniques allows much greater insight into both reaction mechanism and X-ray-induced photoreduction.

Effect of X-ray exposure on the pharmaceutical quality of drug tablets using X-ray inspection equipment.

PubMed

Uehara, Kazuaki; Tagami, Tatsuaki; Miyazaki, Itaru; Murata, Norikazu; Takahashi, Yoshifumi; Ohkubo, Hiroshi; Ozeki, Tetsuya

2015-06-01

X-ray inspection equipment is widely used to detect missing materials and defective goods in opaque containers. Its application has been expanded to the pharmaceutical industry to detect the presence of drug tablets in aluminum foil press-through packaging. However, the effect of X-rays on the pharmaceutical quality of drug tablets is not well known. In this study, the effect of X-rays on the pharmaceutical quality of drug tablets was investigated. Exposure of acetaminophen, loxoprofen and mefenamic acid tablets to X-ray doses of 0.34 mGy (thrice the dose by X-ray scanning) to 300 Gy (maximum dose from our X-ray equipment) was demonstrated, and the samples were evaluated by formulation tests. Exposure to X-rays did not affect the pharmaceutical quality of the drug content. The samples exposed to X-rays exhibited almost the same profile in formulation tests (dissolution test, disintegrating test and hardness test) as control samples (0 Gy). The combination of X-ray exposure with accelerated temperature and humidity tests (six months) also did not affect the pharmaceutical quality. The color change of light-sensitive drugs (nifedipine and furosemide tablets) after X-ray exposure was negligible (< 1.0). In contrast, tablet color was remarkably changed by light from a D65 lamp. The X-ray scanning and X-ray exposure under our experimental conditions did not affect the pharmaceutical quality of drug tablets.

The Compton-thick AGN fraction from the deepest X-ray spectroscopy in the CDF-S

NASA Astrophysics Data System (ADS)

Corral, A.; Georgantopoulos, I.; Akylas, A.; Ranalli, P.

2017-10-01

Highly obscured AGN, especially Compton-thick (CT) AGN, likely play a key role in the galaxy-AGN co-evolution scenario. They would comprise the early stages of AGN activity, preceding the AGN-feedback/star-formation quenching phase, during which most of both the SMBH and galaxy growth take place. However, the actual CT fraction among the AGN population is still largely unconstrained. The most reliable way of confirming the obscured nature of an AGN by X-ray spectroscopy, but very deep observations are needed to extend local analyses to larger distances. We will present the X-ray spectral analysis of the deepest X-ray data obtained to date, the almost 7Ms observation of the Chandra Deep Field South. The unprecedented depth of this survey allow us to carry out reliable spectral analyses down to a flux limit of 10^{-16} erg cm^{-2} s^{-1} in the hard 2-8 keV band. Besides the new deeper X-ray data, our approach also includes the implementation of Bayesian inference in the determination of the CT fraction. Our results favor X-ray background synthesis models which postulate a moderate fraction (25%) of CT objects among the obscured AGN population.

Portable total reflection x-ray fluorescence analysis in the identification of unknown laboratory hazards

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Ying, E-mail: liu.ying.48r@st.kyoto-u.ac.jp; Imashuku, Susumu; Sasaki, Nobuharu

In this study, a portable total reflection x-ray fluorescence (TXRF) spectrometer was used to analyze unknown laboratory hazards that precipitated on exterior surfaces of cooling pipes and fume hood pipes in chemical laboratories. With the aim to examine the accuracy of TXRF analysis for the determination of elemental composition, analytical results were compared with those of wavelength-dispersive x-ray fluorescence spectrometry, scanning electron microscope and energy-dispersive x-ray spectrometry, energy-dispersive x-ray fluorescence spectrometry, inductively coupled plasma atomic emission spectrometry, x-ray diffraction spectrometry (XRD), and x-ray photoelectron spectroscopy (XPS). Detailed comparison of data confirmed that the TXRF method itself was not sufficient tomore » determine all the elements (Z > 11) contained in the samples. In addition, results suggest that XRD should be combined with XPS in order to accurately determine compound composition. This study demonstrates that at least two analytical methods should be used in order to analyze the composition of unknown real samples.« less

Fast two-dimensional grid and transmission X-ray microscopy scanning methods for visualizing and characterizing protein crystals

PubMed Central

Wojdyla, Justyna Aleksandra; Panepucci, Ezequiel; Martiel, Isabelle; Ebner, Simon; Huang, Chia-Ying; Caffrey, Martin; Bunk, Oliver; Wang, Meitian

2016-01-01

A fast continuous grid scan protocol has been incorporated into the Swiss Light Source (SLS) data acquisition and analysis software suite on the macromolecular crystallography (MX) beamlines. Its combination with fast readout single-photon counting hybrid pixel array detectors (PILATUS and EIGER) allows for diffraction-based identification of crystal diffraction hotspots and the location and centering of membrane protein microcrystals in the lipid cubic phase (LCP) in in meso in situ serial crystallography plates and silicon nitride supports. Diffraction-based continuous grid scans with both still and oscillation images are supported. Examples that include a grid scan of a large (50 nl) LCP bolus and analysis of the resulting diffraction images are presented. Scanning transmission X-ray microscopy (STXM) complements and benefits from fast grid scanning. STXM has been demonstrated at the SLS beamline X06SA for near-zero-dose detection of protein crystals mounted on different types of sample supports at room and cryogenic temperatures. Flash-cooled crystals in nylon loops were successfully identified in differential and integrated phase images. Crystals of just 10 µm thickness were visible in integrated phase images using data collected with the EIGER detector. STXM offers a truly low-dose method for locating crystals on solid supports prior to diffraction data collection at both synchrotron microfocusing and free-electron laser X-ray facilities. PMID:27275141

Cosmic X-ray physics

NASA Technical Reports Server (NTRS)

Mccammon, D.; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

1985-01-01

A progress report of research activities carried out in the area of cosmic X-ray physics is presented. The Diffuse X-ray Spectrometer DXS which has been flown twice as a rocket payload is described. The observation times proved to be too small for meaningful X-ray data to be obtained. Data collection and reduction activities from the Ultra-Soft X-ray background (UXT) instrument are described. UXT consists of three mechanically-collimated X-ray gas proportional counters with window/filter combinations which allow measurements in three energy bands, Be (80-110 eV), B (90-187 eV), and O (e84-532 eV). The Be band measurements provide an important constraint on local absorption of X-rays from the hot component of the local interstellar medium. Work has also continued on the development of a calorimetric detector for high-resolution spectroscopy in the 0.1 keV - 8keV energy range.

Multiple pinhole collimator based X-ray luminescence computed tomography

PubMed Central

Zhang, Wei; Zhu, Dianwen; Lun, Michael; Li, Changqing

2016-01-01

X-ray luminescence computed tomography (XLCT) is an emerging hybrid imaging modality, which is able to improve the spatial resolution of optical imaging to hundreds of micrometers for deep targets by using superfine X-ray pencil beams. However, due to the low X-ray photon utilization efficiency in a single pinhole collimator based XLCT, it takes a long time to acquire measurement data. Herein, we propose a multiple pinhole collimator based XLCT, in which multiple X-ray beams are generated to scan a sample at multiple positions simultaneously. Compared with the single pinhole based XLCT, the multiple X-ray beam scanning method requires much less measurement time. Numerical simulations and phantom experiments have been performed to demonstrate the feasibility of the multiple X-ray beam scanning method. In one numerical simulation, we used four X-ray beams to scan a cylindrical object with 6 deeply embedded targets. With measurements from 6 angular projections, all 6 targets have been reconstructed successfully. In the phantom experiment, we generated two X-ray pencil beams with a collimator manufactured in-house. Two capillary targets with 0.6 mm edge-to-edge distance embedded in a cylindrical phantom have been reconstructed successfully. With the two beam scanning, we reduced the data acquisition time by 50%. From the reconstructed XLCT images, we found that the Dice similarity of targets is 85.11% and the distance error between two targets is less than 3%. We have measured the radiation dose during XLCT scan and found that the radiation dose, 1.475 mSv, is in the range of a typical CT scan. We have measured the changes of the collimated X-ray beam size and intensity at different distances from the collimator. We have also studied the effects of beam size and intensity in the reconstruction of XLCT. PMID:27446686

Sulfur Speciation in Biochars by Very High Resolution Benchtop Kα X-ray Emission Spectroscopy.

PubMed

Holden, William M; Seidler, Gerald T; Cheah, Singfoong

2018-05-30

The analytical chemistry of sulfur-containing materials poses substantial technical challenges, especially due to the limitations of 33 S NMR and the time-intensive preparations required for wet-chemistry analyses. A number of prior studies have found that synchrotron-based X-ray absorption near edge structure (XANES) measurements can give detailed speciation of sulfur chemistry in such cases. However, due to the obvious access limitations, synchrotron XANES of sulfur cannot be part of routine analytical practice across the chemical sciences community. Here, in a study of the sulfur chemistry in biochars, we compare and contrast the chemical inferences available from synchrotron XANES with that given by benchtop, extremely high resolution wavelength-dispersive X-ray fluorescence (WD-XRF) spectroscopy, also often called X-ray emission spectroscopy (XES). While the XANES spectra have higher total information content, often giving differentiation between different moieties having the same oxidation state, the lower sensitivity of the S Kα XES to coordination and local structure provides pragmatic benefit for the more limited goal of quantifying the S oxidation state distribution. Within that constrained metric, we find good agreement between the two methods. As the sulfur concentrations were as low as 150 ppm, these measurements provide proof-of-principle for characterization of the sulfur chemistry of biochars and potential applications to other areas such as soils, batteries, catalysts, and fossil fuels and their combustion products.

Research relative to high energy astrophysics. [large area modular array of reflectors, X-ray spectroscopy, and thermal control

NASA Technical Reports Server (NTRS)

Gorenstein, P.

