Acemetacin cocrystal structures by powder X-ray diffraction.

PubMed

Bolla, Geetha; Chernyshev, Vladimir; Nangia, Ashwini

2017-05-01

Cocrystals of acemetacin drug (ACM) with nicotinamide (NAM), p -aminobenzoic acid (PABA), valerolactam (VLM) and 2-pyridone (2HP) were prepared by melt crystallization and their X-ray crystal structures determined by high-resolution powder X-ray diffraction. The powerful technique of structure determination from powder data (SDPD) provided details of molecular packing and hydrogen bonding in pharmaceutical cocrystals of acemetacin. ACM-NAM occurs in anhydrate and hydrate forms, whereas the other structures crystallized in a single crystalline form. The carboxylic acid group of ACM forms theacid-amide dimer three-point synthon R 3 2 (9) R 2 2 (8) R 3 2 (9) with three different syn amides (VLM, 2HP and caprolactam). The conformations of the ACM molecule observed in the crystal structures differ mainly in the mutual orientation of chlorobenzene fragment and the neighboring methyl group, being anti (type I) or syn (type II). ACM hydrate, ACM-NAM, ACM-NAM-hydrate and the piperazine salt of ACM exhibit the type I conformation, whereas ACM polymorphs and other cocrystals adopt the ACM type II conformation. Hydrogen-bond interactions in all the crystal structures were quantified by calculating their molecular electrostatic potential (MEP) surfaces. Hirshfeld surface analysis of the cocrystal surfaces shows that about 50% of the contribution is due to a combination of strong and weak O⋯H, N⋯H, Cl⋯H and C⋯H interactions. The physicochemical properties of these cocrystals are under study.

Acemetacin cocrystal structures by powder X-ray diffraction

PubMed Central

Bolla, Geetha

2017-01-01

Cocrystals of acemetacin drug (ACM) with nicotinamide (NAM), p-aminobenzoic acid (PABA), valerolactam (VLM) and 2-pyridone (2HP) were prepared by melt crystallization and their X-ray crystal structures determined by high-resolution powder X-ray diffraction. The powerful technique of structure determination from powder data (SDPD) provided details of molecular packing and hydrogen bonding in pharmaceutical cocrystals of acemetacin. ACM–NAM occurs in anhydrate and hydrate forms, whereas the other structures crystallized in a single crystalline form. The carboxylic acid group of ACM forms theacid–amide dimer three-point synthon R 3 2(9)R 2 2(8)R 3 2(9) with three different syn amides (VLM, 2HP and caprolactam). The conformations of the ACM molecule observed in the crystal structures differ mainly in the mutual orientation of chlorobenzene fragment and the neighboring methyl group, being anti (type I) or syn (type II). ACM hydrate, ACM—NAM, ACM–NAM-hydrate and the piperazine salt of ACM exhibit the type I conformation, whereas ACM polymorphs and other cocrystals adopt the ACM type II conformation. Hydrogen-bond interactions in all the crystal structures were quantified by calculating their molecular electrostatic potential (MEP) surfaces. Hirshfeld surface analysis of the cocrystal surfaces shows that about 50% of the contribution is due to a combination of strong and weak O⋯H, N⋯H, Cl⋯H and C⋯H interactions. The physicochemical properties of these cocrystals are under study. PMID:28512568

Simulation and Laboratory results of the Hard X-ray Polarimeter: X-Calibur

NASA Astrophysics Data System (ADS)

Guo, Qingzhen; Beilicke, M.; Kislat, F.; Krawczynski, H.

2014-01-01

X-ray polarimetry promises to give qualitatively new information about high-energy sources, such as binary black hole (BH) systems, Microquasars, active galactic nuclei (AGN), GRBs, etc. We designed, built and tested a hard X-ray polarimeter 'X-Calibur' to be flown in the focal plane of the InFOCuS grazing incidence hard X-ray telescope in 2014. X-Calibur combines a low-Z Compton scatterer with a CZT detector assembly to measure the polarization of 20- 80 keV X-rays making use of the fact that polarized photons Compton scatter preferentially perpendicular to the E field orientation. X-Calibur achieves a high detection efficiency of order unity. We optimized of the design of the instrument based on Monte Carlo simulations of polarized and unpolarized X-ray beams and of the most important background components. We have calibrated and tested X-Calibur extensively in the laboratory at Washington University and at the Cornell High-Energy Synchrotron Source (CHESS). Measurements using the highly polarized synchrotron beam at CHESS confirm the polarization sensitivity of the instrument. In this talk we report on the optimization of the design of the instrument based on Monte Carlo simulations, as well as results of laboratory calibration measurements characterizing the performance of the instrument.

The Optics and Alignment of the Divergent Beam Laboratory X-ray Powder Diffractometer and its Calibration Using NIST Standard Reference Materials.

PubMed

Cline, James P; Mendenhall, Marcus H; Black, David; Windover, Donald; Henins, Albert

2015-01-01

The laboratory X-ray powder diffractometer is one of the primary analytical tools in materials science. It is applicable to nearly any crystalline material, and with advanced data analysis methods, it can provide a wealth of information concerning sample character. Data from these machines, however, are beset by a complex aberration function that can be addressed through calibration with the use of NIST Standard Reference Materials (SRMs). Laboratory diffractometers can be set up in a range of optical geometries; considered herein are those of Bragg-Brentano divergent beam configuration using both incident and diffracted beam monochromators. We review the origin of the various aberrations affecting instruments of this geometry and the methods developed at NIST to align these machines in a first principles context. Data analysis methods are considered as being in two distinct categories: those that use empirical methods to parameterize the nature of the data for subsequent analysis, and those that use model functions to link the observation directly to a specific aspect of the experiment. We consider a multifaceted approach to instrument calibration using both the empirical and model based data analysis methods. The particular benefits of the fundamental parameters approach are reviewed.

Spectroscopy of X-ray Photoionized Plasmas in the Laboratory

NASA Astrophysics Data System (ADS)

Liedahl, Duane A.; Loisel, Guillaume; Bailey, James E.; Nagayama, Taisuke; Hansen, Stephanie B.; Rochau, Gregory; Fontes, Christopher J.; Mancini, Roberto; Kallman, Timothy R.

2018-06-01

The physical processes operating in astrophysical plasmas --- heating, cooling, ionization, recombination, level population kinetics, and radiation transport --- are all accessible to observation in the laboratory. What distinguishes X-ray photoionized plasmas from the more common case of high-temperature collisionally-ionized plasmas is the elevated level of importance of the radiation/matter interaction. The advent of laboratory facilities with the capability to generate high-powered X-ray sources has provided the means by which to study this interaction, which is also fundamental to active galactic nuclei and other accretion-powered objects. We discuss recent and ongoing experiments, with an emphasis on X-ray spectroscopic measurements of silicon plasmas obtained at the Sandia Z Pulsed Power Facility.

13.1 micrometers hard X-ray focusing by a new type monocapillary X-ray optic designed for common laboratory X-ray source

NASA Astrophysics Data System (ADS)

Sun, Xuepeng; zhang, Xiaoyun; Zhu, Yu; Wang, Yabing; Shang, Hongzhong; Zhang, Fengshou; Liu, Zhiguo; Sun, Tianxi

2018-04-01

A new type of monocapillary X-ray optic, called 'two bounces monocapillary X-ray optics' (TBMXO), is proposed for generating a small focal spot with high power-density gain for micro X-ray analysis, using a common laboratory X-ray source. TBMXO is consists of two parts: an ellipsoidal part and a tapered part. Before experimental testing, the TBMXO was simulated by the ray tracing method in MATLAB. The simulated results predicted that the proposed TBMXO would produce a smaller focal spot with higher power-density gain than the ellipsoidal monocapillary X-ray optic (EMXO). In the experiment, the TBMXO performance was tested by both an optical device and a Cu target X-ray tube with focal spot of 100 μm. The results indicated that the TBMXO had a slope error of 57.6 μrad and a 13.1 μm focal spot and a 1360 gain in power density were obtained.

On the response of Y 3Al 5O 12: Ce (YAG: Ce) powder scintillating screens to medical imaging X-rays

NASA Astrophysics Data System (ADS)

Kandarakis, I.; Cavouras, D.; Sianoudis, I.; Nikolopoulos, D.; Episkopakis, A.; Linardatos, D.; Margetis, D.; Nirgianaki, E.; Roussou, M.; Melissaropoulos, P.; Kalivas, N.; Kalatzis, I.; Kourkoutas, K.; Dimitropoulos, N.; Louizi, A.; Nomicos, C.; Panayiotakis, G.

2005-02-01

The aim of this study was to examine Y 3Al 5O 12:Ce (also known as YAG:Ce) powder scintillator under X-ray imaging conditions. This material shows a very fast scintillation decay time and it has never been used in X-ray medical imaging. In the present study various scintillator layers (screens) with coating thickness ranging from 13 to 166 mg/cm 2 were prepared in our laboratory by sedimentation of Y 3Al 5O 12: Ce powder. Optical emission spectra and light emission efficiency (spectrum area over X-ray exposure) of the layers were measured under X-ray excitation using X-ray tube voltages (80-120 kVp) often employed in general medical radiography and fluoroscopy. Spectral compatibility with various optical photon detectors (photodiodes, photocathodes, charge coupled devices, films) and intrinsic conversion efficiency values were determined using emission spectrum data. In addition, parameters related to X-ray detection, energy absorption efficiency and K-fluorescence characteristic emission were calculated. A theoretical model describing radiation and light transfer through scattering media was used to fit experimental data. Intrinsic conversion efficiency (η≈0.03-0.05) and light attenuation coefficients (σ≈26.5 cm/g) were derived through this fitting. Y 3Al 5O 12:Ce showed peak emission in the wavelength range 530-550 nm. The light emission efficiency was found to be maximum for the 107 mg/cm 2 layer. Due to its "green" emission spectrum, Y 3Al 5O 12:Ce showed excellent compatibility (of the order of 0.9) with the sensitivity of many currently used photodetectors. Taking into account its very fast response Y 3Al 5O 12:Ce could be considered for application in X-ray imaging especially in various digital detectors.

Validation of powder X-ray diffraction following EN ISO/IEC 17025.

PubMed

Eckardt, Regina; Krupicka, Erik; Hofmeister, Wolfgang

2012-05-01

Powder X-ray diffraction (PXRD) is used widely in forensic science laboratories with the main focus of qualitative phase identification. Little is found in literature referring to the topic of validation of PXRD in the field of forensic sciences. According to EN ISO/IEC 17025, the method has to be tested for several parameters. Trueness, specificity, and selectivity of PXRD were tested using certified reference materials or a combination thereof. All three tested parameters showed the secure performance of the method. Sample preparation errors were simulated to evaluate the robustness of the method. These errors were either easily detected by the operator or nonsignificant for phase identification. In case of the detection limit, a statistical evaluation of the signal-to-noise ratio showed that a peak criterion of three sigma is inadequate and recommendations for a more realistic peak criterion are given. Finally, the results of an international proficiency test showed the secure performance of PXRD. © 2012 American Academy of Forensic Sciences.

X-Ray Spectroscopic Laboratory Experiments In Support of the NASA X-Ray Astronomy Flight Program

NASA Technical Reports Server (NTRS)

Kahn, Steven M.; Savin, D. W.; Gu, M. F.; Beiersdorfer, P.; Liedahl, D. A.; Brown, G.; Utter, S.

1998-01-01

During the 1997 performance period, our work focused on the L-shell X-ray emission from highly charged iron ions in the 10-18 A region. Details of our accomplishments in 1997 are presented in the following. We start by describing the laboratory measurements made and their impact on the X-ray flight program and conclude by an overview of new instrumental capabilities developed for uses in the coming year.

Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

NASA Astrophysics Data System (ADS)

Tanaka, M.; Katsuya, Y.; Matsushita, Y.

2013-03-01

The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe2O4 and Fe3O4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe2+/Fe3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

Quantitative analysis of crystalline pharmaceuticals in powders and tablets by a pattern-fitting procedure using X-ray powder diffraction data.

PubMed

Yamamura, S; Momose, Y

2001-01-16

A pattern-fitting procedure for quantitative analysis of crystalline pharmaceuticals in solid dosage forms using X-ray powder diffraction data is described. This method is based on a procedure for pattern-fitting in crystal structure refinement, and observed X-ray scattering intensities were fitted to analytical expressions including some fitting parameters, i.e. scale factor, peak positions, peak widths and degree of preferred orientation of the crystallites. All fitting parameters were optimized by the non-linear least-squares procedure. Then the weight fraction of each component was determined from the optimized scale factors. In the present study, well-crystallized binary systems, zinc oxide-zinc sulfide (ZnO-ZnS) and salicylic acid-benzoic acid (SA-BA), were used as the samples. In analysis of the ZnO-ZnS system, the weight fraction of ZnO or ZnS could be determined quantitatively in the range of 5-95% in the case of both powders and tablets. In analysis of the SA-BA systems, the weight fraction of SA or BA could be determined quantitatively in the range of 20-80% in the case of both powders and tablets. Quantitative analysis applying this pattern-fitting procedure showed better reproducibility than other X-ray methods based on the linear or integral intensities of particular diffraction peaks. Analysis using this pattern-fitting procedure also has the advantage that the preferred orientation of the crystallites in solid dosage forms can be also determined in the course of quantitative analysis.

Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

NASA Astrophysics Data System (ADS)

Post, J. E.; Bish, D. L.; Heaney, P. J.

2006-05-01

Sepiolite is a hydrous Mg-silicate clay mineral with fibrous morphology that typically occurs as fine-grained, poorly crystalline masses. It occurs in a wide variety of geological environments and has been mined for centuries because of its many uses, e.g. in the pharmaceutical, fertilizer, and pesticide industries. Its versatile functionality derives from the large surface area and microporosity that are characteristic of the material. In recent years, sepiolite has received considerable attention with regard to the adsorption of organics, for use as a support for catalysts, as a molecular sieve, and as an inorganic membrane for ultrafiltration. Because of its fine-grained and poorly crystalline nature, it has not been possible to study sepiolite's crystal structure using single-crystal X-ray diffraction methods, and consequently many details of the structure are still not well known. In this study, Rietveld refinements using synchrotron powder X-ray diffraction data were used to investigate the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room- temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic water site. The RT structure under vacuum retained only ~1/8 of the zeolitic water and the volume decreased 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic water is lost by ~390 K, accompanied by a decrease in the a and c unit-cell parameters. Above ~600 K the sepiolite structure folds as one-half of the crystallographically bound water is lost. Rietveld refinements of the "anhydrous" sepiolite structure reveal that, in general, unit-cell parameters a, b, â and volume steadily decrease with increasing temperature; there is an obvious change in slope at ~820 K suggesting a phase

X-Ray Spectroscopic Laboratory Experiments in Support of the X-Ray Astronomy Program

NASA Technical Reports Server (NTRS)

Kahn, Steven M.

1997-01-01

Our program is to perform a series of laboratory investigations designed to resolved significant atomic physics uncertainties that limit the interpretation of cosmic X-ray spectra. Specific goals include a quantitative characterization of Fe L-shell spectra; the development of new techniques to simulate Maxwellian plasmas using an Electron Beam Ion Trap (EBIT); and the measurement of dielectronic recombination rates for photoionized gas. New atomic calculations have also been carried out in parallel with the laboratory investigations.

High-resolution x-ray tomography using laboratory sources

NASA Astrophysics Data System (ADS)

Tkachuk, Andrei; Feser, Michael; Cui, Hongtao; Duewer, Fred; Chang, Hauyee; Yun, Wenbing

2006-08-01

X-ray computed tomography (XCT) is a powerful nondestructive 3D imaging technique, which enables the visualization of the three dimensional structure of complex, optically opaque samples. High resolution XCT using Fresnel zone plate lenses has been confined in the past to synchrotron radiation centers due to the need for a bright and intense source of x-rays. This confinement severely limits the availability and accessibility of x-ray microscopes and the wide proliferation of this methodology. We are describing a sub-50nm resolution XCT system operating at 8 keV in absorption and Zernike phase contrast mode based on a commercially available laboratory x-ray source. The system utilizes high-efficiency Fresnel zone plates with an outermost zone width of 35 nm and 700 nm structure height resulting in a current spatial resolution better than 50 nm. In addition to the technical description of the system and specifications, we present application examples in the semiconductor field.

Macroscopic X-ray Powder Diffraction Scanning: Possibilities for Quantitative and Depth-Selective Parchment Analysis.

PubMed

Vanmeert, Frederik; De Nolf, Wout; Dik, Joris; Janssens, Koen

2018-06-05

At or below the surface of painted works of art, valuable information is present that provides insights into an object's past, such as the artist's technique and the creative process that was followed or its conservation history but also on its current state of preservation. Various noninvasive techniques have been developed over the past 2 decades that can probe this information either locally (via point analysis) or on a macroscopic scale (e.g., full-field imaging and raster scanning). Recently macroscopic X-ray powder diffraction (MA-XRPD) mapping using laboratory X-ray sources was developed. This method can visualize highly specific chemical distributions at the macroscale (dm 2 ). In this work we demonstrate the synergy between the quantitative aspects of powder diffraction and the noninvasive scanning capability of MA-XRPD highlighting the potential of the method to reveal new types of information. Quantitative data derived from a 15th/16th century illuminated sheet of parchment revealed three lead white pigments with different hydrocerussite-cerussite compositions in specific pictorial elements, while quantification analysis of impurities in the blue azurite pigment revealed two distinct azurite types: one rich in barite and one in quartz. Furthermore, on the same artifact, the depth-selective possibilities of the method that stem from an exploitation of the shift of the measured diffraction peaks with respect to reference data are highlighted. The influence of different experimental parameters on the depth-selective analysis results is briefly discussed. Promising stratigraphic information could be obtained, even though the analysis is hampered by not completely understood variations in the unit cell dimensions of the crystalline pigment phases.

Parts per Million Powder X-ray Diffraction

DOE PAGES

Newman, Justin A.; Schmitt, Paul D.; Toth, Scott J.; ...

2015-10-14

Here in this paper we demonstrate the use of second harmonic generation (SHG) microscopy-guided synchrotron powder X-ray diffraction (PXRD) for the detection of trace crystalline active pharmaceutical ingredients in a common polymer blend. The combined instrument is capable of detecting 100 ppm crystalline ritonavir in an amorphous hydroxypropyl methylcellulose matrix with a high signal-to-noise ratio (>5000). The high spatial resolution afforded by SHG microscopy allows for the use of a minibeam collimator to reduce the total volume of material probed by synchrotron PXRD. The reduction in probed volume results in reduced background from amorphous material. The ability to detect lowmore » crystalline loading has the potential to improve measurements in the formulation pipeline for pharmaceutical solid dispersions, for which even trace quantities of crystalline active ingredients can negatively impact the stability and bioavailability of the final drug product.« less

X-ray/VUV transmission gratings for astrophysical and laboratory applications

NASA Technical Reports Server (NTRS)

Schattenburg, M. L.; Anderson, E. H.; Smith, Henry I.

1990-01-01

This paper describes the techniques used to fabricate deep-submicron-period transmission gratings for astrophysical and laboratory applications, with special attention given to the major steps involved in the transmission grating fabrication. These include the holographic lithography procedure used to pattern the master transmission grating, the fabrication of X-ray mask, the X-ray lithography step used to transfer the X-ray mask pattern into a substrate, and the electroplating of the substrate to form the final grating pattern. The various ways in which transmission gratings can be used in X-ray and VUV spectroscopy are discussed together with some examples of experiments reported in the literature.

X-ray Production in a Laboratory Streamer Discharge

NASA Astrophysics Data System (ADS)

Lehtinen, N. G.; Kochkin, P.; Ostgaard, N.

2016-12-01

A 1D model of a 1-m scale laboratory discharge streamer system [Lehtinen et al, 2016, http://meetingorganizer.copernicus.org/EGU2016/EGU2016-6180.pdf] has reproduced the experimentally-observed [Kochkin et al, 2014, doi:10.1088/0022-3727/47/14/145203] detached streamer systems (pilots). The pilots grow in both directions and thus produce counter-streamers which collide with forward-moving streamers, a mechanism which was proposed to lead to the production of x-rays [Cooray, 2009, doi:10.1016/j.jastp.2009.07.010]. However, the 1D model is insufficient to analyse this process because in this model the electric field between the colliding streamers is averaged in the transverse direction and therefore the maximum fields are underestimated. In this presentation, we include the microscopic processes in the modeling of streamer propagation in order to calculate accurately the electric field enhancement between colliding streamers of opposite polarity. We evaluate the temporal and spatial characteristics of the enhanced electric field, which define the production of relativistic runaway electrons and x-rays. The x-ray output for the conditions occuring in a laboratory discharge is compared to the experimental data [Kochkin et al, 2012, doi:10.1088/0022-3727/45/42/425202; 2015, doi:10.1088/0022-3727/48/2/025205]. We note that the previous modeling of streamer collisions [Ihaddadene and Celestin, 2015, doi:10.1002/2015GL064623] obtained the field enhancements which are insufficient for the observed x-ray production.

Conformational analysis of an acyclic tetrapeptide: ab-initio structure determination from X-ray powder diffraction, Hirshfeld surface analysis and electronic structure.

PubMed

Das, Uday; Naskar, Jishu; Mukherjee, Alok Kumar

2015-12-01

A terminally protected acyclic tetrapeptide has been synthesized, and the crystal structure of its hydrated form, Boc-Tyr-Aib-Tyr-Ile-OMe·2H2O (1), has been determined directly from powder X-ray diffraction data. The backbone conformation of tetrapeptide (1) exhibiting two consecutive β-turns is stabilized by two 4 → 1 intramolecular N-H · · · O hydrogen bonds. In the crystalline state, the tetrapeptide molecules are assembled through water-mediated O-H · · · O hydrogen bonds to form two-dimensional molecular sheets, which are further linked by intermolecular C-H · · · O hydrogen bonds into a three-dimensional supramolecular framework. The molecular electrostatic potential (MEP) surface of (1) has been used to supplement the crystallographic observations. The nature of intermolecular interactions in (1) has been analyzed quantitatively through the Hirshfeld surface and two-dimensional fingerprint plot. The DFT optimized molecular geometry of (1) agrees closely with that obtained from the X-ray structure analysis. The present structure analysis of Boc-Tyr-Aib-Tyr-Ile-OMe·2H2 O (1) represents a case where ab-initio crystal structure of an acyclic tetrapeptide with considerable molecular flexibility has been accomplished from laboratory X-ray powder diffraction data. Copyright © 2015 European Peptide Society and John Wiley & Sons, Ltd.

Laboratory manual: mineral X-ray diffraction data retrieval/plot computer program

USGS Publications Warehouse

Hauff, Phoebe L.; VanTrump, George

1976-01-01

The Mineral X-Ray Diffraction Data Retrieval/Plot Computer Program--XRDPLT (VanTrump and Hauff, 1976a) is used to retrieve and plot mineral X-ray diffraction data. The program operates on a file of mineral powder diffraction data (VanTrump and Hauff, 1976b) which contains two-theta or 'd' values, and intensities, chemical formula, mineral name, identification number, and mineral group code. XRDPLT is a machine-independent Fortran program which operates in time-sharing mode on a DEC System i0 computer and the Gerber plotter (Evenden, 1974). The program prompts the user to respond from a time-sharing terminal in a conversational format with the required input information. The program offers two major options: retrieval only; retrieval and plot. The first option retrieves mineral names, formulas, and groups from the file by identification number, by the mineral group code (a classification by chemistry or structure), or by searches based on the formula components. For example, it enables the user to search for minerals by major groups (i.e., feldspars, micas, amphiboles, oxides, phosphates, carbonates) by elemental composition (i.e., Fe, Cu, AI, Zn), or by a combination of these (i.e., all copper-bearing arsenates). The second option retrieves as the first, but also plots the retrieved 2-theta and intensity values as diagrammatic X-ray powder patterns on mylar sheets or overlays. These plots can be made using scale combinations compatible with chart recorder diffractograms and 114.59 mm powder camera films. The overlays are then used to separate or sieve out unrelated minerals until unknowns are matched and identified.

New developments of X-ray fluorescence imaging techniques in laboratory

NASA Astrophysics Data System (ADS)

Tsuji, Kouichi; Matsuno, Tsuyoshi; Takimoto, Yuki; Yamanashi, Masaki; Kometani, Noritsugu; Sasaki, Yuji C.; Hasegawa, Takeshi; Kato, Shuichi; Yamada, Takashi; Shoji, Takashi; Kawahara, Naoki

2015-11-01

X-ray fluorescence (XRF) analysis is a well-established analytical technique with a long research history. Many applications have been reported in various fields, such as in the environmental, archeological, biological, and forensic sciences as well as in industry. This is because XRF has a unique advantage of being a nondestructive analytical tool with good precision for quantitative analysis. Recent advances in XRF analysis have been realized by the development of new x-ray optics and x-ray detectors. Advanced x-ray focusing optics enables the making of a micro x-ray beam, leading to micro-XRF analysis and XRF imaging. A confocal micro-XRF technique has been applied for the visualization of elemental distributions inside the samples. This technique was applied for liquid samples and for monitoring chemical reactions such as the metal corrosion of steel samples in the NaCl solutions. In addition, a principal component analysis was applied for reducing the background intensity in XRF spectra obtained during XRF mapping, leading to improved spatial resolution of confocal micro-XRF images. In parallel, the authors have proposed a wavelength dispersive XRF (WD-XRF) imaging spectrometer for a fast elemental imaging. A new two dimensional x-ray detector, the Pilatus detector was applied for WD-XRF imaging. Fast XRF imaging in 1 s or even less was demonstrated for Euro coins and industrial samples. In this review paper, these recent advances in laboratory-based XRF imaging, especially in a laboratory setting, will be introduced.

Thermal analysis, X-ray powder diffraction and electron microscopy data related with the production of 1:1 Caffeine:Glutaric Acid cocrystals.

PubMed

Duarte, Íris; Andrade, Rita; Pinto, João F; Temtem, Márcio

2016-09-01

The data presented in this article are related to the production of 1:1 Caffeine:Glutaric Acid cocrystals as part of the research article entitled "Green production of cocrystals using a new solvent-free approach by spray congealing" (Duarte et al., 2016) [1]. More specifically, here we present the thermal analysis and the X-ray powder diffraction data for pure Glutaric Acid, used as a raw material in [1]. We also include the X-ray powder diffraction and electron microscopy data obtained for the 1:1 Caffeine:Glutaric Acid cocrystal (form II) produced using the cooling crystallization method reported in "Operating Regions in Cooling Cocrystallization of Caffeine and Glutaric Acid in Acetonitrile" (Yu et al., 2010) [2]. Lastly, we show the X-ray powder diffraction data obtained for assessing the purity of the 1:1 Caffeine:Glutaric cocrystals produced in [1].

X-Ray Diffraction Reference Intensity Ratios of Amorphous and Poorly Crystalline Phases: Implications for CheMin on the Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Morris, R. V.; Achilles, C. N.; Chipera, S. J.; Ming, D. W.; Rampe, E. B.

2013-01-01

The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity is an X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of providing the mineralogical and chemical compositions of rocks and soils on the surface of Mars. CheMin uses a microfocus X-ray tube with a Co target, transmission geometry, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. Piezoelectric vibration of the cell is used to randomize the sample to reduce preferred orientation effects. Instrument details are provided in [1, 2, 3]. Analyses of rock and soil samples by the Mars Exploration Rovers (MER) show nanophase ferric oxide (npOx) is a significant component of the Martian global soil [4] and is thought to be one of the major contributing phases that the Curiosity rover will encounter if a soil sample is analyzed in Gale Crater. Because of the nature of this material, npOx will likely contribute to an X-ray amorphous or short-order component of a XRD pattern measured by the CheMin instrument.

K(3)TaF(8) from laboratory X-ray powder data.

PubMed

Smrcok, Lubomír; Cerný, Radovan; Boca, Miroslav; Macková, Iveta; Kubíková, Blanka

2010-02-01

The crystal structure of tripotassium octafluoridotantalate, K(3)TaF(8), determined from laboratory powder diffraction data by the simulated annealing method and refined by total energy minimization in the solid state, is built from discrete potassium cations, fluoride anions and monocapped trigonal-prismatic [TaF(7)](2-) ions. All six atoms in the asymmetric unit are in special positions of the P6(3)mc space group: the Ta and one F atom in the 2b (3m) sites, the K and two F atoms in the 6c (m) sites, and one F atom in the 2a (3m) site. The structure consists of face-sharing K(6) octahedra with a fluoride anion at the center of each octahedron, forming chains of composition [FK(3)](2+) running along [001] with isolated [TaF(7)](2-) trigonal prisms in between. The structure of the title compound is different from the reported structure of Na(3)TaF(8) and represents a new structure type.

Observation of X-rays from long laboratory negative discharge in STP air

NASA Astrophysics Data System (ADS)

Kochkin, Pavlo; van Deursen, A. P. J.; Ebert, Ute

2014-05-01

Pulses of x-rays emitted by lightning are one of the most intriguing among unsolved problem in physics of lightning. They have been detected from both - natural and rocket-triggered lightning. In natural lightning x-rays were detected during stepped leader process and later were associated with a single step. In triggered lighting x-rays were found to be originated from a tip of a dart leader that also possesses stepping propagation mechanism. Therefore, stepping mechanism is the key to understanding the x-ray pulses generated by lightning. Unfortunately, leader stepping mechanism itself is far from well understood. Negative long laboratory discharges also develop through a formation of a space stem/leader and they also generate bursts of x-ray radiation. In this study we investigate the development of a long negative laboratory spark in particular focusing on its x-ray emission. A 2 MV Marx generator delivers high-voltage standard lightning pulse with 1.2/50 microsec rise/fall time to a spark gap with conical electrodes. The distance between cone tips was varied between 1 m and 1.75 m. An upper voltage limit is set to about 1 MV level. The voltage is measured by capacitive high-voltage divider. Two Pearson 7427 current probes determine the currents through high-voltage and grounded electrodes. Two LaBr3 scintillator detectors were mounted in EMC-cabinets and recorded the x-rays. Picos4 Stanford Optics camera with intensified CCD is placed in 4 m distance from the spark gap and directed perpendicular to the spark plane. The camera allows us to make ns-fast images of pre-breakdown phenomena in controllable time. We discovered new details of space stem/leader formation and development in long laboratory sparks. The connection moment of positive part of the space stem/leader to negative high-voltage is accompanied by intense x-ray emission. Taking into account our previous study on positive discharge, we conclude that encounter between positive and negative streamers

Laboratory simulation of charge exchange-produced X-ray emission from comets.

PubMed

Beiersdorfer, P; Boyce, K R; Brown, G V; Chen, H; Kahn, S M; Kelley, R L; May, M; Olson, R E; Porter, F S; Stahle, C K; Tillotson, W A

2003-06-06

In laboratory experiments using the engineering spare microcalorimeter detector from the ASTRO-E satellite mission, we recorded the x-ray emission of highly charged ions of carbon, nitrogen, and oxygen, which simulates charge exchange reactions between heavy ions in the solar wind and neutral gases in cometary comae. The spectra are complex and do not readily match predictions. We developed a charge exchange emission model that successfully reproduces the soft x-ray spectrum of comet Linear C/1999 S4, observed with the Chandra X-ray Observatory.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

NASA Astrophysics Data System (ADS)

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; Martin, Aiden A.; Depond, Philip J.; Guss, Gabriel M.; Thampy, Vivek; Fong, Anthony Y.; Weker, Johanna Nelson; Stone, Kevin H.; Tassone, Christopher J.; Kramer, Matthew J.; Toney, Michael F.; Van Buuren, Anthony; Matthews, Manyalibo J.

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ˜1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ˜50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes.

PubMed

Calta, Nicholas P; Wang, Jenny; Kiss, Andrew M; Martin, Aiden A; Depond, Philip J; Guss, Gabriel M; Thampy, Vivek; Fong, Anthony Y; Weker, Johanna Nelson; Stone, Kevin H; Tassone, Christopher J; Kramer, Matthew J; Toney, Michael F; Van Buuren, Anthony; Matthews, Manyalibo J

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ∼1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ∼50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

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.

Laboratory-based micro-X-ray fluorescence setup using a von Hamos crystal spectrometer and a focused beam X-ray tube

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

Kayser, Y., E-mail: yves.kayser@psi.ch; Paul Scherrer Institut, 5232 Villigen-PSI; Błachucki, W.

2014-04-15

The high-resolution von Hamos bent crystal spectrometer of the University of Fribourg was upgraded with a focused X-ray beam source with the aim of performing micro-sized X-ray fluorescence (XRF) measurements in the laboratory. The focused X-ray beam source integrates a collimating optics mounted on a low-power micro-spot X-ray tube and a focusing polycapillary half-lens placed in front of the sample. The performances of the setup were probed in terms of spatial and energy resolution. In particular, the fluorescence intensity and energy resolution of the von Hamos spectrometer equipped with the novel micro-focused X-ray source and a standard high-power water-cooled X-raymore » tube were compared. The XRF analysis capability of the new setup was assessed by measuring the dopant distribution within the core of Er-doped SiO{sub 2} optical fibers.« less

Laboratory-Produced X-Ray Photoionized Plasmas for Astrophysics Exploration

NASA Astrophysics Data System (ADS)

Goyon, Clement; Le Pape, Sebastien; Liedahl, Duane; Ma, Tammy; Berzak-Hopkins, Laura; Reverdin, Charles; Rousseaux, Christophe; Renaudin, Patrick; Blancard, Christophe; Nottet, Edouard; Bidault, Niels; Mancini, Roberto; Koenig, Michel

2015-11-01

X-ray photoionized plasmas are rare in the laboratory, but of broad importance in astrophysical objects such as active galactic nuclei, x-ray binaries. Indeed, existing models are not yet able to accurately describe these plasmas where ionization is driven by radiation rather than electron collisions. Here, we describe an experiment on the LULI2000 facility whose versatility allows for measuring the X-ray absorption of the plasma while independently probing its electron density and temperature. The bright X-ray source is created by the two main beams focused inside a gold hohlraum and is used to photoionise a Neon gas jet. Then, a thin gold foil serves as a source of backlit photons for absorption spectroscopy. The transmitted spectrum through the plasma is collected by a crystal spectrometer. We will present the experimental setup used to characterize both plasma conditions and X-ray emission. Then we will show the transmitted spectra through the plasma to observe the transition from collision dominated to radiation dominated ionization and compare it to model predictions. This work was performed under the auspices of the U.S.Department of Energy by Lawrence Livermore Natl Lab under Contract No. DE-AC52-07NA27344.

Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

PubMed Central

Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

2018-01-01

High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

A laboratory system for element specific hyperspectral X-ray imaging.