1984-01-01

Various parameters which affect the design of the proposed large area modular array of reflectors (LAMAR) are considered, including thermal control, high resolution X-ray spectroscopy, pointing control, and mirror performance. The LAMAR instrument is to be a shuttle-launched X-ray observatory to carry out cosmic X-ray investigations. The capabilities of LAMAR are enumerated. Angular resolution performance of the mirror module prototype was measured to be 30 sec of ARC for 50% of the power. The LAMAR thermal pre-collimator design concepts and test configurations are discussed in detail.

Visualizing chemical states and defects induced magnetism of graphene oxide by spatially-resolved-X-ray microscopy and spectroscopy.

PubMed

Wang, Y F; Singh, Shashi B; Limaye, Mukta V; Shao, Y C; Hsieh, S H; Chen, L Y; Hsueh, H C; Wang, H T; Chiou, J W; Yeh, Y C; Chen, C W; Chen, C H; Ray, Sekhar C; Wang, J; Pong, W F; Takagi, Y; Ohigashi, T; Yokoyama, T; Kosugi, N

2015-10-20

This investigation studies the various magnetic behaviors of graphene oxide (GO) and reduced graphene oxides (rGOs) and elucidates the relationship between the chemical states that involve defects therein and their magnetic behaviors in GO sheets. Magnetic hysteresis loop reveals that the GO is ferromagnetic whereas photo-thermal moderately reduced graphene oxide (M-rGO) and heavily reduced graphene oxide (H-rGO) gradually become paramagnetic behavior at room temperature. Scanning transmission X-ray microscopy and corresponding X-ray absorption near-edge structure spectroscopy were utilized to investigate thoroughly the variation of the C 2p(π*) states that are bound with oxygen-containing and hydroxyl groups, as well as the C 2p(σ*)-derived states in flat and wrinkle regions to clarify the relationship between the spatially-resolved chemical states and the magnetism of GO, M-rGO and H-rGO. The results of X-ray magnetic circular dichroism further support the finding that C 2p(σ*)-derived states are the main origin of the magnetism of GO. Based on experimental results and first-principles calculations, the variation in magnetic behavior from GO to M-rGO and to H-rGO is interpreted, and the origin of ferromagnetism is identified as the C 2p(σ*)-derived states that involve defects/vacancies rather than the C 2p(π*) states that are bound with oxygen-containing and hydroxyl groups on GO sheets.

Visualizing chemical states and defects induced magnetism of graphene oxide by spatially-resolved-X-ray microscopy and spectroscopy

PubMed Central

Wang, Y. F.; Singh, Shashi B.; Limaye, Mukta V.; Shao, Y. C.; Hsieh, S. H.; Chen, L. Y.; Hsueh, H. C.; Wang, H. T.; Chiou, J. W.; Yeh, Y. C.; Chen, C. W.; Chen, C. H.; Ray, Sekhar C.; Wang, J.; Pong, W. F.; Takagi, Y.; Ohigashi, T.; Yokoyama, T.; Kosugi, N.

2015-01-01

This investigation studies the various magnetic behaviors of graphene oxide (GO) and reduced graphene oxides (rGOs) and elucidates the relationship between the chemical states that involve defects therein and their magnetic behaviors in GO sheets. Magnetic hysteresis loop reveals that the GO is ferromagnetic whereas photo-thermal moderately reduced graphene oxide (M-rGO) and heavily reduced graphene oxide (H-rGO) gradually become paramagnetic behavior at room temperature. Scanning transmission X-ray microscopy and corresponding X-ray absorption near-edge structure spectroscopy were utilized to investigate thoroughly the variation of the C 2p(π*) states that are bound with oxygen-containing and hydroxyl groups, as well as the C 2p(σ*)-derived states in flat and wrinkle regions to clarify the relationship between the spatially-resolved chemical states and the magnetism of GO, M-rGO and H-rGO. The results of X-ray magnetic circular dichroism further support the finding that C 2p(σ*)-derived states are the main origin of the magnetism of GO. Based on experimental results and first-principles calculations, the variation in magnetic behavior from GO to M-rGO and to H-rGO is interpreted, and the origin of ferromagnetism is identified as the C 2p(σ*)-derived states that involve defects/vacancies rather than the C 2p(π*) states that are bound with oxygen-containing and hydroxyl groups on GO sheets. PMID:26481557

X-ray Raman spectroscopic study of benzene at high pressure.

PubMed

Pravica, Michael; Grubor-Urosevic, Ognjen; Hu, Michael; Chow, Paul; Yulga, Brian; Liermann, Peter

2007-10-11

We have used X-ray Raman spectroscopy (XRS) to study benzene up to approximately 20 GPa in a diamond anvil cell at ambient temperature. The experiments were performed at the High-Pressure Collaborative Access Team's 16 ID-D undulator beamline at the Advanced Photon Source. Scanned monochromatic X-rays near 10 keV were used to probe the carbon X-ray edge near 284 eV via inelastic scattering. The diamond cell axis was oriented perpendicular to the X-ray beam axis to prevent carbon signal contamination from the diamonds. Beryllium gaskets confined the sample because of their high transmission throughput in this geometry. Spectral alterations with pressure indicate bonding changes that occur with pressure because of phase changes (liquid: phase I, II, III, and III') and possibly due to changes in the hybridization of the bonds. Changes in the XRS spectra were especially evident in the data taken when the sample was in phase III', which may be related to a rate process observed in earlier shock wave studies.

EUV spectroscopy of high-redshift x-ray objects

NASA Astrophysics Data System (ADS)

Kowalski, M. P.; Wolff, M. T.; Wood, K. S.; Barbee, T. W., Jr.; Barstow, M. A.

2010-07-01

As astronomical observations are pushed to cosmological distances (z>3) the spectral energy distributions of X-ray objects, AGN for example, will be redshifted into the EUV waveband. Consequently, a wealth of critical spectral diagnostics, provided by, for example, the Fe L-shell complex and the O VII/VIII lines, will be lost to future planned X-ray missions (e.g., IXO, Gen-X) if operated at traditional X-ray energies. This opens up a critical gap in performance located at short EUV wavelengths, where critical X-ray spectral transitions occur in high-z objects. However, normal-incidence multilayer-grating technology, which performs best precisely at such wavelengths, together with advanced nanolaminate replication techniques have been developed and are now mature to the point where advanced EUV instrument designs with performance complementary to IXO and Gen-X are practical. Such EUV instruments could be flown either independently or as secondary instruments on these X-ray missions. We present here a critical examination of the limits placed on extragalactic EUV measurements by ISM absorption, the range where high-z measurements are practical, and the requirements this imposes on next-generation instrument designs. We conclude with a discussion of a breakthrough technology, nanolaminate replication, which enables such instruments.

Composition analysis of a polymer electrolyte membrane fuel cell microporous layer using scanning transmission X-ray microscopy and near edge X-ray absorption fine structure analysis

NASA Astrophysics Data System (ADS)

George, Michael G.; Wang, Jian; Banerjee, Rupak; Bazylak, Aimy

2016-03-01

The novel application of scanning transmission X-ray microscopy (STXM) to the microporous layer (MPL) of a polymer electrolyte membrane fuel cell is investigated. A spatially resolved chemical component distribution map is obtained for the MPL of a commercially available SGL 25 BC sample. This is achieved with near edge X-ray absorption fine structure spectroscopic analysis. Prior to analysis the sample is embedded in non-reactive epoxy and ultra-microtomed to a thickness of 100 nm. Polytetrafluoroethylene (PTFE), carbon particle agglomerates, and supporting epoxy resin distributions are identified and reconstructed for a scanning area of 6 μm × 6 μm. It is observed that the spatial distribution of PTFE is strongly correlated to the carbon particle agglomerations. Additionally, agglomerate structures of PTFE are identified, possibly indicating the presence of a unique mesostructure in the MPL. STXM analysis is presented as a useful technique for the investigation of chemical species distributions in the MPL.

Characterization of Sb-doped Bi(2)UO(6) solid solutions by X-ray diffraction and X-ray absorption spectroscopy.

PubMed

Misra, N L; Yadav, A K; Dhara, Sangita; Mishra, S K; Phatak, Rohan; Poswal, A K; Jha, S N; Sinha, A K; Bhattacharyya, D

2013-01-01

The preparation and characterization of Sb-doped Bi(2)UO(6) solid solutions, in a limited composition range, is reported for the first time. The solid solutions were prepared by solid-state reactions of Bi(2)O(3), Sb(2)O(3) and U(3)O(8) in the required stoichiometry. The reaction products were characterized by X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) measurements at the Bi and U L(3) edges. The XRD patterns indicate the precipitation of additional phases in the samples when Sb doping exceeds 4 at%. The chemical shifts of the Bi absorption edges in the samples, determined from the XANES spectra, show a systematic variation only up to 4 at% of Sb doping and support the results of XRD measurements. These observations are further supported by the local structure parameters obtained by analysis of the EXAFS spectra. The local structure of U is found to remain unchanged upon Sb doping indicating that Sb(+3) ions replace Bi(+3) during the doping of Bi(2)UO(6) by Sb.

Crystals for astronomical X-ray spectroscopy

NASA Technical Reports Server (NTRS)

Burek, A.

1976-01-01

Crystal spectrometric properties and the factors that affect their measurement are discussed. Theoretical and experimental results on KAP are summarized and theoretical results based on the dynamical theory of X-ray diffraction are given for the acid phthalates as well as for the commonly used planes of ADP, PET and EDDT. Anomalous dispersion is found to be important for understanding the details of crystal Bragg reflection properties at long X-ray wavelengths and some important effects are pointed out. The theory of anomalous dispersion is applied to explain the anomalous reflectivity exhibited by KAP at 23.3 A.

X-ray absorption spectroscopy study of Gd3+-loaded ultra-short carbon nanotubes

NASA Astrophysics Data System (ADS)

Ma, Q.; Jebb, M.; Tweedle, M. F.; Wilson, L. J.