PubMed

Jacques, Simon D M; Egan, Christopher K; Wilson, Matthew D; Veale, Matthew C; Seller, Paul; Cernik, Robert J

2013-02-21

X-ray tomography is a ubiquitous tool used, for example, in medical diagnosis, explosives detection or to check structural integrity of complex engineered components. Conventional tomographic images are formed by measuring many transmitted X-rays and later mathematically reconstructing the object, however the structural and chemical information carried by scattered X-rays of different wavelengths is not utilised in any way. We show how a very simple; laboratory-based; high energy X-ray system can capture these scattered X-rays to deliver 3D images with structural or chemical information in each voxel. This type of imaging can be used to separate and identify chemical species in bulk objects with no special sample preparation. We demonstrate the capability of hyperspectral imaging by examining an electronic device where we can clearly distinguish the atomic composition of the circuit board components in both fluorescence and transmission geometries. We are not only able to obtain attenuation contrast but also to image chemical variations in the object, potentially opening up a very wide range of applications from security to medical diagnostics.

Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

DOE PAGES

Wang, H.; Kirkham, M. J.; Watkins, T. R.; ...

2016-02-17

N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« less

Kinetic products in coordination networks: ab initio X-ray powder diffraction analysis.

PubMed

Martí-Rujas, Javier; Kawano, Masaki

2013-02-19

Porous coordination networks are materials that maintain their crystal structure as molecular "guests" enter and exit their pores. They are of great research interest with applications in areas such as catalysis, gas adsorption, proton conductivity, and drug release. As with zeolite preparation, the kinetic states in coordination network preparation play a crucial role in determining the final products. Controlling the kinetic state during self-assembly of coordination networks is a fundamental aspect of developing further functionalization of this class of materials. However, unlike for zeolites, there are few structural studies reporting the kinetic products made during self-assembly of coordination networks. Synthetic routes that produce the necessary selectivity are complex. The structural knowledge obtained from X-ray crystallography has been crucial for developing rational strategies for design of organic-inorganic hybrid networks. However, despite the explosive progress in the solid-state study of coordination networks during the last 15 years, researchers still do not understand many chemical reaction processes because of the difficulties in growing single crystals suitable for X-ray diffraction: Fast precipitation can lead to kinetic (metastable) products, but in microcrystalline form, unsuitable for single crystal X-ray analysis. X-ray powder diffraction (XRPD) routinely is used to check phase purity, crystallinity, and to monitor the stability of frameworks upon guest removal/inclusion under various conditions, but rarely is used for structure elucidation. Recent advances in structure determination of microcrystalline solids from ab initio XRPD have allowed three-dimensional structure determination when single crystals are not available. Thus, ab initio XRPD structure determination is becoming a powerful method for structure determination of microcrystalline solids, including porous coordination networks. Because of the great interest across scientific

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

Synthesis of nanostructured vanadium powder by high-energy ball milling: X-ray diffraction and high-resolution electron microscopy characterization

NASA Astrophysics Data System (ADS)

Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran

2016-10-01

Vanadium metal powders, ball milled with different surfactants viz., stearic acid, KCl and NaCl, have been studied by X-ray diffraction and transmission electron microscopy. The surfactants alter the microstructural and morphological characteristics of the powders. Ball milling with stearic acid results in solid-state amorphization, while powders milled with KCl yield vanadium-tungsten carbide nanocomposite mixtures. NaCl proved to be an excellent surfactant for obtaining nanostructured fusion-grade vanadium powders. In order to understand the reaction mechanism behind any interstitial addition in the ball-milled powders, CHNOS analysis was performed.

Development of x-ray laminography under an x-ray microscopic condition

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

Hoshino, Masato; Uesugi, Kentaro; Takeuchi, Akihisa

2011-07-15

An x-ray laminography system under an x-ray microscopic condition was developed to obtain a three-dimensional structure of laterally-extended planar objects which were difficult to observe by x-ray tomography. An x-ray laminography technique was introduced to an x-ray transmission microscope with zone plate optics. Three prototype sample holders were evaluated for x-ray imaging laminography. Layered copper grid sheets were imaged as a laminated sample. Diatomite powder on a silicon nitride membrane was measured to confirm the applicability of this method to non-planar micro-specimens placed on the membrane. The three-dimensional information of diatom shells on the membrane was obtained at a spatialmore » resolution of sub-micron. Images of biological cells on the membrane were also obtained by using a Zernike phase contrast technique.« less

Characterization by X-ray tomography of granulated alumina powder during in situ die compaction

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

Cottrino, Sandrine; Jorand, Yves, E-mail: yves.jorand@insa-lyon.fr; Maire, Eric

2013-07-15

Compaction process, the aim of which being to obtain green bodies with low porosity and small size, is often used before sintering treatment. Prior to die filling, the ceramic powder is generally granulated to improve flowability. However during compaction, density heterogeneity and critical size defects may appear due to intergranule and granule-die wall frictions. In this work, the influence of granule formulation on the compact morphology has been studied. To do so, a compaction setup was installed inside an X-ray tomography equipment so that the evolution of the compact morphology could be analysed during the whole compaction process. We havemore » demonstrated that high humidity rate and the addition of binder in the granule formulation increase density heterogeneity and generate larger defects. - Highlights: • An original compaction set up was installed inside an X-Ray tomography equipment. • The compaction process of granulated ceramic powder is imaged. • The compact green microstructure is quantified and related to the compaction stages. • The most detrimental defects of dry-pressed parts are caused by hollow granules. • Formulations without binder allow a reduction of the number of large defects.« less

Laboratory-size three-dimensional x-ray microscope with Wolter type I mirror optics and an electron-impact water window x-ray source

NASA Astrophysics Data System (ADS)

Ohsuka, Shinji; Ohba, Akira; Onoda, Shinobu; Nakamoto, Katsuhiro; Nakano, Tomoyasu; Miyoshi, Motosuke; Soda, Keita; Hamakubo, Takao

2014-09-01

We constructed a laboratory-size three-dimensional water window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques, and observed bio-medical samples to evaluate its applicability to life science research fields. It consists of a condenser and an objective grazing incidence Wolter type I mirror, an electron-impact type oxygen Kα x-ray source, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit of around 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm scale three-dimensional fine structures were resolved.

Laboratory-size three-dimensional x-ray microscope with Wolter type I mirror optics and an electron-impact water window x-ray source.

PubMed

Ohsuka, Shinji; Ohba, Akira; Onoda, Shinobu; Nakamoto, Katsuhiro; Nakano, Tomoyasu; Miyoshi, Motosuke; Soda, Keita; Hamakubo, Takao

2014-09-01

We constructed a laboratory-size three-dimensional water window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques, and observed bio-medical samples to evaluate its applicability to life science research fields. It consists of a condenser and an objective grazing incidence Wolter type I mirror, an electron-impact type oxygen Kα x-ray source, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit of around 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm scale three-dimensional fine structures were resolved.

Services of the CDRH X-ray calibration laboratory and their traceability to National Standards

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

Cerra, F.; Heaton, H.T.

The X-ray Calibration Laboratory (XCL) of the Center for Devices and Radiological Health (CDRH) provides calibration services for the Food and Drug Administration (FDA). The instruments calibrated are used by FDA and contract state inspectors to verify compliance with federal x-ray performance standards and for national surveys of x-ray trends. In order to provide traceability of measurements, the CDRH XCL is accredited by the National Voluntary Laboratory Accreditation Program (NVLAP) for reference, diagnostic, and x-ray survey instrument calibrations. In addition to these accredited services, the CDRH XCL also calibrates non-invasive kVp meters in single- and three-phase x-ray beams, and thermoluminescentmore » dosimeter (TLD) chips used to measure CT beam profiles. The poster illustrates these services and shows the traceability links back to the National Standards.« less

Characterization of SiGe thin films using a laboratory X-ray instrument.

PubMed

Ulyanenkova, Tatjana; Myronov, Maksym; Benediktovitch, Andrei; Mikhalychev, Alexander; Halpin, John; Ulyanenkov, Alex

2013-08-01

The technique of reciprocal space mapping using X-rays is a recognized tool for the nondestructive characterization of epitaxial films. X-ray scattering from epitaxial Si 0.4 Ge 0.6 films on Si(100) substrates using a laboratory X-ray source was investigated. It is shown that a laboratory source with a rotating anode makes it possible to investigate the material parameters of the super-thin 2-6 nm layers. For another set of partially relaxed layers, 50-200 nm thick, it is shown that from a high-resolution reciprocal space map, conditioned from diffuse scattering on dislocations, it is possible to determine quantitatively from the shape of a diffraction peak (possessing no thickness fringes) additional parameters such as misfit dislocation density and layer thickness as well as concentration and relaxation.

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

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

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at themore » Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ~1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ~50 × 100 μm area. In conclusion, we also discuss the utility of these measurements for model validation and process improvement.« less

An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

DOE PAGES

Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; ...

2018-05-01

In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at themore » Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ~1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ~50 × 100 μm area. In conclusion, we also discuss the utility of these measurements for model validation and process improvement.« less

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

Characterization of SiGe thin films using a laboratory X-ray instrument

PubMed Central

Ulyanenkova, Tatjana; Myronov, Maksym; Benediktovitch, Andrei; Mikhalychev, Alexander; Halpin, John; Ulyanenkov, Alex

2013-01-01

The technique of reciprocal space mapping using X-rays is a recognized tool for the nondestructive characterization of epitaxial films. X-ray scattering from epitaxial Si0.4Ge0.6 films on Si(100) substrates using a laboratory X-ray source was investigated. It is shown that a laboratory source with a rotating anode makes it possible to investigate the material parameters of the super-thin 2–6 nm layers. For another set of partially relaxed layers, 50–200 nm thick, it is shown that from a high-resolution reciprocal space map, conditioned from diffuse scattering on dislocations, it is possible to determine quantitatively from the shape of a diffraction peak (possessing no thickness fringes) additional parameters such as misfit dislocation density and layer thickness as well as concentration and relaxation. PMID:24046495

Demonstration of the feasibility of an integrated x ray laboratory for planetary exploration

NASA Technical Reports Server (NTRS)

Franco, E. D.; Kerner, J. A.; Koppel, L. N.; Boyle, M. J.

1993-01-01

The identification of minerals and elemental compositions is an important component in the geological and exobiological exploration of the solar system. X ray diffraction and fluorescence are common techniques for obtaining these data. The feasibility of combining these analytical techniques in an integrated x ray laboratory compatible with the volume, mass, and power constraints imposed by many planetary missions was demonstrated. Breadboard level hardware was developed to cover the range of diffraction lines produced by minerals, clays, and amorphous; and to detect the x ray fluorescence emissions of elements from carbon through uranium. These breadboard modules were fabricated and used to demonstrate the ability to detect elements and minerals. Additional effort is required to establish the detection limits of the breadboard modules and to integrate diffraction and fluorescence techniques into a single unit. It was concluded that this integrated x ray laboratory capability will be a valuable tool in the geological and exobiological exploration of the solar system.

Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

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

Post,J.; Bish, D.; Heaney, P.

2007-01-01

Rietveld refinements using synchrotron powder X-ray diffraction data were used to study the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room-temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic H{sub 2}O site. The RT structure under vacuum retained only {approx}1/8 of the zeolitic H{sub 2}O and the volume decreased by 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic H{sub 2}O is lost bymore » {approx}390 K, accompanied by a decrease in the a and c unit-cell parameters. Above {approx}600 K the sepiolite structure folds as one-half of the crystallographically bound H{sub 2}O is lost. Rietveld refinements of the 'anhydrous' sepiolite structure reveal that, in general, unit-cell parameters a and b and volume steadily decrease with increasing temperature; there is an obvious change in slope at {approx}820 K suggesting a phase transformation coinciding with the loss of the remaining bound H{sub 2}O molecule.« less

Mg(1 + x)Ir(1 - x) (x = 0, 0.037 and 0.054), a binary intermetallic compound with a new orthorhombic structure type determined from powder and single-crystal X-ray diffraction.

PubMed

Cerný, Radovan; Renaudin, Guillaume; Favre-Nicolin, Vincent; Hlukhyy, Viktor; Pöttgen, Rainer

2004-06-01

The new binary compound Mg(1 + x)Ir(1 - x) (x = 0-0.054) was prepared by melting the elements in the Mg:Ir ratio 2:3 in a sealed tantalum tube under an argon atmosphere in an induction furnace (single crystals) or by annealing cold-pressed pellets of the starting composition Mg:Ir 1:1 in an autoclave under an argon atmosphere (powder sample). The structure was independently solved from high-resolution synchrotron powder and single-crystal X-ray data: Pearson symbol oC304, space group Cmca, lattice parameters from synchrotron powder data a = 18.46948 (6), b = 16.17450 (5), c = 16.82131 (5) A. Mg(1 + x)Ir(1 - x) is a topologically close-packed phase, containing 13 Ir and 12 Mg atoms in the asymmetric unit, and has a narrow homogeneity range. Nearly all the atoms have Frank-Kasper-related coordination polyhedra, with the exception of two Ir atoms, and this compound contains the shortest Ir-Ir distances ever observed. The solution of a rather complex crystal structure from powder diffraction, which was fully confirmed by the single-crystal method, shows the power of powder diffraction in combination with the high-resolution data and the global optimization method.

Skull x-ray

MedlinePlus

X-ray - head; X-ray - skull; Skull radiography; Head x-ray ... Chernecky CC, Berger BJ. Radiography of skull, chest, and cervical spine - diagnostic. In: Chernecky CC, Berger BJ, eds. Laboratory Tests and Diagnostic Procedures . 6th ed. ...

Lithium metal for x-ray filters and refractive optics

NASA Astrophysics Data System (ADS)

Pereira, N. R.; Dufresne, Eric; Dierker, Steve

2001-04-01

Lithium is the most x-ray transparent solid element. Lithium is very stable in dry air with a dew point below -50 C or so, but as the humidity increases lithium starts to react with the air's nitrogen and oxygen. Under usual laboratory conditions a shiny piece of lithium metal becomes a white powder within the hour, preventing lithium's widespread use in x-ray work. Use of lithium as a window for pulsed x-rays demands that lithium withstands corrosion in open air for at least 15 minutes. Protection by a one micron layer of parylene turns out to be enough. Although parylene absorbs soft x-rays 12 times more than lithium, the parylene layer can remain in place for the window application. Lithium is also ideal for refractive x-ray lenses. We are evaluating the performance of such lenses with 10 keV photons from the MHATT-CAT beam line at the Advanced Photon Source. These measurements are in progress: the paper will show the results from these measurements as available.

Transmission in situ and operando high temperature X-ray powder diffraction in variable gaseous environments

NASA Astrophysics Data System (ADS)

Schlicker, Lukas; Doran, Andrew; Schneppmüller, Peter; Gili, Albert; Czasny, Mathias; Penner, Simon; Gurlo, Aleksander

2018-03-01

This work describes a device for time-resolved synchrotron-based in situ and operando X-ray powder diffraction measurements at elevated temperatures under controllable gaseous environments. The respective gaseous sample environment is realized via a gas-tight capillary-in-capillary design, where the gas flow is achieved through an open-end 0.5 mm capillary located inside a 0.7 mm capillary filled with a sample powder. Thermal mass flow controllers provide appropriate gas flows and computer-controlled on-the-fly gas mixing capabilities. The capillary system is centered inside an infrared heated, proportional integral differential-controlled capillary furnace allowing access to temperatures up to 1000 °C.

Statistical data of X-ray emission from laboratory sparks

NASA Astrophysics Data System (ADS)

Kochkin, P.; Deursen, D. V.

2011-12-01

In this study we present a summary of the data of 1331 long laboratory sparks in atmospheric pressure intended for a statistical analysis. A 2 MV, 17kJ Marx generator were used to generate 1.2/52μs shape pulses positive and negative polarity. The generator was connected to a spark gap with cone-shaped electrodes. The distance between high-voltage and grounded electrodes was 1.08 meters. Breakdown voltage between electrodes was about 1MV. X-rays have been detected during the development of the discharge channel. The currents through the grounded electrode and through the high-voltage electrode were recorded separately and simultaneously with the voltage and the X-ray signal. X-rays were registered by two LaBr3(Ce+) scintillation detectors in different positions with respect to the forming discharge channel. Detector D1 was placed immediately under the grounded electrode at 15cm distance. Detector D2 was placed at horizontal distances of 143cm and 210cm, at mid-gap height. We also used lead shields of 1.5, 3, and 4 mm thickness for radiation attenuation measurements. For detector collimation we used shields up to 2 cm thickness. Also no metallic objects with pointed surfaces were present within 2 m from the spark gap. Typical plot of positive discharge presented in Figure 1a. Table 1 shows the summary of the X-ray registrations. Signal detection occurred significantly more for positive polarity discharges than for negative. This dependence was observed for both detectors. For detector D2 the probability of X-ray registration decreased proportional to 1/d2 with increasing the distance d to the breakdown gap from 1m43 to 2m10. Detailed energy spectra and time distribution of X-ray emission were obtained; see for example Fig. 1b. For both polarities of the high voltage, the X-rays only occurred when there was a current at the cathode.

A practical superconducting-microcalorimeter X-ray spectrometer for beamline and laboratory science

DOE PAGES

Doriese, W. B.; Abbamonte, P.; Alpert, B. K.; ...