2013-04-01

We present an x-ray absorption spectroscopy study of the local structure around the Gd3+ion loaded in ultra short (20-100 nm) carbon nanotubes (GNTs). X-ray Gd L3 absorption near edge structure data shows that the 31.2-μM GNT suspension exhibits a clear characteristic of hydration at the [GdOn] cluster. Extended x-ray absorption fine structure data show that the Gd3+ ion is coordinated by about 9 oxygen ions and that this first coordination shell exhibits an asymmetry similar to that found in triclinic Gd-acetate or Gd[C2H3O2]3·4H2O or GdAc. After correction for the asymmetry using the cumulant of the third order, the Gd-O bond distance is found to be 2.345 Å, instead of 2.406 Å for a symmetrical (or Gaussian) distribution. It is shorter than that in the Gd-containing MRI contrast agents currently in clinical uses. This may account in part for high proton relaxivity observed for the GNT suspension.

Monitoring Ultrafast Chemical Dynamics by Time-Domain X-ray Photo- and Auger-Electron Spectroscopy.

PubMed

Gessner, Oliver; Gühr, Markus

2016-01-19

The directed flow of charge and energy is at the heart of all chemical processes. Extraordinary efforts are underway to monitor and understand the concerted motion of electrons and nuclei with ever increasing spatial and temporal sensitivity. The element specificity, chemical sensitivity, and temporal resolution of ultrafast X-ray spectroscopy techniques hold great promise to provide new insight into the fundamental interactions underlying chemical dynamics in systems ranging from isolated molecules to application-like devices. Here, we focus on the potential of ultrafast X-ray spectroscopy techniques based on the detection of photo- and Auger electrons to provide new fundamental insight into photochemical processes of systems with various degrees of complexity. Isolated nucleobases provide an excellent testing ground for our most fundamental understanding of intramolecular coupling between electrons and nuclei beyond the traditionally applied Born-Oppenheimer approximation. Ultrafast electronic relaxation dynamics enabled by the breakdown of this approximation is the major component of the nucleobase photoprotection mechanisms. Transient X-ray induced Auger electron spectroscopy on photoexcited thymine molecules provides atomic-site specific details of the extremely efficient coupling that converts potentially bond changing ultraviolet photon energy into benign heat. In particular, the time-dependent spectral shift of a specific Auger band is sensitive to the length of a single bond within the molecule. The X-ray induced Auger transients show evidence for an electronic transition out of the initially excited state within only ∼200 fs in contrast to theoretically predicted picosecond population trapping behind a reaction barrier. Photoinduced charge transfer dynamics between transition metal complexes and semiconductor nanostructures are of central importance for many emerging energy and climate relevant technologies. Numerous demonstrations of photovoltaic and

Dynamic electronic collimation method for 3-D catheter tracking on a scanning-beam digital x-ray system

PubMed Central

Dunkerley, David A. P.; Slagowski, Jordan M.; Funk, Tobias; Speidel, Michael A.

2017-01-01

Abstract. Scanning-beam digital x-ray (SBDX) is an inverse geometry x-ray fluoroscopy system capable of tomosynthesis-based 3-D catheter tracking. This work proposes a method of dose-reduced 3-D catheter tracking using dynamic electronic collimation (DEC) of the SBDX scanning x-ray tube. This is achieved through the selective deactivation of focal spot positions not needed for the catheter tracking task. The technique was retrospectively evaluated with SBDX detector data recorded during a phantom study. DEC imaging of a catheter tip at isocenter required 340 active focal spots per frame versus 4473 spots in full field-of-view (FOV) mode. The dose-area product (DAP) and peak skin dose (PSD) for DEC versus full FOV scanning were calculated using an SBDX Monte Carlo simulation code. The average DAP was reduced to 7.8% of the full FOV value, consistent with the relative number of active focal spots (7.6%). For image sequences with a moving catheter, PSD was 33.6% to 34.8% of the full FOV value. The root-mean-squared-deviation between DEC-based 3-D tracking coordinates and full FOV 3-D tracking coordinates was less than 0.1 mm. The 3-D distance between the tracked tip and the sheath centerline averaged 0.75 mm. DEC is a feasible method for dose reduction during SBDX 3-D catheter tracking. PMID:28439521

Scanning Electron Microscopy and X-Ray Microanalysis

NASA Astrophysics Data System (ADS)

Albee, Arden L.

This outstanding volume has managed the nearly impossible task of combining the expertise of all six authors in a lucid and homogeneous style of writing. Subtitled ‘A Text for Biologists, Material Scientists and Geologists,’ the book has evolved from a short course taught each summer at Lehigh University.The book provides a basic knowledge of (1) the electron optics for these instruments a nd their controls, (2) the characteristics of the electron beam-sample interactions, (3) image formation and interpretation, (4) X ray spectrometry and quantitative X ray microanalysis with separate detailed sections on wavelength dispersive and energy dispersive techniques, and (5) specimen preparation, especially for biological materials.

X-ray Emission Line Spectroscopy of Nearby Galaxies

NASA Astrophysics Data System (ADS)

Wang, Daniel

What are the origins of the diffuse soft X-ray emission from non-AGN galaxies? Preliminary analysis of XMM-Newton RGS spectra shows that a substantial fraction of the emission cannot arise from optically-thin thermal plasma, as commonly assumed, and may originate in charge exchange at the interface with neutral gas. We request the support for a comprehensive observing, data analysis, and modeling program to spectroscopically determine the origins of the emission. First, we will use our scheduled XMM-Newton AO-10 368 ks observations of the nearest compact elliptical galaxy M32 to obtain the first spectroscopic calibration of the cumulative soft X-ray emission from the old stellar population and will develop a spectral model for the charge exchange, as well as analysis tools to measure the spatial and kinematic properties of the X-ray line- emitting plasma. Second, we will characterize the truly diffuse emission from the hot plasma and/or its interplay with the neutral gas in a sample of galactic spheroids and active star forming/starburst regions in nearby galaxies observed by XMM-Newton. In particular, we will map out the spatial distributions of key emission lines and measure (or tightly constrain) the kinematics of hot plasma outflows for a few X-ray-emitting regions with high-quality RGS data. For galaxies with insufficient counting statistics in individual emission lines, we will conduct a spectral stacking analysis to constrain the average properties of the X-ray-emitting plasma. We will use the results of these X-ray spectroscopic analyses, together with complementary X-ray CCD imaging/spectral data and observations in other wavelength bands, to test the models of the emission. In addition to the charge exchange, alternative scenarios such as resonance scattering and relic AGN photo-ionization will also be examined for suitable regions. These studies are important to the understanding of the relationship between the diffuse soft X-ray emission and various

Picosecond excimer laser-plasma x-ray source for microscopy, biochemistry, and lithography

NASA Astrophysics Data System (ADS)

Turcu, I. C. Edmond; Ross, Ian N.; Trenda, P.; Wharton, C. W.; Meldrum, R. A.; Daido, Hiroyuki; Schulz, M. S.; Fluck, P.; Michette, Alan G.; Juna, A. P.; Maldonado, Juan R.; Shields, Harry; Tallents, Gregory J.; Dwivedi, L.; Krishnan, J.; Stevens, D. L.; Jenner, T.; Batani, Dimitri; Goodson, H.

1994-02-01

At Rutherford Appleton Laboratory we developed a high repetition rate, picosecond, excimer laser system which generates a high temperature and density plasma source emitting approximately 200 mW (78 mW/sr) x ray average power at h(nu) approximately 1.2 KeV or 0.28 KeV < h(nu) < 0.53 KeV (the `water window'). At 3.37 nm wavelength the spectral brightness of the source is approximately 9 X 1011 photons/s/mm2/mrad2/0.1% bandwidth. The x-ray source serves a large user community for applications such as: scanning and holographic microscopy, the study of the biochemistry of DNA damage and repair, microlithography and spectroscopy.

High resolution x-ray fluorescence spectroscopy - a new technique for site- and spin-selectivity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Xin

1996-12-01

X-ray spectroscopy has long been used to elucidate electronic and structural information of molecules. One of the weaknesses of x-ray absorption is its sensitivity to all of the atoms of a particular element in a sample. Through out this thesis, a new technique for enhancing the site- and spin-selectivity of the x-ray absorption has been developed. By high resolution fluorescence detection, the chemical sensitivity of K emission spectra can be used to identify oxidation and spin states; it can also be used to facilitate site-selective X-ray Absorption Near Edge Structure (XANES) and site-selective Extended X-ray Absorption Fine Structure (EXAFS). Themore » spin polarization in K fluorescence could be used to generate spin selective XANES or spin-polarized EXAFS, which provides a new measure of the spin density, or the nature of magnetic neighboring atoms. Finally, dramatic line-sharpening effects by the combination of absorption and emission processes allow observation of structure that is normally unobservable. All these unique characters can enormously simplify a complex x-ray spectrum. Applications of this novel technique have generated information from various transition-metal model compounds to metalloproteins. The absorption and emission spectra by high resolution fluorescence detection are interdependent. The ligand field multiplet model has been used for the analysis of K{alpha} and K{beta} emission spectra. First demonstration on different chemical states of Fe compounds has shown the applicability of site selectivity and spin polarization. Different interatomic distances of the same element in different chemical forms have been detected using site-selective EXAFS.« less

Frontiers of X-Ray Astronomy

NASA Astrophysics Data System (ADS)

Fabian, Andrew C.; Pounds, Kenneth A.; Blandford, Roger D.

2004-07-01

Preface; 1. Forty years on from Aerobee 150: a personal perspective K. Pounds; 2. X-ray spectroscopy of astrophysical plasmas S. M. Kahn, E. Behar, A. Kinkhabwala and D. W. Savin; 3. X-rays from stars M. Gudel; 4. X-ray observations of accreting white-dwarf systems M. Cropper, G. Ramsay, C. Hellier, K. Mukai, C. Mauche and D. Pandel; 5. Accretion flows in X-ray binaries C. Done; 6. Recent X-ray observations of supernova remnants C. R. Canizares; 7. Luminous X-ray sources in spiral and star-forming galaxies M. Ward; 8. Cosmological constraints from Chandra observations of galaxy clusters S. W. Allen; 9. Clusters of galaxies: a cosmological probe R. Mushotzky; 10. Obscured active galactic nuclei: the hidden side of the X-ray Universe G. Matt; 11. The Chandra Deep Field-North Survey and the cosmic X-ray background W. N. Brandt, D. M. Alexander, F. E. Bauer and A. E. Hornschemeier; 12. Hunting the first black holes G. Hasinger; 13. X-ray astronomy in the new millennium: a summary R. D. Blandford.