2017-05-01

We describe a series of microcalorimeter X-ray spectrometers designed for a broad suite of measurement applications. The chief advantage of this type of spectrometer is that it can be orders of magnitude more efficient at collecting X-rays than more traditional high-resolution spectrometers that rely on wavelength-dispersive techniques. This advantage is most useful in applications that are traditionally photon-starved and/or involve radiation-sensitive samples. Each energy-dispersive spectrometer is built around an array of several hundred transition-edge sensors (TESs). TESs are superconducting thin films that are biased into their superconducting-to-normal-metal transitions. The spectrometers share a common readout architecture and many design elements, suchmore » as a compact, 65 mK detector package, 8-column time-division-multiplexed superconducting quantum-interference device readout, and a liquid-cryogen-free cryogenic system that is a two-stage adiabatic-demagnetization refrigerator backed by a pulse-tube cryocooler. We have adapted this flexible architecture to mate to a variety of sample chambers and measurement systems that encompass a range of observing geometries. There are two different types of TES pixels employed. The first, designed for X-ray energies below 10 keV, has a best demonstrated energy resolution of 2.1 eV (full-width-at-half-maximum or FWHM) at 5.9 keV. The second, designed for X-ray energies below 2 keV, has a best demonstrated resolution of 1.0 eV (FWHM) at 500 eV. Our team has now deployed seven of these X-ray spectrometers to a variety of light sources, accelerator facilities, and laboratory-scale experiments; these seven spectrometers have already performed measurements related to their applications. Another five of these spectrometers will come online in the near future. We have applied our TES spectrometers to the following measurement applications: synchrotron-based absorption and emission spectroscopy and energy

A practical superconducting-microcalorimeter X-ray spectrometer for beamline and laboratory science

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

Doriese, W. B.; Abbamonte, P.; Alpert, B. K.

We describe a series of microcalorimeter X-ray spectrometers designed for a broad suite of measurement applications. The chief advantage of this type of spectrometer is that it can be orders of magnitude more efficient at collecting X-rays than more traditional high-resolution spectrometers that rely on wavelength-dispersive techniques. This advantage is most useful in applications that are traditionally photon-starved and/or involve radiation-sensitive samples. Each energy-dispersive spectrometer is built around an array of several hundred transition-edge sensors (TESs). TESs are superconducting thin films that are biased into their superconducting-to-normal-metal transitions. The spectrometers share a common readout architecture and many design elements, suchmore » as a compact, 65 mK detector package, 8-column time-division-multiplexed superconducting quantum-interference device readout, and a liquid-cryogen-free cryogenic system that is a two-stage adiabatic-demagnetization refrigerator backed by a pulse-tube cryocooler. We have adapted this flexible architecture to mate to a variety of sample chambers and measurement systems that encompass a range of observing geometries. There are two different types of TES pixels employed. The first, designed for X-ray energies below 10 keV, has a best demonstrated energy resolution of 2.1 eV (full-width-at-half-maximum or FWHM) at 5.9 keV. The second, designed for X-ray energies below 2 keV, has a best demonstrated resolution of 1.0 eV (FWHM) at 500 eV. Our team has now deployed seven of these X-ray spectrometers to a variety of light sources, accelerator facilities, and laboratory-scale experiments; these seven spectrometers have already performed measurements related to their applications. Another five of these spectrometers will come online in the near future. We have applied our TES spectrometers to the following measurement applications: synchrotron-based absorption and emission spectroscopy and energy

A practical superconducting-microcalorimeter X-ray spectrometer for beamline and laboratory science

NASA Astrophysics Data System (ADS)

Doriese, W. B.; Abbamonte, P.; Alpert, B. K.; Bennett, D. A.; Denison, E. V.; Fang, Y.; Fischer, D. A.; Fitzgerald, C. P.; Fowler, J. W.; Gard, J. D.; Hays-Wehle, J. P.; Hilton, G. C.; Jaye, C.; McChesney, J. L.; Miaja-Avila, L.; Morgan, K. M.; Joe, Y. I.; O'Neil, G. C.; Reintsema, C. D.; Rodolakis, F.; Schmidt, D. R.; Tatsuno, H.; Uhlig, J.; Vale, L. R.; Ullom, J. N.; Swetz, D. S.

2017-05-01

We describe a series of microcalorimeter X-ray spectrometers designed for a broad suite of measurement applications. The chief advantage of this type of spectrometer is that it can be orders of magnitude more efficient at collecting X-rays than more traditional high-resolution spectrometers that rely on wavelength-dispersive techniques. This advantage is most useful in applications that are traditionally photon-starved and/or involve radiation-sensitive samples. Each energy-dispersive spectrometer is built around an array of several hundred transition-edge sensors (TESs). TESs are superconducting thin films that are biased into their superconducting-to-normal-metal transitions. The spectrometers share a common readout architecture and many design elements, such as a compact, 65 mK detector package, 8-column time-division-multiplexed superconducting quantum-interference device readout, and a liquid-cryogen-free cryogenic system that is a two-stage adiabatic-demagnetization refrigerator backed by a pulse-tube cryocooler. We have adapted this flexible architecture to mate to a variety of sample chambers and measurement systems that encompass a range of observing geometries. There are two different types of TES pixels employed. The first, designed for X-ray energies below 10 keV, has a best demonstrated energy resolution of 2.1 eV (full-width-at-half-maximum or FWHM) at 5.9 keV. The second, designed for X-ray energies below 2 keV, has a best demonstrated resolution of 1.0 eV (FWHM) at 500 eV. Our team has now deployed seven of these X-ray spectrometers to a variety of light sources, accelerator facilities, and laboratory-scale experiments; these seven spectrometers have already performed measurements related to their applications. Another five of these spectrometers will come online in the near future. We have applied our TES spectrometers to the following measurement applications: synchrotron-based absorption and emission spectroscopy and energy-resolved scattering

A practical superconducting-microcalorimeter X-ray spectrometer for beamline and laboratory science.

PubMed

Doriese, W B; Abbamonte, P; Alpert, B K; Bennett, D A; Denison, E V; Fang, Y; Fischer, D A; Fitzgerald, C P; Fowler, J W; Gard, J D; Hays-Wehle, J P; Hilton, G C; Jaye, C; McChesney, J L; Miaja-Avila, L; Morgan, K M; Joe, Y I; O'Neil, G C; Reintsema, C D; Rodolakis, F; Schmidt, D R; Tatsuno, H; Uhlig, J; Vale, L R; Ullom, J N; Swetz, D S

2017-05-01

We describe a series of microcalorimeter X-ray spectrometers designed for a broad suite of measurement applications. The chief advantage of this type of spectrometer is that it can be orders of magnitude more efficient at collecting X-rays than more traditional high-resolution spectrometers that rely on wavelength-dispersive techniques. This advantage is most useful in applications that are traditionally photon-starved and/or involve radiation-sensitive samples. Each energy-dispersive spectrometer is built around an array of several hundred transition-edge sensors (TESs). TESs are superconducting thin films that are biased into their superconducting-to-normal-metal transitions. The spectrometers share a common readout architecture and many design elements, such as a compact, 65 mK detector package, 8-column time-division-multiplexed superconducting quantum-interference device readout, and a liquid-cryogen-free cryogenic system that is a two-stage adiabatic-demagnetization refrigerator backed by a pulse-tube cryocooler. We have adapted this flexible architecture to mate to a variety of sample chambers and measurement systems that encompass a range of observing geometries. There are two different types of TES pixels employed. The first, designed for X-ray energies below 10 keV, has a best demonstrated energy resolution of 2.1 eV (full-width-at-half-maximum or FWHM) at 5.9 keV. The second, designed for X-ray energies below 2 keV, has a best demonstrated resolution of 1.0 eV (FWHM) at 500 eV. Our team has now deployed seven of these X-ray spectrometers to a variety of light sources, accelerator facilities, and laboratory-scale experiments; these seven spectrometers have already performed measurements related to their applications. Another five of these spectrometers will come online in the near future. We have applied our TES spectrometers to the following measurement applications: synchrotron-based absorption and emission spectroscopy and energy-resolved scattering

Laboratory-size three-dimensional water-window x-ray microscope with Wolter type I mirror optics

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

Ohsuka, Shinji; The Graduate School for the Creation of New Photonics Industries, 1955-1 Kurematsu-cho, Nishi-ku, Hamamatsu-City, 431-1202; Ohba, Akira

2016-01-28

We constructed a laboratory-size three-dimensional water-window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques. It consists of an electron-impact x-ray source emitting oxygen Kα x-rays, Wolter type I grazing incidence mirror optics, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit better than 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm-scale three-dimensional fine structures were resolved.

3D chemical imaging in the laboratory by hyperspectral X-ray computed tomography

PubMed Central

Egan, C. K.; Jacques, S. D. M.; Wilson, M. D.; Veale, M. C.; Seller, P.; Beale, A. M.; Pattrick, R. A. D.; Withers, P. J.; Cernik, R. J.

2015-01-01

We report the development of laboratory based hyperspectral X-ray computed tomography which allows the internal elemental chemistry of an object to be reconstructed and visualised in three dimensions. The method employs a spectroscopic X-ray imaging detector with sufficient energy resolution to distinguish individual elemental absorption edges. Elemental distributions can then be made by K-edge subtraction, or alternatively by voxel-wise spectral fitting to give relative atomic concentrations. We demonstrate its application to two material systems: studying the distribution of catalyst material on porous substrates for industrial scale chemical processing; and mapping of minerals and inclusion phases inside a mineralised ore sample. The method makes use of a standard laboratory X-ray source with measurement times similar to that required for conventional computed tomography. PMID:26514938

Sub-25-nm laboratory x-ray microscopy using a compound Fresnel zone plate.

PubMed

von Hofsten, Olov; Bertilson, Michael; Reinspach, Julia; Holmberg, Anders; Hertz, Hans M; Vogt, Ulrich

2009-09-01

Improving the resolution in x-ray microscopes is of high priority to enable future applications in nanoscience. However, high-resolution zone-plate optics often have low efficiency, which makes implementation in laboratory microscopes difficult. We present a laboratory x-ray microscope based on a compound zone plate. The compound zone plate utilizes multiple diffraction orders to achieve high resolution while maintaining reasonable efficiency. We analyze the illumination conditions necessary for this type of optics in order to suppress stray light and demonstrate microscopic imaging resolving 25 nm features.

X-ray Heating and Electron Temperature of Laboratory Photoionized Plasmas

NASA Astrophysics Data System (ADS)

Mancini, Roberto; Lockard, Tom; Mayes, Daniel C.; Loisel, Guillaume; Bailey, James E.; Rochau, Gregory; Abdallah, J.; Golovkin, I.

2018-06-01

In separate experiments performed at the Z facility of Sandia National Laboratories two different samples were employed to produce and characterize photoionized plasmas. One was a gas cell filled with neon, and the other was a thin silicon layer coated with plastic. Both samples were driven by the broadband x-ray flux produced at the collapse of a wire array z-pinch implosion. Transmission spectroscopy of a narrowband portion of the x-ray flux was used to diagnose the charge state distribution, and the electron temperature was extracted from a Li-like ion level population ratio. To interpret the temperature measurement, we performed Boltzmann kinetics and radiation-hydrodynamic simulations. We found that non-equilibrium atomic physics and the coupling of the radiation flux to the atomic level population kinetics play a critical role in modeling the x-ray heating of photoionized plasmas. In spite of being driven by similar x-ray drives, differences of ionization and charged state distributions in the neon and silicon plasmas are reflected in the plasma heating and observed electron temperatures.This work was sponsored in part by DOE Office of Science Grant DE-SC0014451, and the Z Facility Fundamental Science Program of SNL.

3D nanoscale imaging of biological samples with laboratory-based soft X-ray sources

NASA Astrophysics Data System (ADS)

Dehlinger, Aurélie; Blechschmidt, Anne; Grötzsch, Daniel; Jung, Robert; Kanngießer, Birgit; Seim, Christian; Stiel, Holger

2015-09-01

In microscopy, where the theoretical resolution limit depends on the wavelength of the probing light, radiation in the soft X-ray regime can be used to analyze samples that cannot be resolved with visible light microscopes. In the case of soft X-ray microscopy in the water-window, the energy range of the radiation lies between the absorption edges of carbon (at 284 eV, 4.36 nm) and oxygen (543 eV, 2.34 nm). As a result, carbon-based structures, such as biological samples, posses a strong absorption, whereas e.g. water is more transparent to this radiation. Microscopy in the water-window, therefore, allows the structural investigation of aqueous samples with resolutions of a few tens of nanometers and a penetration depth of up to 10μm. The development of highly brilliant laser-produced plasma-sources has enabled the transfer of Xray microscopy, that was formerly bound to synchrotron sources, to the laboratory, which opens the access of this method to a broader scientific community. The Laboratory Transmission X-ray Microscope at the Berlin Laboratory for innovative X-ray technologies (BLiX) runs with a laser produced nitrogen plasma that emits radiation in the soft X-ray regime. The mentioned high penetration depth can be exploited to analyze biological samples in their natural state and with several projection angles. The obtained tomogram is the key to a more precise and global analysis of samples originating from various fields of life science.

Characterization of Beryllium Windows for Coherent X-ray Optics

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

Goto, Shunji; Yabashi, Makina; Tamasaku, Kenji

2007-01-19

Beryllium foils fabricated by several processes were characterized using spatially coherent x rays at 1-km beamline of SPring-8. By thickness dependence of bright x-ray spot density due to Fresnel diffraction from several-micron deficiencies, we found that speckles (bright x-ray spots) were due to voids with densities 103-104 mm-3 in powder foils and ingot foils. Compared with powder and ingot foils, a polished physical-vapor-deposited (PVD) beryllium foil gave highly uniform beams with no speckles. The PVD process eliminates the internal voids in principle and the PVD foil is the best for coherent x-ray applications.

X-Ray Data Booklet

Science.gov Websites

X-RAY DATA BOOKLET Center for X-ray Optics and Advanced Light Source Lawrence Berkeley National Laboratory Introduction X-Ray Properties of Elements Electron Binding Energies X-Ray Energy Emission Energies Table of X-Ray Properties Synchrotron Radiation Characteristics of Synchrotron Radiation History of X

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl(6) and other alloys are twinned cubic crystals.

PubMed

Pauling, L

1987-06-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl(6) and Mg(32)(Al,Zn)(49) and the neutron powder diffraction pattern of MnAl(6) are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 A (x-ray) and 23.416 A (neutron) for MnAl(6) and 24.313 A (x-ray) for Mg(32)(Al,Zn)(49).

Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl6 and other alloys are twinned cubic crystals

PubMed Central

Pauling, Linus

1987-01-01

It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl6 and Mg32(Al,Zn)49 and the neutron powder diffraction pattern of MnAl6 are compatible with the proposed 820-atom primitive cubic structure [Pauling, L. (1987) Phys. Rev. Lett. 58, 365-368]. The values found for the edge of the unit cube are 23.365 Å (x-ray) and 23.416 Å (neutron) for MnAl6 and 24.313 Å (x-ray) for Mg32(Al,Zn)49. PMID:16593841

A laboratory based system for laue micro x-ray diffraction.

PubMed

Lynch, P A; Stevenson, A W; Liang, D; Parry, D; Wilkins, S; Tamura, N

2007-02-01

A laboratory diffraction system capable of illuminating individual grains in a polycrystalline matrix is described. Using a microfocus x-ray source equipped with a tungsten anode and prefigured monocapillary optic, a micro-x-ray diffraction system with a 10 microm beam was developed. The beam profile generated by the ellipsoidal capillary was determined using the "knife edge" approach. Measurement of the capillary performance, indicated a beam divergence of 14 mrad and a useable energy bandpass from 5.5 to 19 keV. Utilizing the polychromatic nature of the incident x-ray beam and application of the Laue indexing software package X-Ray Micro-Diffraction Analysis Software, the orientation and deviatoric strain of single grains in a polycrystalline material can be studied. To highlight the system potential the grain orientation and strain distribution of individual grains in a polycrystalline magnesium alloy (Mg 0.2 wt % Nd) was mapped before and after tensile loading. A basal (0002) orientation was identified in the as-rolled annealed alloy; after tensile loading some grains were observed to undergo an orientation change of 30 degrees with respect to (0002). The applied uniaxial load was measured as an increase in the deviatoric tensile strain parallel to the load axis.

Pollen structure visualization using high-resolution laboratory-based hard X-ray tomography.

PubMed

Li, Qiong; Gluch, Jürgen; Krüger, Peter; Gall, Martin; Neinhuis, Christoph; Zschech, Ehrenfried

2016-10-14

A laboratory-based X-ray microscope is used to investigate the 3D structure of unstained whole pollen grains. For the first time, high-resolution laboratory-based hard X-ray microscopy is applied to study pollen grains. Based on the efficient acquisition of statistically relevant information-rich images using Zernike phase contrast, both surface- and internal structures of pine pollen - including exine, intine and cellular structures - are clearly visualized. The specific volumes of these structures are calculated from the tomographic data. The systematic three-dimensional study of pollen grains provides morphological and structural information about taxonomic characters that are essential in palynology. Such studies have a direct impact on disciplines such as forestry, agriculture, horticulture, plant breeding and biodiversity. Copyright © 2016 Elsevier Inc. All rights reserved.

A laboratory demonstration of high-resolution hard X-ray and gamma-ray imaging using Fourier-transform techniques

NASA Technical Reports Server (NTRS)

Palmer, David; Prince, Thomas A.