The Cambridge-Cambridge X-ray Serendipity Survey: I X-ray luminous galaxies

NASA Technical Reports Server (NTRS)

Boyle, B. J.; Mcmahon, R. G.; Wilkes, B. J.; Elvis, M.

1994-01-01

We report on the first results obtained from a new optical identification program of 123 faint X-ray sources with S(0.5-2 keV) greater than 2 x 10(exp -14) erg/s/sq cm serendipitously detected in ROSAT PSPC pointed observations. We have spectroscopically identified the optical counterparts to more than 100 sources in this survey. Although the majority of the sample (68 objects) are QSO's, we have also identified 12 narrow emission line galaxies which have extreme X-ray luminosities (10(exp 42) less than L(sub X) less than 10(exp 43.5) erg/s). Subsequent spectroscopy reveals them to be a mixture of star-burst galaxies and Seyfert 2 galaxies in approximately equal numbers. Combined with potentially similar objects identified in the Einstein Extended Medium Sensitivity Survey, these X-ray luminous galaxies exhibit a rate of cosmological evolution, L(sub X) varies as (1 + z)(exp 2.5 +/- 1.0), consistent with that derived for X-ray QSO's. This evolution, coupled with the steep slope determined for the faint end of the X-ray luminosity function (Phi(L(sub X)) varies as L(sub X)(exp -1.9)), implies that such objects could comprise 15-35% of the soft (1-2 keV) X-ray background.

Lu.sub.1-xI.sub.3:Ce.sub.x-a scintillator for gamma-ray spectroscopy and time-of-flight pet

DOEpatents

Shah, Kanai S [Newton, MA

2008-02-12

The present invention includes very fast scintillator materials including lutetium iodide doped with Cerium (Lu.sub.1-xI.sub.3:Ce.sub.x; LuI.sub.3:Ce). The LuI.sub.3 scintillator material has surprisingly good characteristics including high light output, high gamma-ray stopping efficiency, fast response, low cost, good proportionality, and minimal afterglow that the material is useful for gamma-ray spectroscopy, medical imaging, nuclear and high energy physics research, diffraction, non-destructive testing, nuclear treaty verification and safeguards, and geological exploration.

Sequential single shot X-ray photon correlation spectroscopy at the SACLA free electron laser

DOE PAGES

Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech; ...

2015-11-27

In this study, hard X-ray free electron lasers allow for the first time to access dynamics of condensed matter samples ranging from femtoseconds to several hundred seconds. In particular, the exceptional large transverse coherence of the X-ray pulses and the high time-averaged flux promises to reach time and length scales that have not been accessible up to now with storage ring based sources. However, due to the fluctuations originating from the stochastic nature of the self-amplified spontaneous emission (SASE) process the application of well established techniques such as X-ray photon correlation spectroscopy (XPCS) is challenging. Here we demonstrate a single-shotmore » based sequential XPCS study on a colloidal suspension with a relaxation time comparable to the SACLA free-electron laser pulse repetition rate. High quality correlation functions could be extracted without any indications for sample damage. This opens the way for systematic sequential XPCS experiments at FEL sources.« less

Sequential single shot X-ray photon correlation spectroscopy at the SACLA free electron laser

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lehmkühler, Felix; Kwaśniewski, Paweł; Roseker, Wojciech

In this study, hard X-ray free electron lasers allow for the first time to access dynamics of condensed matter samples ranging from femtoseconds to several hundred seconds. In particular, the exceptional large transverse coherence of the X-ray pulses and the high time-averaged flux promises to reach time and length scales that have not been accessible up to now with storage ring based sources. However, due to the fluctuations originating from the stochastic nature of the self-amplified spontaneous emission (SASE) process the application of well established techniques such as X-ray photon correlation spectroscopy (XPCS) is challenging. Here we demonstrate a single-shotmore » based sequential XPCS study on a colloidal suspension with a relaxation time comparable to the SACLA free-electron laser pulse repetition rate. High quality correlation functions could be extracted without any indications for sample damage. This opens the way for systematic sequential XPCS experiments at FEL sources.« less

Ultrafast Absorption Spectroscopy of Aluminum Plasmas Created by LCLS using Betatron X-Ray Radiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Albert, Felicie

2016-10-12

This document summarizes the goals and accomplishments of a six month-long LDRD project, awarded through the LLNL director Early and Mid Career Recognition (EMCR) program. This project allowed us to support beamtime awarded at the Matter under Extreme Conditions (MEC) end station of the Linac Coherent Light Source (LCLS). The goal of the experiment was to heat metallic samples with the bright x-rays from the LCLS free electron laser. Then, we studied how they relaxed back to equilibrium by probing them with ultrafast x-ray absorption spectroscopy using laser-based betatron radiation. Our work enabled large collaborations between LLNL, SLAC, LBNL, andmore » institutions in France and in the UK, while providing training to undergraduate and graduate students during the experiment. Following this LDRD project, the PI was awarded a 5-year DOE early career research grant to further develop applications of laser-driven x-ray sources for high energy density science experiments and warm dense matter states.« less

X-ray Raman spectroscopy of lithium-ion battery electrolyte solutions in a flow cell.

PubMed

Ketenoglu, Didem; Spiekermann, Georg; Harder, Manuel; Oz, Erdinc; Koz, Cevriye; Yagci, Mehmet C; Yilmaz, Eda; Yin, Zhong; Sahle, Christoph J; Detlefs, Blanka; Yavaş, Hasan

2018-03-01

The effects of varying LiPF 6 salt concentration and the presence of lithium bis(oxalate)borate additive on the electronic structure of commonly used lithium-ion battery electrolyte solvents (ethylene carbonate-dimethyl carbonate and propylene carbonate) have been investigated. X-ray Raman scattering spectroscopy (a non-resonant inelastic X-ray scattering method) was utilized together with a closed-circle flow cell. Carbon and oxygen K-edges provide characteristic information on the electronic structure of the electrolyte solutions, which are sensitive to local chemistry. Higher Li + ion concentration in the solvent manifests itself as a blue-shift of both the π* feature in the carbon edge and the carbonyl π* feature in the oxygen edge. While these oxygen K-edge results agree with previous soft X-ray absorption studies on LiBF 4 salt concentration in propylene carbonate, carbon K-edge spectra reveal a shift in energy, which can be explained with differing ionic conductivities of the electrolyte solutions.

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

NASA Astrophysics Data System (ADS)

Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

2014-04-01

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called ``molecular movie'' within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.

The characterization of Cr secondary oxide phases in ZnO films studied by X-ray spectroscopy and photoemission spectroscopy

NASA Astrophysics Data System (ADS)

Chiou, J. W.; Chang, S. Y.; Huang, W. H.; Chen, Y. T.; Hsu, C. W.; Hu, Y. M.; Chen, J. M.; Chen, C.-H.; Kumar, K.; Guo, J.-H.

2011-03-01

X-ray absorption near-edge structure (XANES), X-ray emission spectroscopy (XES), and X-ray photoemission spectroscopy (XPS) were used to characterize the Cr secondary oxide phases in ZnO films that had been prepared using a co-sputtering method. Analysis of the Cr L3,2-edge XANES spectra reveals that the intensity of white-line features decreases subtly as the sputtering power increases, indicating that the occupation of Cr 3 d orbitals increases with Cr concentration in (Zn, Cr)O films. The O K-edge spectra show that the intensity of XANES features of (Zn, Cr)O films is lower than those of ZnO film, suggesting enhanced occupation of O 2 p-derived states through O 2 p-Cr 3 d hybridization. The XES and XPS spectra indicate that the line shapes in the valence band of (Zn, Cr)O films are quite different from those of ZnO and that the Cr 2O 3 phase dominates the spinel structure of (Zn, Cr)O films increasingly as the Cr sputtering power is increased. Over all results suggest that the non-ferromagnetic behavior of (Zn, Cr)O films can be attributed to the dominant presence of Cr 2O 3, whereas the bulk comprise phase segregations of Cr 2O 3 and/or ZnCr 2O 4, which results them the most stable TM-doped ZnO material against etching.

Characterization of the LCLS “nanosecond two-bunch” mode for x-ray speckle visibility spectroscopy experiments

DOE PAGES

Sun, Yanwen; Zhu, Diling; Song, Sanghoon; ...

2017-05-23

The generation of two X-ray pulses with tunable nanosecond scale time separations has recently been demonstrated at the Linac Coherent Light Source using an accelerator based technique. This approach offers the opportunity to extend X-ray Photon Correlation Spectroscopy techniques to the yet unexplored regime of nanosecond timescales by means of X-ray Speckle Visibility Spectroscopy. As the two pulses originate from two independent Spontaneous Amplified Stimulated Emission processes, the beam properties fluctuate from pulse pair to pulse pair, but as well between the individual pulses within a pair. However, two-pulse XSVS experiments require the intensity of the individual pulses to bemore » either identical in the ideal case, or with a accurately known intensity ratio. We present the design and performances of a non-destructive intensity diagnostic based on measurement of scattering from a transparent target using a high-speed photo-detector. Individual pulses within a pulse pair with time delays as short as 0.7 ns can be resolved. Moreover, using small angle coherent scattering, we characterize the averaged spatial overlap of the focused pulse pairs. Furthermore, the multi-shot average-speckle contrasts from individual pulses and pulse pairs are compared.« less

X-ray photoelectron spectroscopy and atomic force microscopy characterization of the effects of etching Zn xCd 1- xTe surfaces

NASA Astrophysics Data System (ADS)

George, M. A.; Azoulay, M.; Jayatirtha, H. N.; Burger, A.; Collins, W. E.; Silberman, E.

1993-10-01

X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) was used for the first time to characterize the chemical composition of modified surfaces of Zn xCd 1- xTe single crystals. These surface treatments were selected for their relevance to device preparation procedures. The XPS peaks indicated an increase of the tellurium and a depletion of the cadmium concentrations upon etching in bromine methanol solution. AFM revealed the formation of pronounced Te inclusions. Higher x values correlated with a decrease in residual bromine left on the surface, while cut and polished samples had higher oxide concentrations and increased bromination of the surface than cleaved samples.

Broadband high resolution X-ray spectral analyzer

DOEpatents

Silver, Eric H.; Legros, Mark; Madden, Norm W.; Goulding, Fred; Landis, Don

1998-01-01

A broad bandwidth high resolution x-ray fluorescence spectrometer has a performance that is superior in many ways to those currently available. It consists of an array of 4 large area microcalorimeters with 95% quantum efficiency at 6 keV and it produces x-ray spectra between 0.2 keV and 7 keV with an energy resolution of 7 to 10 eV. The resolution is obtained at input count rates per array element of 10 to 50 Hz in real-time, with analog pulse processing and thermal pile-up rejection. This performance cannot be matched by currently available x-ray spectrometers. The detectors are incorporated into a compact and portable cryogenic refrigerator system that is ready for use in many analytical spectroscopy applications as a tool for x-ray microanalysis or in research applications such as laboratory and astrophysical x-ray and particle spectroscopy.

Broadband high resolution X-ray spectral analyzer

DOEpatents

Silver, E.H.; Legros, M.; Madden, N.W.; Goulding, F.; Landis, D.

1998-07-07

A broad bandwidth high resolution X-ray fluorescence spectrometer has a performance that is superior in many ways to those currently available. It consists of an array of 4 large area microcalorimeters with 95% quantum efficiency at 6 keV and it produces X-ray spectra between 0.2 keV and 7 keV with an energy resolution of 7 to 10 eV. The resolution is obtained at input count rates per array element of 10 to 50 Hz in real-time, with analog pulse processing and thermal pile-up rejection. This performance cannot be matched by currently available X-ray spectrometers. The detectors are incorporated into a compact and portable cryogenic refrigerator system that is ready for use in many analytical spectroscopy applications as a tool for X-ray microanalysis or in research applications such as laboratory and astrophysical X-ray and particle spectroscopy. 6 figs.

X-ray magnetic circular dichroism measured at the Fe K-edge with a reduced intrinsic broadening: x-ray absorption spectroscopy versus resonant inelastic x-ray scattering measurements

NASA Astrophysics Data System (ADS)

Juhin, Amélie; Sainctavit, Philippe; Ollefs, Katharina; Sikora, Marcin; Filipponi, Adriano; Glatzel, Pieter; Wilhelm, Fabrice; Rogalev, Andrei

2016-12-01

X-ray magnetic circular dichroism is measured at the Fe K pre-edge in yttrium iron garnet using two different procedures that allow reducing the intrinsic broadening due to the 1s corehole lifetime. First, deconvolution of XMCD data measured in total fluorescence yield (TFY) with an extremely high signal-to-noise ratio enables a factor of 2.4 to be gained in the XMCD intensity. Ligand field multiplet calculations performed with different values of intrinsic broadening show that deconvolving such high quality XMCD data is similar to reducing the lifetime broadening from a 1s corehole to a 2p corehole. Second, MCD is measured by resonant inelastic x-ray scattering spectroscopy as a function of incident energy and emission energy. Selection of a fixed emission energy, instead of using the TFY, allows enhancing the MCD intensity up to a factor of  ˜4.7. However, this significantly changes the spectral shape of the XMCD signal, which cannot be interpreted any more as an absorption spectrum.

Saccharose solid matrix embedded proteins: a new method for sample preparation for X-ray absorption spectroscopy.

PubMed

Ascone, I; Sabatucci, A; Bubacco, L; Di Muro, P; Salvato, B

2000-01-01

In this study, solid samples of hemoglobin and hemocyanin have been prepared by embedding the proteins into a saccharose-based matrix. These materials have been developed specifically for specimens for X-ray absorption spectroscopy (XAS). The preservation of protein conformation and active site organization was tested, making comparisons between the solid and the corresponding liquid samples, using resonance Raman, infra red, fluorescence and XAS. The XAS spectra of irradiated solid and liquid samples were then compared, and the preservation of biological activity of the proteins during both preparation procedure and X-ray irradiation was assessed. In all cases, the measurements clearly demonstrate that protein solid samples are both structurally and functionally quite well preserved, much better than those in the liquid state. The saccharose matrix provides an excellent protection against X-ray damages, allowing for longer exposure to the X-ray beam. Moreover, the demonstrated long-term stability of samples permits their preparation and storage in optimal conditions, allowing for the repetition of data collection with the same sample in several experimental sessions. The very high protein concentration that can be reached results in a significantly better signal-to-noise ratio, particularly useful for high molecular weight proteins with a low metal-to-protein ratio. On the bases of the above-mentioned results, we propose the new method as a standard procedure for the preparation of biological samples to be used for XAS spectroscopy.

Adaptive design of an X-ray magnetic circular dichroism spectroscopy experiment with Gaussian process modelling

NASA Astrophysics Data System (ADS)

Ueno, Tetsuro; Hino, Hideitsu; Hashimoto, Ai; Takeichi, Yasuo; Sawada, Masahiro; Ono, Kanta

2018-01-01

Spectroscopy is a widely used experimental technique, and enhancing its efficiency can have a strong impact on materials research. We propose an adaptive design for spectroscopy experiments that uses a machine learning technique to improve efficiency. We examined X-ray magnetic circular dichroism (XMCD) spectroscopy for the applicability of a machine learning technique to spectroscopy. An XMCD spectrum was predicted by Gaussian process modelling with learning of an experimental spectrum using a limited number of observed data points. Adaptive sampling of data points with maximum variance of the predicted spectrum successfully reduced the total data points for the evaluation of magnetic moments while providing the required accuracy. The present method reduces the time and cost for XMCD spectroscopy and has potential applicability to various spectroscopies.

In-vivo analysis of the uptake process of heavy metals through maize roots by using synchrotron X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Hwang, Bae Geun; Lee, Sang Joon; Gil, Kyehwan

2016-12-01

The uptake of heavy metals by plants has been receiving much attention for crop contamination and phytoremediation. We employed synchrotron X-ray fluorescence (XRF) spectroscopy for an in-vivo analysis of heavy-metal uptake through a strand of maize root. A focused X-ray beam of 2.5 × 2.5 μm2 in physical dimensions was scanned along horizontal lines of the maize root at intervals of 3 μm at the 4B X-ray micro-diffraction beamline of the Pohang Accelerator Laboratory (PAL). Time-resolved mapping of the fluorescence intensities from multiple metallic elements in the root tissues provided information about the radial distributions of heavy-metal elements and their temporal variations. The concentrated core stream of heavy-metal elements spread radially up to roughly 500 μm, corresponding to 40 % of the root diameter. The absorption characteristics of three heavy metals, Cr, Mn and Ni, and their physiological features were analyzed. The absolute concentrations and the contents of the heavy-metal elements in the tested maize roots were quantitatively evaluated by using the calibration curve obtained from reference samples with preset concentrations. The uptake quantities of the tested heavy-metal elements are noticeably different, although their molecular weights are similar. This study should be helpful for understanding plant physiology related with heavy-metal uptake.

Summary: Update to ASTM Guide E 1523 to Charge Control and Charge Referencing Techniques in X-ray Photoelectron Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baer, Donald R.

2005-04-22

An updated version of the ASTM guide E1523 to the methods to charge control and charge referencing techniques in x-ray photoelectron spectroscopy has been released by ASTM. The guide is meant to acquaint x-ray photoelectron spectroscopy (XPS) users with the various charge control and charge referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens. The current guide has been expanded to include new references as well as recommendations for reporting information on charge control and charge referencing. The previous version of the document had been published in 1997.

Sulfur Speciation in Biochars by Very High Resolution Benchtop Ka X-Ray Emission Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cheah, Singfoong; Holden, William M.; Seidler, Gerald T.

The analytical chemistry of sulfur-containing materials poses substantial technical challenges, especially due to the limitations of 33S NMR and the time-intensive preparations required for wet-chemistry analyses. A number of prior studies have found that synchrotron-based X-ray absorption near edge structure (XANES) measurements can give detailed speciation of sulfur chemistry in such cases. However, due to the obvious access limitations, synchrotron XANES of sulfur cannot be part of routine analytical practice across the chemical sciences community. Here, in a study of the sulfur chemistry in biochars, we compare and contrast the chemical inferences available from synchrotron XANES with that given bymore » benchtop, extremely high resolution wavelength-dispersive X-ray fluorescence (WD-XRF) spectroscopy, also often called X-ray emission spectroscopy (XES). While the XANES spectra have higher total information content, often giving differentiation between different moieties having the same oxidation state, the lower sensitivity of the S Ka XES to coordination and local structure provides pragmatic benefit for the more limited goal of quantifying the S oxidation state distribution. Within that constrained metric, we find good agreement between the two methods. As the sulfur concentrations were as low as 150 ppm, these measurements provide proof-of-principle for characterization of the sulfur chemistry of biochars and potential applications to other areas such as soils, batteries, catalysts, and fossil fuels and their combustion products.« less

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

PubMed Central

Gaudin, J.; Fourment, C.; Cho, B. I.; Engelhorn, K.; Galtier, E.; Harmand, M.; Leguay, P. M.; Lee, H. J.; Nagler, B.; Nakatsutsumi, M.; Ozkan, C.; Störmer, M.; Toleikis, S.; Tschentscher, Th; Heimann, P. A.; Dorchies, F.