1987-01-01

A laboratory imaging system has been developed to study the use of Fourier-transform techniques in high-resolution hard X-ray and gamma-ray imaging, with particular emphasis on possible applications to high-energy astronomy. Considerations for the design of a Fourier-transform imager and the instrumentation used in the laboratory studies is described. Several analysis methods for image reconstruction are discussed including the CLEAN algorithm and maximum entropy methods. Images obtained using these methods are presented.

Application of powder X-ray diffraction in studying the compaction behavior of bulk pharmaceutical powders.

PubMed

Bandyopadhyay, Rebanta; Selbo, Jon; Amidon, Gregory E; Hawley, Michael

2005-11-01

This study investigates the effects of crystal lattice deformation on the powder X-ray diffraction (PXRD) patterns of compressed polycrystalline specimen (compacts/tablets) made from molecular, crystalline powders. The displacement of molecules and the corresponding adjustment of interplanar distances (d-spacings) between diffracting planes of PNU-288034 and PNU-177553, which have crystal habits with a high aspect ratio favoring preferred orientation during tableting, are demonstrated by shifts in the diffracted peak positions. The direction of shift in diffracted peak positions suggests a reduction of interplanar d-spacing in the crystals of PNU-288034 and PNU-177553 following compaction. There is also a general reduction of peak intensities following compression at the different compressive loads. The lattice strain representing the reduction in d-spacing is proportional to the original d-spacing of the uncompressed sample suggesting that, as with systems that obey a simple Hooke's law relationship, the further apart the planes of atoms/molecules within the lattice are, the easier it is for them to approach each other under compressive stresses. For a third model compound comprising more equant-shaped crystals of PNU-141659, the shift in diffracted peak positions are consistent with an expansion of lattice spacing after compression. This apparent anomaly is supported by the PXRD studies of the bulk powder consisting of fractured crystals where also, the shift in peak position suggests expansion of the lattice planes. Thus the crystals of PNU-141659 may be fracturing under the compressive loads used to produce the compacts. Additional studies are underway to relate the PXRD observations with the bulk tableting properties of these model compounds.

Six dimensional X-ray Tensor Tomography with a compact laboratory setup

NASA Astrophysics Data System (ADS)

Sharma, Y.; Wieczorek, M.; Schaff, F.; Seyyedi, S.; Prade, F.; Pfeiffer, F.; Lasser, T.

2016-09-01

Attenuation based X-ray micro computed tomography (XCT) provides three-dimensional images with micrometer resolution. However, there is a trade-off between the smallest size of the structures that can be resolved and the measurable sample size. In this letter, we present an imaging method using a compact laboratory setup that reveals information about micrometer-sized structures within samples that are several orders of magnitudes larger. We combine the anisotropic dark-field signal obtained in a grating interferometer and advanced tomographic reconstruction methods to reconstruct a six dimensional scattering tensor at every spatial location in three dimensions. The scattering tensor, thus obtained, encodes information about the orientation of micron-sized structures such as fibres in composite materials or dentinal tubules in human teeth. The sparse acquisition schemes presented in this letter enable the measurement of the full scattering tensor at every spatial location and can be easily incorporated in a practical, commercially feasible laboratory setup using conventional X-ray tubes, thus allowing for widespread industrial applications.

X-ray photoelectron spectroscopy (XPS) investigation of the surface film on magnesium powders.

PubMed

Burke, Paul J; Bayindir, Zeynel; Kipouros, Georges J

2012-05-01

Magnesium (Mg) and its alloys are attractive for use in automotive and aerospace applications because of their low density and good mechanical properties. However, difficulty in forming magnesium and the limited number of available commercial alloys limit their use. Powder metallurgy may be a suitable solution for forming near-net-shape parts. However, sintering pure magnesium presents difficulties due to surface film that forms on the magnesium powder particles. The present work investigates the composition of the surface film that forms on the surface of pure magnesium powders exposed to atmospheric conditions and on pure magnesium powders after compaction under uniaxial pressing at a pressure of 500 MPa and sintering under argon at 600 °C for 40 minutes. Initially, focused ion beam microscopy was utilized to determine the thickness of the surface layer of the magnesium powder and found it to be ~10 nm. The X-ray photoelectron analysis of the green magnesium sample prior to sintering confirmed the presence of MgO, MgCO(3)·3H(2)O, and Mg(OH)(2) in the surface layer of the powder with a core of pure magnesium. The outer portion of the surface layer was found to contain MgCO(3)·3H(2)O and Mg(OH)(2), while the inner portion of the layer is primarily MgO. After sintering, the MgCO(3)·3H(2)O was found to be almost completely absent, and the amount of Mg(OH)(2) was also decreased significantly. This is postulated to occur by decomposition of the compounds to MgO and gases during the high temperature of sintering. An increase in the MgO content after sintering supports this theory.

A readout system for X-ray powder crystallography

NASA Astrophysics Data System (ADS)

Loukas, D.; Haralabidis, N.; Pavlidis, A.; Karvelas, E.; Psycharis ^a, K. Misiakos, V.; Mousa, J.; Dre, Ch.

2000-06-01

A system for capturing and processing data, from radiation detectors, in the field of X-ray crystallography has been developed. The system includes a custom-made mixed analog-digital 16-channel VLSI circuit in 50 μm pitch. Each channel comprises a charge amplifier, a shaper, a comparator and a 21-bit counter. The circuit can be scaled in a daisy chain configuration. Data acquisition is performed with a custom made PCI card while the control software is developed with Visual C++ under the MS Windows NT environment. Performance of a fully operational system, in terms of electronic noise, statistical variations and data capture speed is presented. The noise level permits counting of X-rays down to 8 keV while the counting capability is in excess of 200 kHz. The system is intended for X-ray crystallography with silicon detectors.

Ground Laboratory Soft X-Ray Durability Evaluation of Aluminized Teflon FEP Thermal Control Insulation

NASA Technical Reports Server (NTRS)

Banks, Bruce A.; deGroh, Kim K.; Stueber, Thomas J.; Sechkar, Edward A.

1998-01-01

Metallized Teflon fluorinated ethylene propylene (FEP) thermal control insulation is mechanically degraded if exposed to a sufficient fluence of soft x-ray radiation. Soft x-ray photons (4-8 A in wavelength or 1.55 - 3.2 keV) emitted during solar flares have been proposed as a cause of mechanical properties degradation of aluminized Teflon FEP thermal control insulation on the Hubble Space Telescope (HST). Such degradation can be characterized by a reduction in elongation-to-failure of the Teflon FER Ground laboratory soft x-ray exposure tests of aluminized Teflon FEP were conducted to assess the degree of elongation degradation which would occur as a result of exposure to soft x-rays in the range of 3-10 keV. Tests results indicate that soft x-ray exposure in the 3-10 keV range, at mission fluence levels, does not alone cause the observed reduction in elongation of flight retrieved samples. The soft x-ray exposure facility design, mechanical properties degradation results and implications will be presented.

Enabling three-dimensional densitometric measurements using laboratory source X-ray micro-computed tomography

NASA Astrophysics Data System (ADS)

Pankhurst, M. J.; Fowler, R.; Courtois, L.; Nonni, S.; Zuddas, F.; Atwood, R. C.; Davis, G. R.; Lee, P. D.

2018-01-01

We present new software allowing significantly improved quantitative mapping of the three-dimensional density distribution of objects using laboratory source polychromatic X-rays via a beam characterisation approach (c.f. filtering or comparison to phantoms). One key advantage is that a precise representation of the specimen material is not required. The method exploits well-established, widely available, non-destructive and increasingly accessible laboratory-source X-ray tomography. Beam characterisation is performed in two stages: (1) projection data are collected through a range of known materials utilising a novel hardware design integrated into the rotation stage; and (2) a Python code optimises a spectral response model of the system. We provide hardware designs for use with a rotation stage able to be tilted, yet the concept is easily adaptable to virtually any laboratory system and sample, and implicitly corrects the image artefact known as beam hardening.

Characterization of cubic ceria?zirconia powders by X-ray diffraction and vibrational and electronic spectroscopy

NASA Astrophysics Data System (ADS)

Sánchez Escribano, Vicente; Fernández López, Enrique; Panizza, Marta; Resini, Carlo; Gallardo Amores, José Manuel; Busca, Guido

2003-10-01

The X-ray diffraction (XRD) patterns and the Infrared, Raman and UV-visible spectra of CeO 2ZrO 2 powders prepared by co-precipitation are presented. Raman spectra provide evidence for the largely predominant cubic structure of the powders with CeO 2 molar composition higher than 25%. Also skeletal IR spectra allow to distinguish cubic from tetragonal phases which are instead not easily distinguished on the basis of the XRD patterns. All mixed oxides including pure ceria are strong UV absorbers although also absorb in the violet visible region. By carefully selecting their composition and treatment temperature, the onset of the radiation that they cut off can be chosen in the 425-475 nm interval. Although they are likely metastable, the cubic phases are still pure even after heating at 1173 K for 4 h.

X-ray astronomy in the laboratory with a miniature compact object produced by laser-driven implosion

NASA Astrophysics Data System (ADS)

Fujioka, Shinsuke; Takabe, Hideaki; Yamamoto, Norimasa; Salzmann, David; Wang, Feilu; Nishimura, Hiroaki; Li, Yutong; Dong, Quanli; Wang, Shoujun; Zhang, Yi; Rhee, Yong-Joo; Lee, Yong-Woo; Han, Jae-Min; Tanabe, Minoru; Fujiwara, Takashi; Nakabayashi, Yuto; Zhao, Gang; Zhang, Jie; Mima, Kunioki

2009-11-01

X-ray spectroscopy is an important tool for understanding the extreme photoionization processes that drive the behaviour of non-thermal equilibrium plasmas in compact astrophysical objects such as black holes. Even so, the distance of these objects from the Earth and the inability to control or accurately ascertain the conditions that govern their behaviour makes it difficult to interpret the origin of the features in astronomical X-ray measurements. Here, we describe an experiment that uses the implosion driven by a 3TW, 4kJ laser system to produce a 0.5keV blackbody radiator that mimics the conditions that exist in the neighbourhood of a black hole. The X-ray spectra emitted from photoionized silicon plasmas resemble those observed from the binary stars Cygnus X-3 (refs 7, 8) and Vela X-1 (refs 9, 10 11) with the Chandra X-ray satellite. As well as demonstrating the ability to create extreme radiation fields in a laboratory plasma, our theoretical interpretation of these laboratory spectra contrasts starkly with the generally accepted explanation for the origin of similar features in astronomical observations. Our experimental approach offers a powerful means to test and validate the computer codes used in X-ray astronomy.

Raman scattering and X-ray powder diffraction studies of hydrate layered perovskites: dirubidium aquapentafluoromanganate(III) and dipotassium aquapentafluoroferrate(III)

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

Galicka, Karolina; Slodczyk, Aneta; Ratuszna, Alicja

2004-06-08

The structural and vibrational properties of above mentioned crystals were determined using X-ray powder diffraction and Raman scattering experiments. At room temperature hydrate layered perovskites: Rb{sub 2}MnF{sub 5}{center_dot}H{sub 2}O and K{sub 2}FeF{sub 5}{center_dot}H{sub 2}O exhibit orthorhombic--Cmcm (D{sub 2h}{sup 17}) and monoclinic--C2/c (C{sub 2h}{sup 6}) symmetry. Their structure is built up of MnF{sub 6} or FeF{sub 5}{center_dot}H{sub 2}O octahedra forming trans-linked zig-zag chains or hydrogen bonded zig-zag chains along the major crystallographic direction [0 0 1], respectively. To confirm crystal structures and to describe lattice dynamics of these compounds the vibrational normal modes (in {gamma} point of first Brillouin zone) weremore » calculated on the base of the group theory analysis and compared with the spectra obtained from Raman scattering experiments. A relatively good reliability was obtained for both X-ray powder diffraction and Raman scattering.« less

Simultaneous emissions of X-rays and microwaves from long laboratory sparks and downward lightning leaders

NASA Astrophysics Data System (ADS)

Montanya, J.; Oscar, V. D. V.; Tapia, F. F.

2017-12-01

Since the discovery of the Terrestrial Gamma-ray Flashes more than 20 years ago, investigations on high energy emissions from natural lightning and high voltage laboratory sparks gained significant interest. X-ray emissions from lightning as well from high voltage laboratory sparks have in common the role played by negative leaders/streamers. On the other hand, negative leaders are well known to produce much more VHF and microwave radiation than positive leaders. Moreover, in previous works, microwave emissions from lightning leaders have been attributed to Bremsstrahlung process. The object of this work is to investigate if X-rays and RF microwave emissions share the same origin. We present simultaneous measurements of X-rays and microwaves in high voltage sparks and natural lightning. The instrumentation consists on a NaI(Tl) and LaBr3 scintillation detectors and two different receivers. One is fix tuned at 2.4 GHz with a bandwidth of 5.5 MHz. The second can be tuned at any frequency up to 18 GHz with different selectable bandwidths of 10 MHz, 40 MHz and 100 MHz. In the laboratory, results have shown that all the sparks presented microwave radiation before the breakdown of the gap, either X-rays were detected or not. In the cases where X-rays were identified, microwave emissions peaked at the same time (in the microsecond scale). We found that the power amplitudes of the microwave emissions are related to the applied voltage to the gap. In the same configuration, those cases where X-rays were detected microwave emissions presented higher power levels. The results suggest that in some part of the discharge electrons are very fast accelerated allowing, in some cases, to reach enought energy to produce X-rays. In the field, we have found similar results. On 13th of June of 2015 a bipolar cloud-to-ground flash struck 200 m close to the Eagle Nest instrumented tower (Spanish Pyrenees, 2536 m ASL). The flash presented four strokes and, in all of them, microwave

Characterization of As-polluted soils by laboratory X-ray-based techniques coupled with sequential extractions and electron microscopy: the case of Crocette gold mine in the Monte Rosa mining district (Italy).

PubMed

Allegretta, Ignazio; Porfido, Carlo; Martin, Maria; Barberis, Elisabetta; Terzano, Roberto; Spagnuolo, Matteo

2018-06-24

Arsenic concentration and distribution were studied by combining laboratory X-ray-based techniques (wavelength dispersive X-ray fluorescence (WDXRF), micro X-ray fluorescence (μXRF), and X-ray powder diffraction (XRPD)), field emission scanning electron microscopy equipped with microanalysis (FE-SEM-EDX), and sequential extraction procedure (SEP) coupled to total reflection X-ray fluorescence (TXRF) analysis. This approach was applied to three contaminated soils and one mine tailing collected near the gold extraction plant at the Crocette gold mine (Macugnaga, VB) in the Monte Rosa mining district (Piedmont, Italy). Arsenic (As) concentration, measured with WDXRF, ranged from 145 to 40,200 mg/kg. XRPD analysis evidenced the presence of jarosite and the absence of any As-bearing mineral, suggesting a high weathering grade and strong oxidative conditions. However, small domains of Fe arsenate were identified by combining μXRF with FE-SEM-EDX. SEP results revealed that As was mainly associated to amorphous Fe oxides/hydroxides or hydroxysulfates (50-80%) and the combination of XRPD and FE-SEM-EDX suggested that this phase could be attributed to schwertmannite. On the basis of the reported results, As is scarcely mobile, even if a consistent As fraction (1-3 g As/kg of soil) is still potentially mobilizable. In general, the proposed combination of laboratory X-ray techniques could be successfully employed to unravel environmental issues related to metal(loid) pollution in soil and sediments.

X-ray diffraction-based electronic structure calculations and experimental x-ray analysis for medical and materials applications

NASA Astrophysics Data System (ADS)

Mahato, Dip Narayan

This thesis includes x-ray experiments for medical and materials applications and the use of x-ray diffraction data in a first-principles study of electronic structures and hyperfine properties of chemical and biological systems. Polycapillary focusing lenses were used to collect divergent x rays emitted from conventional x-ray tubes and redirect them to form an intense focused beam. These lenses are routinely used in microbeam x-ray fluorescence analysis. In this thesis, their potential application to powder diffraction and focused beam orthovoltage cancer therapy has been investigated. In conventional x-ray therapy, very high energy (˜ MeV) beams are used, partly to reduce the skin dose. For any divergent beam, the dose is necessarily highest at the entry point, and decays exponentially into the tissue. To reduce the skin dose, high energy beams, which have long absorption lengths, are employed, and rotated about the patient to enter from different angles. This necessitates large expensive specialized equipment. A focused beam could concentrate the dose within the patient. Since this is inherently skin dose sparing, lower energy photons could be employed. A primary concern in applying focused beams to therapy is whether the focus would be maintained despite Compton scattering within the tissue. To investigate this, transmission and focal spot sizes as a function of photon energy of two polycapillary focusing lenses were measured. The effects of tissue-equivalent phantoms of different thicknesses on the focal spot size were studied. Scatter fraction and depth dose were calculated. For powder diffraction, the polycapillary optics provide clean Gaussian peaks, which result in angular resolution that is much smaller than the peak width due to the beam convergence. Powder diffraction (also called coherent scatter) without optics can also be used to distinguish between tissue types that, because they have different nanoscale structures, scatter at different angles

X-ray chemical analyzer for field applications

DOEpatents

Gamba, Otto O. M.

1977-01-01

A self-supporting portable field multichannel X-ray chemical analyzer system comprising a lightweight, flexibly connected, remotely locatable, radioisotope-excited sensing probe utilizing a cryogenically-cooled solid state semi-conductor crystal detector for fast in situ non-destructive, qualitative and quantitative analysis of elements in solid, powder, liquid or slurried form, utilizing an X-ray energy dispersive spectrometry technique.