2014-01-01

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level of the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes. PMID:24740172

Towards simultaneous measurements of electronic and structural properties in ultra-fast x-ray free electron laser absorption spectroscopy experiments

DOE PAGES

Gaudin, J.; Fourment, C.; Cho, B. I.; ...

2014-04-17

The rapidly growing ultrafast science with X-ray lasers unveils atomic scale processes with unprecedented time resolution bringing the so called “molecular movie” within reach. X-ray absorption spectroscopy is one of the most powerful x-ray techniques providing both local atomic order and electronic structure when coupled with ad-hoc theory. Collecting absorption spectra within few x-ray pulses is possible only in a dispersive setup. We demonstrate ultrafast time-resolved measurements of the LIII-edge x-ray absorption near-edge spectra of irreversibly laser excited Molybdenum using an average of only few x-ray pulses with a signal to noise ratio limited only by the saturation level ofmore » the detector. The simplicity of the experimental set-up makes this technique versatile and applicable for a wide range of pump-probe experiments, particularly in the case of non-reversible processes.« less

Effect of Pressure on Valence and Structural Properties of YbFe 2 Ge 2 Heavy Fermion Compound—A Combined Inelastic X-ray Spectroscopy, X-ray Diffraction, and Theoretical Investigation

DOE PAGES

Kumar, Ravhi S.; Svane, Axel; Vaitheeswaran, Ganapathy; ...

2015-10-19

We measured the crystal structure and the Yb valence of the YbFe 2Ge 2 heavy fermion compound at room temperature and under high pressures using high-pressure powder X-ray diffraction and X-ray absorption spectroscopy via both partial fluorescence yield and resonant inelastic X-ray emission techniques. Moreover, the measurements are complemented by first-principles density functional theoretical calculations using the self-interaction corrected local spin density approximation investigating in particular the magnetic structure and the Yb valence. Finally, while the ThCr 2Si 2-type tetragonal (I4/mmm) structure is stable up to 53 GPa, the X-ray emission results show an increase of the Yb valence frommore » v = 2.72(2) at ambient pressure to v = 2.93(3) at ~9 GPa, where at low temperature a pressure-induced quantum critical state was reported.« less

Long Duration X-ray Bursts Observed by MAXI

NASA Astrophysics Data System (ADS)

Serino, Motoko; Iwakiri, Wataru; Tamagawa, Toru; Sakamoto, Takanori; Nakahira, Satoshi; Matsuoka, Masaru; Yamaoka, Kazutaka; Negoro, Hitoshi

Monitor of All-sky X-ray Image (MAXI) is X-ray mission on the International Space Station. MAXI scans all sky every 92 min and detects various X-ray transient events including X-ray bursts. Among the X-ray bursts observed by MAXI, eleven had long duration and were observed more than one scan. Six out of eleven long bursts have the e-folding time of >1 h, that should be classified as "superbursts", while the rest are "intermediate-duration bursts". The total emitted energy of these long X-ray bursts range from 1041 to 1042 ergs. The lower limits of the superburst recurrence time of 4U 0614+091 and Ser X-1 are calculated as 4400 and 59 days, which may be consistent with the observed recurrence time of 3523 and 1148 days, respectively.

Composition of RF-sputtered refractory compounds determined by X-ray photoelectron spectroscopy

NASA Technical Reports Server (NTRS)

Wheeler, D. R.; Brainard, W. A.

1978-01-01

RF-sputtered coatings of CrB2, MoSi2, Mo2C, TiC, and MoS2 were examined by X-ray photoelectron spectroscopy (XPS). Data on stoichiometry, impurity content, and chemical bonding were obtained. The influences of sputtering target history, deposition time, RF power level, and substrate bias were studied. Significant deviations from stoichiometry and high oxide levels were related to target outgassing. The effect of substrate bias depended on the particular coating material studied.

Electrosynthesis of ZnO nanorods and nanotowers: Morphology and X-ray Absorption Near Edge Spectroscopy studies

NASA Astrophysics Data System (ADS)

Sigircik, Gokmen; Erken, Ozge; Tuken, Tunc; Gumus, Cebrail; Ozkendir, Osman M.; Ufuktepe, Yuksel

2015-06-01

Deposition mechanism of nano-structured ZnO films has been investigated in the absence and presence of chloride ions from aqueous solution. The resulting opto-electronic properties were interpreted extensively, using X-ray diffraction (XRD), X-ray Absorption Near Edge Spectroscopy (XANES), field emission scanning electron microscopy (FE-SEM), UV-Visible spectroscopy and four probe techniques. The ZnO deposition is mass transport controlled process and the interaction of chloride ions with the surface has great influence on diffusion kinetics, considering the substantial species (Zn2+ and OH-) involved in the construction of ZnO film. This effect does not change major lattice parameters, as shown with detailed analysis of XRD data. However, the texture coefficient (Tc) (0 0 2) value is higher in presence of chloride ions containing synthesis solution which gave vertically aligned, well defined and uniformly dispersed nanorods structure. The calculated Eg values are in the range 3.28-3.41 eV and 3.22-3.31 eV for ZnO nanorods and nanotowers synthesized at different deposition periods, respectively. Furthermore, the charge mobility values regarding the deposition periods were measured to be in the ranges from 130.4 to 449.2 cm2 V-1 s-1 and 126.2 to 204.7 cm2 V-1 s-1 for nanorods and nanotowers, respectively. From XANES results, it was shown that the Zn K-edge spectrum is dominated by the transition of Zn 1s core electrons into the unoccupied Zn 4p states of the conduction band. Comparing the rod and tower nano-structured ZnO thin films, the excitation behavior of valence band electrons is different. Moreover, the density states of Zn 4p are higher for ZnO nanorods.

Quantitative study of mammalian cells by scanning transmission soft X-ray microscopy

NASA Astrophysics Data System (ADS)

Shinohara, K.; Ohigashi, T.; Toné, S.; Kado, M.; Ito, A.

2017-06-01

Molecular distribution in mammalian cells was studied by soft X-ray scanning transmission microscopy with respect to the quantitative aspect of analysis. NEXAFS profiles at the C, N and O K-absorption edges were combined and used for the analysis. For the estimation of quantity for nucleic acids and proteins, NEXAFS profiles of DNA and bovine serum albumin (BSA) at the N K-absorption edge were applied assuming that those were their representatives. The method has a potential to explore the other molecular components than nucleic acids and proteins.

High-pressure studies with x-rays using diamond anvil cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shen, Guoyin; Mao, Ho Kwang

2016-11-22

Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials' properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. Thesemore » HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and

High-pressure studies with x-rays using diamond anvil cells

NASA Astrophysics Data System (ADS)

Shen, Guoyin; Mao, Ho Kwang

2017-01-01

Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials’ properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. These HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and

AEGIS: An Astrophysics Experiment for Grating and Imaging Spectroscopy---a Soft X-ray, High-resolution Spectrometer

NASA Astrophysics Data System (ADS)

Huenemoerder, David; Bautz, M. W.; Davis, J. E.; Heilmann, R. K.; Houck, J. C.; Marshall, H. L.; Neilsen, J.; Nicastro, F.; Nowak, M. A.; Schattenburg, M. L.; Schulz, N. S.; Smith, R. K.; Wolk, S.; AEGIS Team

2012-01-01

AEGIS is a concept for a high-resolution soft X-ray spectroscopic observatory developed in response to NASA's request for definitions of the next X-ray astronomy mission. At a small fraction of the cost of the once-planned International X-ray Observatory (IXO), AEGIS has capabilities that surpass IXO grating spectrometer requirements, and which are far superior to those of existing soft X-ray spectrometers. AEGIS incorporates innovative technology in X-ray optics, diffraction gratings and detectors. The mirror uses high area-to-mass ratio segmented glass architecture developed for IXO, but with smaller aperture and larger graze angles optimized for high-throughput grating spectroscopy with low mass and cost. The unique Critical Angle Transmission gratings combine low mass and relaxed figure and alignment tolerances of Chandra transmission gratings but with high diffraction efficiency and resolving power of blazed reflection gratings. With more than an order of magnitude better performance over Chandra and XMM grating spectrometers, AEGIS can obtain high quality spectra of bright AGN in a few hours rather than 10 days. Such high resolving power allows detailed kinematic studies of galactic outflows, hot gas in galactic haloes, and stellar accretion flows. Absorption line spectroscopy will be used to study large scale structure, cosmic feedback, and growth of black holes in thousands of sources to great distances. AEGIS will enable powerful multi-wavelength investigations, for example with Hubble/COS in the UV to characterize the intergalactic medium. AEGIS will be the first observatory with sufficient resolution below 1 keV to resolve thermally-broadened lines in hot ( 10 MK) plasmas. Here we describe key science investigations enable by Aegis, its scientific payload and mission plan. Acknowledgements: Support was provided in part by: NASA SAO contract SV3-73016 to MIT for the Chandra X-ray Center and Science Instruments; NASA grant NNX08AI62G; and the MKI

Interlaced X-ray diffraction computed tomography

PubMed Central

Vamvakeros, Antonios; Jacques, Simon D. M.; Di Michiel, Marco; Senecal, Pierre; Middelkoop, Vesna; Cernik, Robert J.; Beale, Andrew M.

2016-01-01

An X-ray diffraction computed tomography data-collection strategy that allows, post experiment, a choice between temporal and spatial resolution is reported. This strategy enables time-resolved studies on comparatively short timescales, or alternatively allows for improved spatial resolution if the system under study, or components within it, appear to be unchanging. The application of the method for studying an Mn–Na–W/SiO2 fixed-bed reactor in situ is demonstrated. Additionally, the opportunities to improve the data-collection strategy further, enabling post-collection tuning between statistical, temporal and spatial resolutions, are discussed. In principle, the interlaced scanning approach can also be applied to other pencil-beam tomographic techniques, like X-ray fluorescence computed tomography, X-ray absorption fine structure computed tomography, pair distribution function computed tomography and tomographic scanning transmission X-ray microscopy. PMID:27047305

Can X-ray spectrum imaging replace backscattered electrons for compositional contrast in the scanning electron microscope?

PubMed

Newbury, Dale E; Ritchie, Nicholas W M

2011-01-01

The high throughput of the silicon drift detector energy dispersive X-ray spectrometer (SDD-EDS) enables X-ray spectrum imaging (XSI) in the scanning electron microscope to be performed in frame times of 10-100 s, the typical time needed to record a high-quality backscattered electron (BSE) image. These short-duration XSIs can reveal all elements, except H, He, and Li, present as major constituents, defined as 0.1 mass fraction (10 wt%) or higher, as well as minor constituents in the range 0.01-0.1 mass fraction, depending on the particular composition and possible interferences. Although BSEs have a greater abundance by a factor of 100 compared with characteristic X-rays, the strong compositional contrast in element-specific X-ray maps enables XSI mapping to compete with BSE imaging to reveal compositional features. Differences in the fraction of the interaction volume sampled by the BSE and X-ray signals lead to more delocalization of the X-ray signal at abrupt compositional boundaries, resulting in poorer spatial resolution. Improved resolution in X-ray elemental maps occurs for the case of a small feature composed of intermediate to high atomic number elements embedded in a matrix of lower atomic number elements. XSI imaging strongly complements BSE imaging, and the SDD-EDS technology enables an efficient combined BSE-XSI measurement strategy that maximizes the compositional information. If 10 s or more are available for the measurement of an area of interest, the analyst should always record the combined BSE-XSI information to gain the advantages of both measures of compositional contrast. Copyright © 2011 Wiley Periodicals, Inc.

Report on the 18th International Conference on X-ray and Inner-Shell Processes (X99).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gemmell, D. S.; Physics

2000-01-01

The 18th conference of the series served as a forum for discussing fundamental issues in the field of x-ray and inner-shell processes and their application in various disciplines of science and technology. Special emphasis was given to the opportunities offered by modern synchrotron x-ray sources. The program included plenary talks, progress reports and poster presentations relating to new developments in the field of x-ray and inner-shell processes. The range of topics included: X-ray interactions with atoms, molecules, clusters, surfaces and solids; Decay processes for inner-shell vacancies; X-ray absorption and emission spectroscopy - Photoionization processes; Phenomena associated with highly charged ionsmore » and collisions with energetic particles; Electron-spin and -momentum spectroscopy; X-ray scattering and spectroscopy in the study of magnetic systems; Applications in materials science, biology, geosciences, and other disciplines; Elastic and inelastic x-ray scattering processes in atoms and molecules; Threshold phenomena (post-collision interaction, resonant Raman processes, etc.); Nuclear absorption and scattering of x-rays; 'Fourth-generation' x-ray sources; Processes exploiting the polarization and coherence properties of x-ray beams; Developments in experimental techniques (x-ray optics, temporal techniques, detectors); Microscopy, spectromicroscopy, and various imaging techniques; Non-linear processes and x-ray lasers; Ionization and excitation induced by charged particles and by x-rays; and Exotic atoms (including 'hollow' atoms and atoms that contain 'exotic' particles).« less

The superconducting high-resolution soft X-ray spectrometer at the advanced biological and environmental X-ray facility

NASA Astrophysics Data System (ADS)

Friedrich, S.; Drury, O. B.; George, S. J.; Cramer, S. P.

2007-11-01

We have built a 36-pixel superconducting tunnel junction X-ray spectrometer for chemical analysis of dilute samples in the soft X-ray band. It offers an energy resolution of ˜10-20 eV FWHM below 1 keV, a solid angle coverage of ˜10 -3, and can be operated at total rates of up to ˜10 6 counts/s. Here, we describe the spectrometer performance in speciation measurements by fluorescence-detected X-ray absorption spectroscopy at the Advanced Biological and Environmental X-ray facility at the ALS synchrotron.

The spatial coherence function in scanning transmission electron microscopy and spectroscopy.

PubMed

Nguyen, D T; Findlay, S D; Etheridge, J

2014-11-01

We investigate the implications of the form of the spatial coherence function, also referred to as the effective source distribution, for quantitative analysis in scanning transmission electron microscopy, and in particular for interpreting the spatial origin of imaging and spectroscopy signals. These questions are explored using three different source distribution models applied to a GaAs crystal case study. The shape of the effective source distribution was found to have a strong influence not only on the scanning transmission electron microscopy (STEM) image contrast, but also on the distribution of the scattered electron wavefield and hence on the spatial origin of the detected electron intensities. The implications this has for measuring structure, composition and bonding at atomic resolution via annular dark field, X-ray and electron energy loss STEM imaging are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

X-Ray Weak Broad-Line Quasars: Absorption or Intrinsic X-Ray Weakness

NASA Technical Reports Server (NTRS)

Risaliti, Guido; Mushotzky, Richard F. (Technical Monitor)

2004-01-01

XMM observations of X-ray weak quasars have been performed during 2003. The data for all but the last observation are now available (there has been a delay of several months on the initial schedule, due to high background flares which contaminated the observations: as a consequence, most of them had to be rescheduled). We have reduced and analyzed these data, and obtained interesting preliminary scientific results. Out of the eight sources, 4 are confirmed to be extrimely X-ray weak, in agreement with the results of previous Chandra observations. 3 sources are confirmed to be highly variable both in flux (by factors 20-50) and in spectral properties (dramatic changes in spectral index). For both these groups of objects, an article is in preparation. Preliminary results have been presented at an international workshop on AGN surveys in December 2003, in Cozumel (Mexico). In order to further understand the nature of these X-ray weak quasars, we submitted proposals for spectroscopy at optical and infrared telescopes. We obtained time at the TNG 4 meter telescope for near-IR observations, and at the Hobby-Eberly Telescope for optical high-resolution spectroscopy. These observations will be performed in early 2004, and will complement the XMM data, in order to understand whether the X-ray weakness of these sources is an intrinsic property or is due to absorption by circumnuclear material.

X-Ray Testing Constellation-X Optics at MSFC's 100-m Facility

NASA Technical Reports Server (NTRS)

O'Dell, Stephen; Baker, Markus; Content, David; Freeman, Mark; Glenn, Paul; Gubarev, Mikhail; Hair, Jason; Jones, William; Joy, Marshall

2003-01-01

In addition to the 530-m-long X-Ray Calibration Facility (XRCF), NASA's Marshall Space Flight Center (MSFC) operates a 104-m-long (source-to-detector) X-ray-test facility. Originally developed and still occasionally used for stray-light testing of visible-fight optical systems, the so-called "Stray-Light Facility" now serves primarily as a convenient and inexpensive facility for performance evaluation and calibration of X-ray optics and detectors. The facility can accommodate X-ray optics up to about 1-m diameter and 12-m focal length. Currently available electron-impact sources at the facility span the approximate energy range 0.2 to 100 keV, thus supporting testing of soft- and hard-X-ray optics and detectors. Available MSFC detectors are a front-illuminated CCD (charge-coupled device) and a scanning CZT (cadmium--zinc--telluride) detector, with low-energy cut-offs of about 0.8 and 3 keV, respectively. In order to test developmental optics for the Constellation-X Project, led by NASA's Goddard Space Flight Center (GSFC), MSFC undertook several enhancements to the facility. Foremost among these was development and fabrication of a five-degree-of-freedom (5-DoF) optics mount and control system, which translates and tilts the user-provided mirror assembly suspended from its interface plate. Initial Constellation-X tests characterize the performance of the Optical Alignment Pathfinder Two (OAP2) for the large Spectroscopy X-ray Telescope (SXT) and of demonstration mirror assemblies for the Hard X-ray Telescope (HXT). With the Centroid Detector Assembly (CDA), used for precision alignment of the Chandra (nee AXAF) mirrors, the Constellation-X SXT Team optically aligned the individual mirrors of the OAPZ at GSFC. The team then developed set-up and alignment procedures, including transfer of the alignment from the optical alignment facility at GSFC to the X-ray test facility at MSFC, using a reference flat and fiducials. The OAPZ incorporates additional ancillary

High average power, highly brilliant laser-produced plasma source for soft X-ray spectroscopy.

PubMed

Mantouvalou, Ioanna; Witte, Katharina; Grötzsch, Daniel; Neitzel, Michael; Günther, Sabrina; Baumann, Jonas; Jung, Robert; Stiel, Holger; Kanngiesser, Birgit; Sandner, Wolfgang

2015-03-01

In this work, a novel laser-produced plasma source is presented which delivers pulsed broadband soft X-radiation in the range between 100 and 1200 eV. The source was designed in view of long operating hours, high stability, and cost effectiveness. It relies on a rotating and translating metal target and achieves high stability through an on-line monitoring device using a four quadrant extreme ultraviolet diode in a pinhole camera arrangement. The source can be operated with three different laser pulse durations and various target materials and is equipped with two beamlines for simultaneous experiments. Characterization measurements are presented with special emphasis on the source position and emission stability of the source. As a first application, a near edge X-ray absorption fine structure measurement on a thin polyimide foil shows the potential of the source for soft X-ray spectroscopy.

X-ray irradiation-induced structural changes on Single Wall Carbon Nanotubes

NASA Astrophysics Data System (ADS)

Bardi, N.; Jurewicz, I.; King, A. K.; Alkhorayef, M. A.; Bradley, D.; Dalton, A. B.

2017-11-01

Dosimetry devices based on Carbon Nanotubes are a promising new technology. In particular using devices based on single wall Carbon Nanotubes may offer a tissue equivalent response with the possibility for device miniaturisation, high scale manufacturing and low cost. An important precursor to device fabrication requires a quantitative study of the effects of X-ray radiation on the physical and chemical properties of the individual nanotubes. In this study, we concentrate on the effects of relatively low doses, 20 cGy and 45 cGy , respectively. We use a range of characterization techniques including scanning electron microscopy, Raman spectroscopy and X-ray photoelectron spectroscopy to quantify the effects of the radiation dose on inherent properties of the nanotubes. Specifically we find that the radiation exposure results in a reduction in the sp2 nature of the nanotube bond structure. Moreover, our analysis indicates that the exposure results in nanotubes that have an increased defect density which ultimately effects the electrical properties of the nanotubes.