Asymmetric masks for laboratory-based X-ray phase-contrast imaging with edge illumination.

PubMed

Endrizzi, Marco; Astolfo, Alberto; Vittoria, Fabio A; Millard, Thomas P; Olivo, Alessandro

2016-05-05

We report on an asymmetric mask concept that enables X-ray phase-contrast imaging without requiring any movement in the system during data acquisition. The method is compatible with laboratory equipment, namely a commercial detector and a rotating anode tube. The only motion required is that of the object under investigation which is scanned through the imaging system. Two proof-of-principle optical elements were designed, fabricated and experimentally tested. Quantitative measurements on samples of known shape and composition were compared to theory with good agreement. The method is capable of measuring the attenuation, refraction and (ultra-small-angle) X-ray scattering, does not have coherence requirements and naturally adapts to all those situations in which the X-ray image is obtained by scanning a sample through the imaging system.

Resolution of x-ray parabolic compound refractive diamond lens defined at the home laboratory

NASA Astrophysics Data System (ADS)

Polyakov, S. N.; Zholudev, S. I.; Gasilov, S. V.; Martyushov, S. Yu.; Denisov, V. N.; Terentiev, S. A.; Blank, V. D.

2017-05-01

Here we demonstrate performance of an original lab system designed for testing of X-ray parabolic compound refractive lenses (CRL) manufactured from a high-quality single-crystalline synthetic diamond grown by the high-pressure hightemperature technique. The basic parameters of a diamond CRL comprised from 28 plano-concave lenses such as the focal length of 634 mm, transmissivity of 0.36, field of view of 1 mm and resolution of 6 µm have been determined. Usually such measurements are performed on synchrotron radiation facilities. In this work characterization of CRL was performed by means of instruments and components that are available for laboratories such as the Rigaku 9kW rotating anode X-ray generator, the PANalytical parallel beam X-ray mirror, a 6 m long optical bench, high precision multi-axis goniometers, high resolution X-ray emulsion films, and ultra-fast high-sensitive X-ray area detector PIXel3D. Developed setup was used to find differences between experimental and design parameters, which is very important for the improvement of CRLs manufacturing technology.

Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders.

PubMed

Yun, Yifeng; Zou, Xiaodong; Hovmöller, Sven; Wan, Wei

2015-03-01

Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED) data collection, namely automated diffraction tomography (ADT) and rotation electron diffraction (RED), have been developed. Compared with X-ray diffraction (XRD) and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD) provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni-Se-O-Cl crystals, zeolites, germanates, metal-organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three-dimensional ED methods

Ground Laboratory Soft X-Ray Durability Evaluation of Aluminized Teflon FEP Thermal Control Insulation. Revised

NASA Technical Reports Server (NTRS)

Banks, Bruce A.; deGroh, Kim K.; Stueber, Thomas J.; Sechkar, Edward A.; Hall, Rachelle L.

1998-01-01

Metallized Teflon fluorinated ethylene propylene (FEP) thermal control insulation is mechanically degraded if exposed to a sufficient fluence of soft x-ray radiation. Soft x-ray photons (4-8 A in wavelength or 1.55 - 3.2 keV) emitted during solar flares have been proposed as a cause of mechanical properties degradation of aluminized Teflon FEP thermal control insulation on the Hubble Space Telescope (HST). Such degradation can be characterized by a reduction in elongation-to-failure of the Teflon FEP. Ground laboratory soft x-ray exposure tests of aluminized Teflon FEP were conducted to assess the degree of elongation degradation which would occur as a result of exposure to soft x-rays in the range of 3-10 keV. Tests results indicate that soft x-ray exposure in the 3-10 keV range, at mission fluence levels, does not alone cause the observed reduction in elongation of flight retrieved samples. The soft x-ray exposure facility design, mechanical properties degradation results and implications will be presented.

Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis.

PubMed

Moorhouse, Saul J; Wu, Yue; Buckley, Hannah C; O'Hare, Dermot

2016-11-24

We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses. During the flux synthesis of the n = 4 Aurivillius phase, Bi 5 Ti 3 Fe 0.5 Cr 0.5 O 15 at 950 °C in molten Na 2 SO 4 we observe the progression of numerous metastable phases. Using sequential multiphase Rietveld refinement of the time-dependent in situ XRD data, we are able to obtain mechanistic understanding of this reaction under a range of conditions.

Hard X-ray irradiation of cosmic silicate analogs: structural evolution and astrophysical implications

NASA Astrophysics Data System (ADS)

Gavilan, L.; Jäger, C.; Simionovici, A.; Lemaire, J. L.; Sabri, T.; Foy, E.; Yagoubi, S.; Henning, T.; Salomon, D.; Martinez-Criado, G.

2016-03-01

Context. Protoplanetary disks, interstellar clouds, and active galactic nuclei contain X-ray-dominated regions. X-rays interact with the dust and gas present in such environments. While a few laboratory X-ray irradiation experiments have been performed on ices, X-ray irradiation experiments on bare cosmic dust analogs have been scarce up to now. Aims: Our goal is to study the effects of hard X-rays on cosmic dust analogs via in situ X-ray diffraction. By using a hard X-ray synchrotron nanobeam, we seek to simulate cumulative X-ray exposure on dust grains during their lifetime in these astrophysical environments and provide an upper limit on the effect of hard X-rays on dust grain structure. Methods: We prepared enstatite (MgSiO3) nanograins, which are analogs to cosmic silicates, via the melting-quenching technique. These amorphous grains were then annealed to obtain polycrystalline grains. These were characterized via scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) before irradiation. Powder samples were prepared in X-ray transparent substrates and were irradiated with hard X-rays nanobeams (29.4 keV) provided by beamline ID16B of the European Synchrotron Radiation Facility (Grenoble). X-ray diffraction images were recorded in transmission mode, and the ensuing diffractograms were analyzed as a function of the total X-ray exposure time. Results: We detected the amorphization of polycrystalline silicates embedded in an organic matrix after an accumulated X-ray exposure of 6.4 × 1027 eV cm-2. Pure crystalline silicate grains (without resin) do not exhibit amorphization. None of the amorphous silicate samples (pure and embedded in resin) underwent crystallization. We analyze the evolution of the polycrystalline sample embedded in an organic matrix as a function of X-ray exposure. Conclusions: Loss of diffraction peak intensity, peak broadening, and the disappearance of discrete spots and arcs reveal the amorphization

Investigation of recrystallization of amorphous trehalose through hot-humidity stage X-ray powder diffraction.

PubMed

Jójárt-Laczkovich, Orsolya; Katona, Gábor; Aigner, Zoltán; Szabó-Révész, Piroska

2016-12-01

The aim of this work was an investigation of the physical changes of the amorphous model material spray-dried trehalose through the use of various analytical techniques and to identify a suitable, rapid method able to quantify the changes. The crystallinity changes and recrystallization process of amorphous samples were investigated by hot-humidity stage X-ray powder diffractometry (HH-XRPD) with fresh samples, conventional X-ray powder diffractometry (XRPD) used stored samples and by differential scanning calorimetry (DSC). The data from the three methods were compared and the various forms of trehalose were analysed. HH-XRPD demonstrated that the recrystallization began at 40 and 60°C up to 45% RH and at 70°C up to 30% RH into dihydrate form. At 70°C up to 60% RH the anhydrous form of trehalose appeared too. Conventional XRPD results showed, that in the 28days stored samples the dihydrate form was detected at 40°C, 50% RH. Storage at 60°C, 40% RH resulted in the appearance of the anhydrous form and at 60°C, 50% RH both polymorphic forms were detected. By carrying out the DSC measurements at different temperatures the fraction of recrystallized trehalose dihydrate was detected. The recrystallization investigated by HH-XRPD and DSC followed Avrami kinetics, the calculated rate constants of isothermal crystallization (K) were same. Both HH-XRPD and conventional XRPD was suitable for the detection of the physical changes of the amorphous model material. DSC measurements showed similar results as HH-XRPD. Primarily HH-XRPD could be suggested for prediction, because the method is fast and every changes could be studied on one sample. Copyright © 2016 Elsevier B.V. All rights reserved.

Pollen structure visualization using high-resolution laboratory-based hard X-ray tomography

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

Li, Qiong; Gluch, Jürgen; Krüger, Peter

A laboratory-based X-ray microscope is used to investigate the 3D structure of unstained whole pollen grains. For the first time, high-resolution laboratory-based hard X-ray microscopy is applied to study pollen grains. Based on the efficient acquisition of statistically relevant information-rich images using Zernike phase contrast, both surface- and internal structures of pine pollen - including exine, intine and cellular structures - are clearly visualized. The specific volumes of these structures are calculated from the tomographic data. The systematic three-dimensional study of pollen grains provides morphological and structural information about taxonomic characters that are essential in palynology. Such studies have amore » direct impact on disciplines such as forestry, agriculture, horticulture, plant breeding and biodiversity. - Highlights: • The unstained whole pine pollen was visualized by high-resolution laboratory-based HXRM for the first time. • The comparison study of pollen grains by LM, SEM and high-resolution laboratory-based HXRM. • Phase contrast imaging provides significantly higher contrast of the raw images compared to absorption contrast imaging. • Surface and internal structure of the pine pollen including exine, intine and cellular structures are clearly visualized. • 3D volume data of unstained whole pollen grains are acquired and the specific volumes of the different layer are calculated.« less

Inter-laboratory comparison of X-ray fluorescence analyses of eruptive products of El Chichón Volcano, Chiapas, Mexico

USGS Publications Warehouse

Tilling, Robert I.; Bornhorst, Theodore J.; Taggart, Joseph E.; Rose, William I.; McGee, James J.

1987-01-01

An inter-laboratory comparison has been made of X-ray fluorescence analyses of 10 samples of lava and pumices from El Chichón Volcano, Chiapas, Mexico. Some determinations of major-element constituents agree within analytical uncertainty, whereas others exchibit significant bias. Analyses carried out at the Michigan Technological University (MTU) laboratory are systematically lower in MgO (26–48%), Fetotal(5–18%), CaO (4–15%) and higher in K2O (0–15%) than analyses made at the U.S. Geological Survey (USGS) Denver laboratory. These differences are ascribed in part to a complex combination of calibration assumptionsand mineralogical and particle-size effects inherent in the use of pressed rock-powder pellets in the analytical procedure of the MTU laboratory. Other, but as yet unknown, differences in sample preparation and/or analytical technique may also be important; effects related to natural sample inhomogeneityare believed to be insignificant. The inter-laboratory differences in the analytical data complicated accurate assessment of whether El Chichón magmas have changed composition during the past 300 000 a. Knowledge of such change is needed for understanding petrogenetic history and for such related studies as evaluation of volcanic hazards.

The devitrification of a LAS glass matrix studied by X-ray powder diffraction

NASA Astrophysics Data System (ADS)

Rocherullé, Jean; Bénard-Rocherullé, Patricia

2002-06-01

The crystallisation kinetics of a Li 0.6Al 0.1Si 0.6O 1.65 glass matrix has been performed by means of X-ray powder diffraction. Data diffraction have shown the simultaneous formation of two crystalline phases Li 2SiO 3 and Li 0.6Al 0.6Si 2.4O 6 (so-called virgilite) for heat treatments conducted at 700 and 750 °C. The kinetic parameters of crystallisation have been determined for each phase from several time-dependent X-ray diffraction studies. The two values of the Avrami exponent, close to 1.5, suggest that crystallisation is controlled by a diffusion process, the nucleation being non-existent in the temperature range from 700 to 750 °C. With regard to the activation energy of the overall crystallisation phenomenon, the values obtained, close to 175 kJ mol -1, provide to this glass a relative ability to crystallise compared to others glasses from MSiAlO systems, where M is an alkaline-earth or a rare-earth element. With respect to the Li 0.6Al 0.6Si 2.4O 6 phase, long time heat treatments at 750 °C have revealed a phase transition from the hexagonal symmetry to the tetragonal one. The corresponding value of the Avrami exponent (i.e., 1) suggests a diffusionless transformation with a one-dimensional growth.

Additional evidence from x-ray powder diffraction patterns that icosahedral quasi-crystals of intermetallic compounds are twinned cubic crystals

PubMed Central

Pauling, Linus

1988-01-01

Analysis of the measured values of Q for the weak peaks (small maxima, usually considered to be background fluctuations, “noise”) on the x-ray powder diffraction curves for 17 rapidly quenched alloys leads directly to the conclusion that they are formed by an 820-atom or 1012-atom primitive cubic structure that by icosahedral twinning produces the so-called icosahedral quasi-crystals. PMID:16593948

Low-temperature high magnetic field powder x-ray diffraction setup for field-induced structural phase transition studies from 2 to 300 K and at 0 to 8-T field

NASA Astrophysics Data System (ADS)

Shahee, Aga; Sharma, Shivani; Kumar, Dhirendra; Yadav, Poonam; Bhardwaj, Preeti; Ghodke, Nandkishor; Singh, Kiran; Lalla, N. P.; Chaddah, P.

2016-10-01

A low-temperature and high magnetic field powder x-ray diffractometer (XRD) has been developed at UGC-DAE CSR (UGC: University Grant Commission, DAE: Department of Atomic Energy, and CSR: Consortium for scientific research), Indore, India. The setup has been developed around an 18 kW rotating anode x-ray source delivering Cu-Kα x-rays coming from a vertical line source. It works in a symmetric θ-2θ parallel beam geometry. It consists of a liquid helium cryostat with an 8 T split-pair Nb-Ti superconducting magnet comprising two x-ray windows each covering an angular range of 65°. This is mounted on a non-magnetic type heavy duty goniometer equipped with all necessary motions along with data collection accessories. The incident x-ray beam has been made parallel using a parabolic multilayer mirror. The scattered x-ray is detected using a NaI detector through a 0.1° acceptance solar collimator. To control the motions of the goniometer, a computer programme has been developed. The wide-angle scattering data can be collected in a range of 2°-115° of 2θ with a resolution of ˜0.1°. The whole setup is tightly shielded for the scattered x-rays using a lead hutch. The functioning of the goniometer and the artifacts arising possibly due to the effect of stray magnetic field on the goniometer motions, on the x-ray source, and on the detector have been characterized by collecting powder XRD data of a National Institute of Standards and Technology certified standard reference material LaB6 (SRM-660b) and Si powder in zero-field and in-field conditions. Occurrence of field induced structural-phase transitions has been demonstrated on various samples like Pr0.5Sr0.5MnO3, Nd0.49Sr0.51MnO3-δ and La0.175Pr0.45Ca0.375MnO3 by collecting data in zero field cool and field cool conditions.

Morphology and structural development of reduced anatase-TiO{sub 2} by pure Ti powder upon annealing and nitridation: Synthesis of TiO{sub x} and TiO{sub x}N{sub y} powders

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

Bolokang, A.S., E-mail: Sylvester.Bolokang@transnet.net; DST/CSIR National Centre for Nano-Structured Materials, Council for Scientific and Industrial Research, Pretoria 0001; Transnet Engineering, Product Development, Private Bag X 528, Kilnerpark 0127

2015-02-15

It is well known that nitriding of titanium is suitable for surface coating of biomaterials and in other applications such as anti-reflective coating, while oxygen-rich titanium oxynitride has been applied in thin film resistors and photocatalysis. Thus in this work anatase was reduced with pure titanium powder during annealing in argon. This was done to avoid any metallic contamination and unwanted residual metal doping. As a result, interesting and different types of particle morphology were synthesized when the pre-milled elemental anatase and titanium powders were mixed. The formation of metastable face centred cubic and monoclinic titanium monoxide was detected bymore » the X-ray diffraction technique. The phases were confirmed by energy dispersive X-ray spectroscopy analysis. Raman analysis revealed weak intensity peaks for samples annealed in argon as compared to those annealed under nitrogen. - Graphical abstract: Display Omitted - Highlights: • Reaction of TiO{sub 2} and Ti induced metastable FCC and monoclinic TiO{sub x}. • Compositions of mixed powder were prepared from the unmilled and pre-milled powders. • Nitridation of TiO{sub x} yielded TiO{sub x}N{sub y} phase. • Mixed morphology was observed on all three powder samples.« less

Atomic Calculations and Laboratory Measurements Relevant to X-ray Warm Absorbers

NASA Technical Reports Server (NTRS)

Kallman, Tim; Bautista, M.; Palmeri, P.

2007-01-01

This viewgraph document reviews the atomic calculations and the measurements from the laboratory that are relevant to our understanding of X-Ray Warm Absorbers. Included is a brief discussion of the theoretical and the experimental tools. Also included is a discussion of the challenges, and calculations relevant to dielectronic recombination, photoionization cross sections, and collisional ionization. A review of the models is included, and the sequence that the models were applied.

Combined Approach for the Structural Characterization of Alkali Fluoroscandates: Solid-State NMR, Powder X-ray Diffraction, and Density Functional Theory Calculations.

PubMed

Rakhmatullin, Aydar; Polovov, Ilya B; Maltsev, Dmitry; Allix, Mathieu; Volkovich, Vladimir; Chukin, Andrey V; Boča, Miroslav; Bessada, Catherine

2018-02-05

The structures of several fluoroscandate compounds are presented here using a characterization approach combining powder X-ray diffraction and solid-state NMR. The structure of K 5 Sc 3 F 14 was fully determined from Rietveld refinement performed on powder X-ray diffraction data. Moreover, the local structures of NaScF 4 , Li 3 ScF 6 , KSc 2 F 7 , and Na 3 ScF 6 compounds were studied in detail from solid-state 19 F and 45 Sc NMR experiments. The 45 Sc chemical shift ranges for six- and seven-coordinated scandium environments were defined. The 19 F chemical shift ranges for bridging and terminal fluorine atoms were also determined. First-principles calculations of the 19 F and 45 Sc NMR parameters were carried out using plane-wave basis sets and periodic boundary conditions (CASTEP), and the results were compared with the experimental data. A good agreement between the calculated shielding constants and experimental chemical shifts was obtained. This demonstrates the good potential of computational methods in spectroscopic assignments of solid-state 45 Sc NMR spectroscopy.

Crystal structure of pentasodium hydrogen dicitrate from synchrotron X-ray powder diffraction data and DFT comparison

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

Rammohan, Alagappa; Kaduk, James A.

2017-01-27

The crystal structure of pentasodium hydrogen dicitrate, Na 5H(C 6H 5O 7) 2, has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Each of the two independent citrate anions is joined into a dimer by very strong centrosymmetric O—H...O hydrogen bonds, with O...O distances of 2.419 and 2.409 Å. Four octahedrally coordinated Na +ions share edges to form open layers parallel to theabplane. A fifth Na +ion in trigonal–bipyramidal coordination shares faces with NaO 6octahedra on both sides of these layers.

Compact low power infrared tube furnace for in situ X-ray powder diffraction

NASA Astrophysics Data System (ADS)

Doran, A.; Schlicker, L.; Beavers, C. M.; Bhat, S.; Bekheet, M. F.; Gurlo, A.

2017-01-01

We describe the development and implementation of a compact, low power, infrared heated tube furnace for in situ powder X-ray diffraction experiments. Our silicon carbide (SiC) based furnace design exhibits outstanding thermal performance in terms of accuracy control and temperature ramping rates while simultaneously being easy to use, robust to abuse and, due to its small size and low power, producing minimal impact on surrounding equipment. Temperatures in air in excess of 1100 °C can be controlled at an accuracy of better than 1%, with temperature ramping rates up to 100 °C/s. The complete "add-in" device, minus power supply, fits in a cylindrical volume approximately 15 cm long and 6 cm in diameter and resides as close as 1 cm from other sensitive components of our experimental synchrotron endstation without adverse effects.

X-ray pinhole camera setups used in the Atomki ECR Laboratory for plasma diagnostics.

PubMed

Rácz, R; Biri, S; Pálinkás, J; Mascali, D; Castro, G; Caliri, C; Romano, F P; Gammino, S

2016-02-01

Imaging of the electron cyclotron resonance (ECR) plasmas by using CCD camera in combination with a pinhole is a non-destructive diagnostics method to record the strongly inhomogeneous spatial density distribution of the X-ray emitted by the plasma and by the chamber walls. This method can provide information on the location of the collisions between warm electrons and multiple charged ions/atoms, opening the possibility to investigate the direct effect of the ion source tuning parameters to the plasma structure. The first successful experiment with a pinhole X-ray camera was carried out in the Atomki ECR Laboratory more than 10 years ago. The goal of that experiment was to make the first ECR X-ray photos and to carry out simple studies on the effect of some setting parameters (magnetic field, extraction, disc voltage, gas mixing, etc.). Recently, intensive efforts were taken to investigate now the effect of different RF resonant modes to the plasma structure. Comparing to the 2002 experiment, this campaign used wider instrumental stock: CCD camera with a lead pinhole was placed at the injection side allowing X-ray imaging and beam extraction simultaneously. Additionally, Silicon Drift Detector (SDD) and High Purity Germanium (HPGe) detectors were installed to characterize the volumetric X-ray emission rate caused by the warm and hot electron domains. In this paper, detailed comparison study on the two X-ray camera and detector setups and also on the technical and scientific goals of the experiments is presented.

Production of photoionized plasmas in the laboratory with x-ray line radiation

NASA Astrophysics Data System (ADS)

White, S.; Irwin, R.; Warwick, J. R.; Gribakin, G. F.; Sarri, G.; Keenan, F. P.; Riley, D.; Rose, S. J.; Hill, E. G.; Ferland, G. J.; Han, B.; Wang, F.; Zhao, G.

2018-06-01

In this paper we report the experimental implementation of a theoretically proposed technique for creating a photoionized plasma in the laboratory using x-ray line radiation. Using a Sn laser plasma to irradiate an Ar gas target, the photoionization parameter, ξ =4 π F /Ne , reached values of order 50 ergcm s-1 , where F is the radiation flux in ergc m-2s-1 . The significance of this is that this technique allows us to mimic effective spectral radiation temperatures in excess of 1 keV. We show that our plasma starts to be collisionally dominated before the peak of the x-ray drive. However, the technique is extendable to higher-energy laser systems to create plasmas with parameters relevant to benchmarking codes used to model astrophysical objects.

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

Non-destructive mapping of grain orientations in 3D by laboratory X-ray microscopy

NASA Astrophysics Data System (ADS)

McDonald, S. A.; Reischig, P.; Holzner, C.; Lauridsen, E. M.; Withers, P. J.; Merkle, A. P.; Feser, M.

2015-10-01

The ability to characterise crystallographic microstructure, non-destructively and in three-dimensions, is a powerful tool for understanding many aspects related to damage and deformation mechanisms in polycrystalline materials. To this end, the technique of X-ray diffraction contrast tomography (DCT) using monochromatic synchrotron and polychromatic laboratory X-ray sources has been shown to be capable of mapping crystal grains and their orientations non-destructively in 3D. Here we describe a novel laboratory-based X-ray DCT modality (LabDCT), enabling the wider accessibility of the DCT technique for routine use and in-depth studies of, for example, temporal changes in crystallographic grain structure non-destructively over time through ‘4D’ in situ time-lapse studies. The capability of the technique is demonstrated by studying a titanium alloy (Ti-β21S) sample. In the current implementation the smallest grains that can be reliably detected are around 40 μm. The individual grain locations and orientations are reconstructed using the LabDCT method and the results are validated against independent measurements from phase contrast tomography and electron backscatter diffraction respectively. Application of the technique promises to provide important insights related to the roles of recrystallization and grain growth on materials properties as well as supporting 3D polycrystalline modelling of materials performance.

Non-destructive mapping of grain orientations in 3D by laboratory X-ray microscopy.

PubMed

McDonald, S A; Reischig, P; Holzner, C; Lauridsen, E M; Withers, P J; Merkle, A P; Feser, M

2015-10-23

The ability to characterise crystallographic microstructure, non-destructively and in three-dimensions, is a powerful tool for understanding many aspects related to damage and deformation mechanisms in polycrystalline materials. To this end, the technique of X-ray diffraction contrast tomography (DCT) using monochromatic synchrotron and polychromatic laboratory X-ray sources has been shown to be capable of mapping crystal grains and their orientations non-destructively in 3D. Here we describe a novel laboratory-based X-ray DCT modality (LabDCT), enabling the wider accessibility of the DCT technique for routine use and in-depth studies of, for example, temporal changes in crystallographic grain structure non-destructively over time through '4D' in situ time-lapse studies. The capability of the technique is demonstrated by studying a titanium alloy (Ti-β21S) sample. In the current implementation the smallest grains that can be reliably detected are around 40 μm. The individual grain locations and orientations are reconstructed using the LabDCT method and the results are validated against independent measurements from phase contrast tomography and electron backscatter diffraction respectively. Application of the technique promises to provide important insights related to the roles of recrystallization and grain growth on materials properties as well as supporting 3D polycrystalline modelling of materials performance.

Technological Challenges to X-Ray FELs

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

Nuhn, Heinz-Dieter

1999-09-16

There is strong interest in the development of x-ray free electron lasers (x-ray FELs). The interest is driven by the scientific opportunities provided by intense, coherent x-rays. An x-ray FEL has all the characteristics of a fourth-generation source: brightness several orders of magnitude greater than presently achieved in third-generation sources, full transverse coherence, and sub-picosecond long pulses. The SLAC and DESY laboratories have presented detailed design studies for X-Ray FEL user facilities around the 0.1 nm wavelength-regime (LCLS at SLAC, TESLA X-Ray FEL at DESY). Both laboratories are engaged in proof-of-principle experiments are longer wavelengths (TTF FEL Phase I atmore » 71 nm, VISA at 600-800 nm) with results expected in 1999. The technologies needed to achieve the proposed performances are those of bright electron sources, of acceleration systems capable of preserving the brightness of the source, and of undulators capable of meeting the magnetic and mechanical tolerances that are required for operation in the SASE mode. This paper discusses the technological challenges presented by the X-Ray FEL projects.« less

Phase quantification by X-ray photoemission valence band analysis applied to mixed phase TiO2 powders

NASA Astrophysics Data System (ADS)

Breeson, Andrew C.; Sankar, Gopinathan; Goh, Gregory K. L.; Palgrave, Robert G.

2017-11-01

A method of quantitative phase analysis using valence band X-ray photoelectron spectra is presented and applied to the analysis of TiO2 anatase-rutile mixtures. The valence band spectra of pure TiO2 polymorphs were measured, and these spectral shapes used to fit valence band spectra from mixed phase samples. Given the surface sensitive nature of the technique, this yields a surface phase fraction. Mixed phase samples were prepared from high and low surface area anatase and rutile powders. In the samples studied here, the surface phase fraction of anatase was found to be linearly correlated with photocatalytic activity of the mixed phase samples, even for samples with very different anatase and rutile surface areas. We apply this method to determine the surface phase fraction of P25 powder. This method may be applied to other systems where a surface phase fraction is an important characteristic.

X-ray pinhole camera setups used in the Atomki ECR Laboratory for plasma diagnostics

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

Rácz, R., E-mail: rracz@atomki.hu; Biri, S.; Pálinkás, J.

Imaging of the electron cyclotron resonance (ECR) plasmas by using CCD camera in combination with a pinhole is a non-destructive diagnostics method to record the strongly inhomogeneous spatial density distribution of the X-ray emitted by the plasma and by the chamber walls. This method can provide information on the location of the collisions between warm electrons and multiple charged ions/atoms, opening the possibility to investigate the direct effect of the ion source tuning parameters to the plasma structure. The first successful experiment with a pinhole X-ray camera was carried out in the Atomki ECR Laboratory more than 10 years ago.more » The goal of that experiment was to make the first ECR X-ray photos and to carry out simple studies on the effect of some setting parameters (magnetic field, extraction, disc voltage, gas mixing, etc.). Recently, intensive efforts were taken to investigate now the effect of different RF resonant modes to the plasma structure. Comparing to the 2002 experiment, this campaign used wider instrumental stock: CCD camera with a lead pinhole was placed at the injection side allowing X-ray imaging and beam extraction simultaneously. Additionally, Silicon Drift Detector (SDD) and High Purity Germanium (HPGe) detectors were installed to characterize the volumetric X-ray emission rate caused by the warm and hot electron domains. In this paper, detailed comparison study on the two X-ray camera and detector setups and also on the technical and scientific goals of the experiments is presented.« less

Mineralogy by X-ray Diffraction on Mars: The Chemin Instrument on Mars Science Laboratory

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Bristow, T. F.; Bish, D. L.; Ming, D. W.; Blake, D. F.; Morris, R. V.; Rampe, E. B.; Chipera, S. J.; Treiman, A. H.; Morrison, S. M.;

2011 U.S. National School on Neutron and X-ray Scattering

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

Lang, Jonathan; te Vethuis, Suzanne; Ekkebus, Allen E

The 13th annual U.S. National School on Neutron and X-ray Scattering was held June 11 to 25, 2011, at both Oak Ridge and Argonne National Laboratories. This school brought together 65 early career graduate students from 56 different universities in the US and provided them with a broad introduction to the techniques available at the major large-scale neutron and synchrotron x-ray facilities. This school is focused primarily on techniques relevant to the physical sciences, but also touches on cross-disciplinary bio-related scattering measurements. During the school, students received lectures by over 30 researchers from academia, industry, and national laboratories and participatedmore » in a number of short demonstration experiments at Argonne's Advanced Photon Source (APS) and Oak Ridge's Spallation neutron Source (SNS) and High Flux Isotope Reactor (HFIR) facilities to get hands-on experience in using neutron and synchrotron sources. The first week of this year's school was held at Oak Ridge National Lab, where Lab director Thom Mason welcomed the students and provided a shitorical perspective of the neutron and x-ray facilities both at Oak Ridge and Argonne. The first few days of the school were dedicated to lectures laying out the basics of scattering theory and the differences and complementarity between the neutron and x-ray probes given by Sunil Sinha. Jack Carpenter provided an introduction into how neutrons are generated and detected. After this basic introduction, the students received lectures each morning on specific techniques and conducted demonstration experiments each afternoon on one of 15 different instruments at either the SNS or HFIR. Some of the topics covered during this week of the school included inelastic neutron scattering by Bruce Gaulin, x-ray and neutron reflectivity by Chuck Majkrazak, small-angle scattering by Volker Urban, powder diffraction by Ashfia Huq and diffuse scattering by Gene Ice.« less

Microcalorimeters for High Resolution X-Ray Spectroscopy of Laboratory and Astrophysical Plasmas

NASA Technical Reports Server (NTRS)

Silver, E.; Flowers, Bobby J. (Technical Monitor)

2003-01-01

The proposal has three major objectives. The first focuses on advanced neutron-transmutation-doped (NTD)-based microcalorimeter development. Our goal is to develop an array of microcalorimeters with sub- 5 eV energy resolution that can operate with pile-up-free throughput of at least 100 Hz per pixel. The second objective is to establish our microcalorimeter as an essential x-ray diagnostic for laboratory astrophysics studies. We propose to develop a dedicated microcalorimeter spectrometer for the EBIT (electron beam ion trap). This instrument will incorporate the latest detector and cryogenic technology that we have available. The third objective is to investigate innovative ideas related to possible flight opportunities. These include compact, long lived cryo-systems, ultra-low temperature cold stages, low mass and low power electronics, and novel assemblies of thin windows with high x-ray transmission.

PAL-XFEL soft X-ray scientific instruments and X-ray optics: First commissioning results

NASA Astrophysics Data System (ADS)

Park, Sang Han; Kim, Minseok; Min, Changi-Ki; Eom, Intae; Nam, Inhyuk; Lee, Heung-Soo; Kang, Heung-Sik; Kim, Hyeong-Do; Jang, Ho Young; Kim, Seonghan; Hwang, Sun-min; Park, Gi-Soo; Park, Jaehun; Koo, Tae-Yeong; Kwon, Soonnam

2018-05-01

We report an overview of soft X-ray scientific instruments and X-ray optics at the free electron laser (FEL) of the Pohang Accelerator Laboratory, with selected first-commissioning results. The FEL exhibited a pulse energy of 200 μJ/pulse, a pulse width of <50 fs full width at half maximum, and an energy bandwidth of 0.44% at a photon energy of 850 eV. Monochromator resolving power of 10 500 was achieved. The estimated total time resolution between optical laser and X-ray pulses was <270 fs. A resonant inelastic X-ray scattering spectrometer was set up; its commissioning results are also reported.

A compact dispersive refocusing Rowland circle X-ray emission spectrometer for laboratory, synchrotron, and XFEL applications

DOE PAGES

Holden, William M.; Hoidn, Oliver R.; Ditter, Alexander S.; ...

2017-07-27

X-ray emission spectroscopy is emerging as an important complement to x-ray absorption fine structure spectroscopy, providing a characterization of the occupied electronic density of states local to the species of interest. Here, we present details of the design and performance of a compact x-ray emission spectrometer that uses a dispersive refocusing Rowland (DRR) circle geometry to achieve excellent performance for the 2-2.5 keV range, i.e., especially for the K-edge emission from sulfur and phosphorous. The DRR approach allows high energy resolution even for unfocused x-ray sources. This property enables high count rates in laboratory studies, approaching those of insertion-device beamlinesmore » at third-generation synchrotrons, despite use of only a low-powered, conventional x-ray tube. The spectrometer, whose overall scale is set by use of a 10-cm diameter Rowland circle and a new small-pixel complementary metal-oxide-semiconductor x-ray camera, is easily portable to synchrotron or x-ray free electron laser beamlines. Photometrics from measurements at the Advanced Light Source show excellent overall instrumental efficiency. In addition, the compact size of this instrument lends itself to future multiplexing to gain large factors in net collection efficiency or its implementation in controlled gas gloveboxes either in the lab or in an endstation.« less

Coupling of in-situ X-ray Microtomography Observations with Discrete Element Simulations-Application to Powder Sintering

NASA Astrophysics Data System (ADS)

Olmos, L.; Bouvard, D.; Martin, C. L.; Bellet, D.; Di Michiel, M.

2009-06-01

The sintering of both a powder with a wide particle size distribution (0-63 μm) and of a powder with artificially created pores is investigated by coupling in situ X-ray microtomography observations with Discrete Element simulations. The micro structure evolution of the copper particles is observed by microtomography all along a typical sintering cycle at 1050° C at the European Synchrotron Research Facilities (ESRF, Grenoble, France). A quantitative analysis of the 3D images provides original data on interparticle indentation, coordination and particle displacements throughout sintering. In parallel, the sintering of similar powder systems has been simulated with a discrete element code which incorporates appropriate sintering contact laws from the literature. The initial numerical packing is generated directly from the 3D microtomography images or alternatively from a random set of particles with the same size distribution. The comparison between the information drawn from the simulations and the one obtained by tomography leads to the conclusion that the first method is not satisfactory because real particles are not perfectly spherical as the numerical ones. On the opposite the packings built with the second method show sintering behaviors close to the behaviors of real materials, although particle rearrangement is underestimated by DEM simulations.