GSFC Contributions to the NATO X-ray Astronomy Institute, Erice, July 1979. [X-ray spectra of supernova remants, galactic X-ray sources, active galactic nuclei, and clusters of galaxies

NASA Technical Reports Server (NTRS)

Holt, S. S.; Mushotzky, R. F.

1979-01-01

An overview of X-ray astronomical spectroscopy in general is presented and results obtained by HEAO 1 and 2 as well as earlier spacecraft are examined. Particular emphasis is given to the spectra of supernova remnants; galactic binary X-ray sources, cataclysmic variables, bulges, pulsars, and stars; the active nuclei of Seyfert 1 galaxy, BL Lac, and quasars; the diffuse X-ray background; and galactic clusters.

X-ray Weak Broad-line Qquasars: Absorption or Intrinsic X-ray Weakness

NASA Technical Reports Server (NTRS)

Mushotzky, Richard (Technical Monitor); Risaliti, Guida

2005-01-01

XMM observations of X-ray weak quasars have been performed during 2003 and 2004. The data for all the observations have become available in 2004 (there has been a delay of several months on the initial schedule, due to high background flares which contaminated the observations: as a consequence, most of them had to be rescheduled). We have reduced and analyzed all the data, and obtained interesting scientific results. Out of the eight sources, 4 are confirmed to be extremely X-ray weak, in agreement with the results of previous Chandra observations. 3 sources are confined to be highly variable both in flux (by factor 20-50) and in spectral properties (dramatic changes in spectral index). For both these groups of objects we are completing a publication: 1) For the X-ray weak sources, a paper is submitted with a complete analysis of the X-ray spectra both from Chandra and XMM-Newton, and a comparison with optical and near-IR photometry obtained from all-sky surveys. Possible models for the unusual spectral energy distribution of these sources are also presented. 2) For the variable sources, a paper is being finalized where the X-ray spectra obtained with XMM-Newton are compared with previous X-ray observations and with observations at other wavelengths. It is shown that these sources are high luminosity and extreme cases of the highly variable class of narrow-line Seyfert Is. In order to further understand the nature of these X-ray weak quasars, we submitted proposals for spectroscopy at optical and infrared telescopes. We obtained time at the TNG 4 meter telescope for near-IR observations and at the Hobby-Eberly Telescope for optical high-resolution spectroscopy. These observations have been performed in early 2004. They will complement the XMM data and will lead to understanding of whether the X-ray weakness of these sources is an intrinsic property or is due to absorption by circum-nuclear material. The infrared spectra of the variable sources have been already

Crystallography with online optical and X-ray absorption spectroscopies demonstrates an ordered mechanism in copper nitrite reductase.

PubMed

Hough, Michael A; Antonyuk, Svetlana V; Strange, Richard W; Eady, Robert R; Hasnain, S Samar

2008-04-25

Nitrite reductases are key enzymes that perform the first committed step in the denitrification process and reduce nitrite to nitric oxide. In copper nitrite reductases, an electron is delivered from the type 1 copper (T1Cu) centre to the type 2 copper (T2Cu) centre where catalysis occurs. Despite significant structural and mechanistic studies, it remains controversial whether the substrates, nitrite, electron and proton are utilised in an ordered or random manner. We have used crystallography, together with online X-ray absorption spectroscopy and optical spectroscopy, to show that X-rays rapidly and selectively photoreduce the T1Cu centre, but that the T2Cu centre does not photoreduce directly over a typical crystallographic data collection time. Furthermore, internal electron transfer between the T1Cu and T2Cu centres does not occur, and the T2Cu centre remains oxidised. These data unambiguously demonstrate an 'ordered' mechanism in which electron transfer is gated by binding of nitrite to the T2Cu. Furthermore, the use of online multiple spectroscopic techniques shows their value in assessing radiation-induced redox changes at different metal sites and demonstrates the importance of ensuring the correct status of redox centres in a crystal structure determination. Here, optical spectroscopy has shown a very high sensitivity for detecting the change in T1Cu redox state, while X-ray absorption spectroscopy has reported on the redox status of the T2Cu site, as this centre has no detectable optical absorption.

Scanning Microscopes Using X Rays and Microchannels

NASA Technical Reports Server (NTRS)

Wang, Yu

2003-01-01

Scanning microscopes that would be based on microchannel filters and advanced electronic image sensors and that utilize x-ray illumination have been proposed. Because the finest resolution attainable in a microscope is determined by the wavelength of the illumination, the xray illumination in the proposed microscopes would make it possible, in principle, to achieve resolutions of the order of nanometers about a thousand times as fine as the resolution of a visible-light microscope. Heretofore, it has been necessary to use scanning electron microscopes to obtain such fine resolution. In comparison with scanning electron microscopes, the proposed microscopes would likely be smaller, less massive, and less expensive. Moreover, unlike in scanning electron microscopes, it would not be necessary to place specimens under vacuum. The proposed microscopes are closely related to the ones described in several prior NASA Tech Briefs articles; namely, Miniature Microscope Without Lenses (NPO-20218), NASA Tech Briefs, Vol. 22, No. 8 (August 1998), page 43; and Reflective Variants of Miniature Microscope Without Lenses (NPO-20610), NASA Tech Briefs, Vol. 26, No. 9 (September 2002) page 6a. In all of these microscopes, the basic principle of design and operation is the same: The focusing optics of a conventional visible-light microscope are replaced by a combination of a microchannel filter and a charge-coupled-device (CCD) image detector. A microchannel plate containing parallel, microscopic-cross-section holes much longer than they are wide is placed between a specimen and an image sensor, which is typically the CCD. The microchannel plate must be made of a material that absorbs the illuminating radiation reflected or scattered from the specimen. The microchannels must be positioned and dimensioned so that each one is registered with a pixel on the image sensor. Because most of the radiation incident on the microchannel walls becomes absorbed, the radiation that reaches the

Characterization of the calcification of cardiac valve bioprostheses by environmental scanning electron microscopy and vibrational spectroscopy.

PubMed

Delogne, Christophe; Lawford, Patricia V; Habesch, Steven M; Carolan, Vikki A

2007-10-01

Bioprosthetic heart valve tissue and associated calcification were studied in their natural state, using environmental scanning electron microscopy (ESEM). Energy dispersive X-ray micro-analysis, X-ray diffraction, Fourier-transform infrared and Raman spectroscopy were used to characterize the various calcific deposits observed with ESEM. The major elements present in calcified valves were also analyzed by inductively coupled plasma-optical emission spectroscopy. To better understand the precursor formation of the calcific deposits, results from the elemental analyses were statistically correlated. ESEM revealed the presence of four broad types of calcium phosphate crystal morphology. In addition, two main patterns of organization of calcific deposits were observed associated with the collagen fibres. Energy dispersive X-ray micro-analysis identified the crystals observed by ESEM as salts containing mainly calcium and phosphate with ratios from 1.340 (possibly octacalcium phosphate, which has a Ca/P ratio of 1.336) to 2.045 (possibly hydroxyapatite with incorporation of carbonate and metal ion contaminants, such as silicon and magnesium, in the crystal lattice). Raman and fourier-transform infrared spectroscopy also identified the presence of carbonate and the analyses showed spectral features very similar to a crystalline hydroxyapatite spectrum, also refuting the presence of precursor phases such as beta-tricalcium phosphate, octacalcium phosphate and dicalcium phosphate dihydrate. The results of this study raised the possibility of the presence of precursor phases associated with the early stages of calcification.

Identifying anthropogenic uranium compounds using soft X-ray near-edge absorption spectroscopy

NASA Astrophysics Data System (ADS)

Ward, Jesse D.; Bowden, Mark; Tom Resch, C.; Eiden, Gregory C.; Pemmaraju, C. D.; Prendergast, David; Duffin, Andrew M.

2017-01-01

Uranium ores mined for industrial use are typically acid-leached to produce yellowcake and then converted into uranium halides for enrichment and purification. These anthropogenic chemical forms of uranium are distinct from their mineral counterparts. The purpose of this study is to use soft X-ray absorption spectroscopy to characterize several common anthropogenic uranium compounds important to the nuclear fuel cycle. Chemical analyses of these compounds are important for process and environmental monitoring. X-ray absorption techniques have several advantages in this regard, including element-specificity, chemical sensitivity, and high spectral resolution. Oxygen K-edge spectra were collected for uranyl nitrate, uranyl fluoride, and uranyl chloride, and fluorine K-edge spectra were collected for uranyl fluoride and uranium tetrafluoride. Interpretation of the data is aided by comparisons to calculated spectra. The effect of hydration state on the sample, a potential complication in interpreting oxygen K-edge spectra, is discussed. These compounds have unique spectral signatures that can be used to identify unknown samples.

Identifying anthropogenic uranium compounds using soft X-ray near-edge absorption spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ward, Jesse D.; Bowden, Mark; Tom Resch, C.

2017-01-01

Uranium ores mined for industrial use are typically acid-leached to produce yellowcake and then converted into uranium halides for enrichment and purification. These anthropogenic chemical forms of uranium are distinct from their mineral counterparts. The purpose of this study is to use soft X-ray absorption spectroscopy to characterize several common anthropogenic uranium compounds important to the nuclear fuel cycle. Non-destructive chemical analyses of these compounds is important for process and environmental monitoring and X-ray absorption techniques have several advantages in this regard, including element-specificity, chemical sensitivity, and high spectral resolution. Oxygen K-edge spectra were collected for uranyl nitrate, uranyl fluoride,more » and uranyl chloride, and fluorine K-edge spectra were collected for uranyl fluoride and uranium tetrafluoride. Interpretation of the data is aided by comparisons to calculated spectra. These compounds have unique spectral signatures that can be used to identify unknown samples.« less

X-ray absorption spectroscopy and EPR studies of oriented spinach thylakoid preparations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Andrews, J.C.