Quantitative determination of mineral composition by powder x-ray diffraction

DOEpatents

Pawloski, G.A.

1984-08-10

An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.

Quantitative determination of mineral composition by powder X-ray diffraction

DOEpatents

Pawloski, Gayle A.

1986-01-01

An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.

Solid state characterization and crystal structure from X-ray powder diffraction of two polymorphic forms of ranitidine base.

PubMed

de Armas, Héctor Novoa; Peeters, Oswald M; Blaton, Norbert; Van Gyseghem, Elke; Martens, Johan; Van Haele, Gerrit; Van Den Mooter, Guy

2009-01-01

Ranitidine hydrochloride (RAN-HCl), a known anti-ulcer drug, is the product of reaction between HCl and ranitidine base (RAN-B). RAN-HCl has been extensively studied; however this is not the case of the RAN-B. The solid state characterization of RAN-B polymorphs has been carried out using different analytical techniques (microscopy, thermal analysis, Fourier transform infrared spectrometry in the attenuated total reflection mode, (13)C-CPMAS-NMR spectroscopy and X-ray powder diffraction). The crystal structures of RAN-B form I and form II have been determined using conventional X-ray powder diffraction in combination with simulated annealing and whole profile pattern matching, and refined using rigid-body Rietveld refinement. RAN-B form I is a monoclinic polymorph with cell parameters: a = 7.317(2), b = 9.021(2), c = 25.098(6) A, beta = 95.690(1) degrees and space group P2(1)/c. The form II is orthorhombic: a = 31.252(4), b = 13.052(2), c = 8.0892(11) A with space group Pbca. In RAN-B polymorphs, the nitro group is involved in a strong intramolecular hydrogen bond responsible for the existence of a Z configuration in the enamine portion of the molecules. A tail to tail packing motif can be denoted via intermolecular hydrogen bonds. The crystal structures of RAN-B forms are compared to those of RAN-HCl polymorphs. RAN-B polymorphs are monotropic polymorphic pairs. (c) 2008 Wiley-Liss, Inc. and the American Pharmacists Association

X-ray Spectral Formation In High-mass X-ray Binaries: The Case Of Vela X-1

NASA Astrophysics Data System (ADS)

Akiyama, Shizuka; Mauche, C. W.; Liedahl, D. A.; Plewa, T.

2007-05-01

We are working to develop improved models of radiatively-driven mass flows in the presence of an X-ray source -- such as in X-ray binaries, cataclysmic variables, and active galactic nuclei -- in order to infer the physical properties that determine the X-ray spectra of such systems. The models integrate a three-dimensional time-dependent hydrodynamics capability (FLASH); a comprehensive and uniform set of atomic data, improved calculations of the line force multiplier that account for X-ray photoionization and non-LTE population kinetics, and X-ray emission-line models appropriate to X-ray photoionized plasmas (HULLAC); and a Monte Carlo radiation transport code that simulates Compton scattering and recombination cascades following photoionization. As a test bed, we have simulated a high-mass X-ray binary with parameters appropriate to Vela X-1. While the orbital and stellar parameters of this system are well constrained, the physics of X-ray spectral formation is less well understood because the canonical analytical wind velocity profile of OB stars does not account for the dynamical and radiative feedback effects due to the rotation of the system and to the irradiation of the stellar wind by X-rays from the neutron star. We discuss the dynamical wind structure of Vela X-1 as determined by the FLASH simulation, where in the binary the X-ray emission features originate, and how the spatial and spectral properties of the X-ray emission features are modified by Compton scattering, photoabsorption, and fluorescent emission. This work was performed under the auspices of the U.S. Department of Energy by University of California, Lawrence Livermore National Laboratory under Contract W-7405-Eng-48.

The Viking X ray fluorescence experiment - Sampling strategies and laboratory simulations. [Mars soil sampling

NASA Technical Reports Server (NTRS)

Baird, A. K.; Castro, A. J.; Clark, B. C.; Toulmin, P., III; Rose, H., Jr.; Keil, K.; Gooding, J. L.

1977-01-01

Ten samples of Mars regolith material (six on Viking Lander 1 and four on Viking Lander 2) have been delivered to the X ray fluorescence spectrometers as of March 31, 1977. An additional six samples at least are planned for acquisition in the remaining Extended Mission (to January 1979) for each lander. All samples acquired are Martian fines from the near surface (less than 6-cm depth) of the landing sites except the latest on Viking Lander 1, which is fine material from the bottom of a trench dug to a depth of 25 cm. Several attempts on each lander to acquire fresh rock material (in pebble sizes) for analysis have yielded only cemented surface crustal material (duricrust). Laboratory simulation and experimentation are required both for mission planning of sampling and for interpretation of data returned from Mars. This paper is concerned with the rationale for sample site selections, surface sampler operations, and the supportive laboratory studies needed to interpret X ray results from Mars.

Characterization of photocatalytic TiO 2 powder under varied environments using near ambient pressure X-ray photoelectron spectroscopy

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

Krishnan, Padmaja; Liu, Minghui; Itty, Pierre A.

Consecutive eight study phases under the successive presence and absence of UV irradiation, water vapor, and oxygen were conducted to characterize surface changes in the photocatalytic TiO2 powder using near-ambient-pressure X-ray photoelectron spectroscopy (XPS). Both Ti 2p and O 1s spectra show hysteresis through the experimental course. Under all the study environments, the bridging hydroxyl (OH br) and terminal hydroxyl (OH t) are identified at 1.1–1.3 eV and 2.1–2.3 eV above lattice oxygen, respectively. This enables novel and complementary approach to characterize reactivity of TiO 2 powder. The dynamic behavior of surface-bound water molecules under each study environment is identified,more » while maintaining a constant distance of 1.3 eV from the position of water vapor. In the dark, the continual supply of both water vapor and oxygen is the key factor retaining the activated state of the TiO 2 powder for a time period. Two new surface peaks at 1.7–1.8 and 4.0–4.2 eV above lattice oxygen are designated as peroxides (OOH/H 2O 2) and H 2O 2 dissolved in water, respectively. The persistent peroxides on the powder further explain previously observed prolonged oxidation capability of TiO 2 powder without light irradiation.« less

Characterization of photocatalytic TiO 2 powder under varied environments using near ambient pressure X-ray photoelectron spectroscopy

DOE PAGES

Krishnan, Padmaja; Liu, Minghui; Itty, Pierre A.; ...

2017-02-27

Consecutive eight study phases under the successive presence and absence of UV irradiation, water vapor, and oxygen were conducted to characterize surface changes in the photocatalytic TiO2 powder using near-ambient-pressure X-ray photoelectron spectroscopy (XPS). Both Ti 2p and O 1s spectra show hysteresis through the experimental course. Under all the study environments, the bridging hydroxyl (OH br) and terminal hydroxyl (OH t) are identified at 1.1–1.3 eV and 2.1–2.3 eV above lattice oxygen, respectively. This enables novel and complementary approach to characterize reactivity of TiO 2 powder. The dynamic behavior of surface-bound water molecules under each study environment is identified,more » while maintaining a constant distance of 1.3 eV from the position of water vapor. In the dark, the continual supply of both water vapor and oxygen is the key factor retaining the activated state of the TiO 2 powder for a time period. Two new surface peaks at 1.7–1.8 and 4.0–4.2 eV above lattice oxygen are designated as peroxides (OOH/H 2O 2) and H 2O 2 dissolved in water, respectively. The persistent peroxides on the powder further explain previously observed prolonged oxidation capability of TiO 2 powder without light irradiation.« less

Non-destructive mapping of grain orientations in 3D by laboratory X-ray microscopy

PubMed Central

McDonald, S. A.; Reischig, P.; Holzner, C.; Lauridsen, E. M.; Withers, P. J.; Merkle, A. P.; Feser, M.

2015-01-01

The ability to characterise crystallographic microstructure, non-destructively and in three-dimensions, is a powerful tool for understanding many aspects related to damage and deformation mechanisms in polycrystalline materials. To this end, the technique of X-ray diffraction contrast tomography (DCT) using monochromatic synchrotron and polychromatic laboratory X-ray sources has been shown to be capable of mapping crystal grains and their orientations non-destructively in 3D. Here we describe a novel laboratory-based X-ray DCT modality (LabDCT), enabling the wider accessibility of the DCT technique for routine use and in-depth studies of, for example, temporal changes in crystallographic grain structure non-destructively over time through ‘4D’ in situ time-lapse studies. The capability of the technique is demonstrated by studying a titanium alloy (Ti-β21S) sample. In the current implementation the smallest grains that can be reliably detected are around 40 μm. The individual grain locations and orientations are reconstructed using the LabDCT method and the results are validated against independent measurements from phase contrast tomography and electron backscatter diffraction respectively. Application of the technique promises to provide important insights related to the roles of recrystallization and grain growth on materials properties as well as supporting 3D polycrystalline modelling of materials performance. PMID:26494523

High Pressure X-Ray Crystallography With the Diamond Cell at NIST/NBS

PubMed Central

Piermarini, Gasper J.

2001-01-01

Scientists in the Crystallography Section at NIST/NBS made several outstanding contributions which greatly promoted the development and advancement of high pressure x-ray crystallography during the second-half of the 20th century. These milestone achievements or “firsts” included: (1) the invention of the lever-arm type diamond anvil cell (DAC) in 1958; (2) the development of DAC technology for powder x-ray diffraction at high pressure in 1960; (3) the introduction of DAC methodology for single crystal x-ray diffraction at high pressure in 1964; (4) the invention of the optical fluorescence ruby method of pressure measurement in 1971; and (5) the discovery of hydrostatic pressure-transmitting media useful to unprecedented pressures for that time. These achievements provided the spark that ignited the explosion of activity in high pressure research that occurred in laboratories throughout the world during the latter part of the 20th century. It is still going on, unabated, today. An estimated 5000 DACs were built during the last 40 years. PMID:27500054

Producing X-rays at the APS

ScienceCinema

None

2017-12-09

An introduction and overview of the Advanced Photon Source at Argonne National Laboratory, the technology that produces the brightest X-ray beams in the Western Hemisphere, and the research carried out by scientists using those X-rays.

Active x-ray optics for Generation-X, the next high resolution x-ray observatory

NASA Astrophysics Data System (ADS)

Elvis, Martin; Brissenden, R. J.; Fabbiano, G.; Schwartz, D. A.; Reid, P.; Podgorski, W.; Eisenhower, M.; Juda, M.; Phillips, J.; Cohen, L.; Wolk, S.

2006-06-01

X-rays provide one of the few bands through which we can study the epoch of reionization, when the first galaxies, black holes and stars were born. To reach the sensitivity required to image these first discrete objects in the universe needs a major advance in X-ray optics. Generation-X (Gen-X) is currently the only X-ray astronomy mission concept that addresses this goal. Gen-X aims to improve substantially on the Chandra angular resolution and to do so with substantially larger effective area. These two goals can only be met if a mirror technology can be developed that yields high angular resolution at much lower mass/unit area than the Chandra optics, matching that of Constellation-X (Con-X). We describe an approach to this goal based on active X-ray optics that correct the mid-frequency departures from an ideal Wolter optic on-orbit. We concentrate on the problems of sensing figure errors, calculating the corrections required, and applying those corrections. The time needed to make this in-flight calibration is reasonable. A laboratory version of these optics has already been developed by others and is successfully operating at synchrotron light sources. With only a moderate investment in these optics the goals of Gen-X resolution can be realized.

The Ferrara hard X-ray facility for testing/calibrating hard X-ray focusing telescopes

NASA Astrophysics Data System (ADS)

Loffredo, Gianluca; Frontera, Filippo; Pellicciotta, Damiano; Pisa, Alessandro; Carassiti, Vito; Chiozzi, Stefano; Evangelisti, Federico; Landi, Luca; Melchiorri, Michele; Squerzanti, Stefano

2005-12-01

We will report on the current configuration of the X-ray facility of the University of Ferrara recently used to perform reflectivity tests of mosaic crystals and to calibrate the experiment JEM X aboard Integral. The facility is now located in the technological campus of the University of Ferrara in a new building (named LARIX laboratory= LARge Italian X-ray facility) that includes a tunnel 100 m long with, on the sides, two large experimental rooms. The facility is being improved for determining the optical axis of mosaic crystals in Laue configuration, for calibrating Laue lenses and hard X-ray mirror prototypes.

Study of Initial Stages of Ball-Milling of Cu Powder Using X-ray Diffraction

NASA Astrophysics Data System (ADS)

Gayathri, N.; Mukherjee, Paramita

2018-04-01

The initial stage of size refinement of Cu powder is studied using detailed X-ray diffraction (XRD) analysis to understand the mechanism of formation of nanomaterials during the ball-milling process. The study was restricted to samples obtained for milling time up to 240 min to understand the deformation mechanism at the early stages of ball milling. Various model based approaches for the analysis of the XRD were used to study the evolution of the microstructural parameters such as domain size and microstrain along the different crystallographic planes. It was seen that the domain size saturates at a low value along the (311) plane whereas the size along the (220) and (200) plane is still higher. The r.m.s microstrain showed a non-monotonic change along the different crystallographic directions up to the milling time of 240 min.

Quantification of febuxostat polymorphs using powder X-ray diffraction technique.

PubMed

Qiu, Jing-bo; Li, Gang; Sheng, Yue; Zhu, Mu-rong

2015-03-25

Febuxostat is a pharmaceutical compound with more than 20 polymorphs of which form A is most widely used and usually exists in a mixed polymorphic form with form G. In the present study, a quantification method for polymorphic form A and form G of febuxostat (FEB) has been developed using powder X-ray diffraction (PXRD). Prior to development of a quantification method, pure polymorphic form A and form G are characterized. A continuous scan with a scan rate of 3° min(-1) over an angular range of 3-40° 2θ is applied for the construction of the calibration curve using the characteristic peaks of form A at 12.78° 2θ (I/I0100%) and form G at 11.72° 2θ (I/I0100%). The linear regression analysis data for the calibration plots shows good linear relationship with R(2)=0.9985 with respect to peak area in the concentration range 10-60 wt.%. The method is validated for precision, recovery and ruggedness. The limits of detection and quantitation are 1.5% and 4.6%, respectively. The obtained results prove that the method is repeatable, sensitive and accurate. The proposed developed PXRD method can be applied for the quantitative analysis of mixtures of febuxostat polymorphs (forms A and G). Copyright © 2015 Elsevier B.V. All rights reserved.

Synchrotron X-ray studies of model SOFC cathodes, part II: Porous powder cathodes

DOE PAGES

Chang, Kee-Chul; Ingram, Brian; Ilavsky, Jan; ...

2017-10-28

Infiltrated La 0.6Sr 0.4Co 0.2Fe 0.8O 3-δ (LSCF) sintered porous powder cathodes for solid oxide fuel cells have been investigated by synchrotron ultra-small angle x-ray scattering (USAXS). Here, we demonstrated that atomic layer deposition (ALD) is the method for a uniform coating and liquid-phase infiltration for growing nanoscale particles on the porous LSCF surfaces. The MnO infiltrate, grown by ALD, forms a conformal layer with a uniform thickness throughout the pores evidenced by USAXS thickness fringes. The La 0.6Sr 0.4CoO 3 (LSC) and La 2Zr 2O 7 (LZO) infiltrates, grown by liquid-phase infiltration, were found to form nanoscale particles onmore » the surfaces of LSCF particles resulting in increased surface areas. In conclusion, impedance measurements suggest that the catalytic property of LSC infiltrate, not the increased surface area of LZO, is important for increasing oxygen reduction activities.« less

Synchrotron X-ray studies of model SOFC cathodes, part II: Porous powder cathodes

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

Chang, Kee-Chul; Ingram, Brian; Ilavsky, Jan

Infiltrated La 0.6Sr 0.4Co 0.2Fe 0.8O 3-δ (LSCF) sintered porous powder cathodes for solid oxide fuel cells have been investigated by synchrotron ultra-small angle x-ray scattering (USAXS). Here, we demonstrated that atomic layer deposition (ALD) is the method for a uniform coating and liquid-phase infiltration for growing nanoscale particles on the porous LSCF surfaces. The MnO infiltrate, grown by ALD, forms a conformal layer with a uniform thickness throughout the pores evidenced by USAXS thickness fringes. The La 0.6Sr 0.4CoO 3 (LSC) and La 2Zr 2O 7 (LZO) infiltrates, grown by liquid-phase infiltration, were found to form nanoscale particles onmore » the surfaces of LSCF particles resulting in increased surface areas. In conclusion, impedance measurements suggest that the catalytic property of LSC infiltrate, not the increased surface area of LZO, is important for increasing oxygen reduction activities.« less

High pressure and high temperature in situ X-ray diffraction studies in the Paris-Edinburgh cell using a laboratory X-ray source†

NASA Astrophysics Data System (ADS)

Toulemonde, Pierre; Goujon, Céline; Laversenne, Laetitia; Bordet, Pierre; Bruyère, Rémy; Legendre, Murielle; Leynaud, Olivier; Prat, Alain; Mezouar, Mohamed

2014-04-01

We have developed a new laboratory experimental set-up to study in situ the pressure-temperature phase diagram of a given pure element or compound, its associated phase transitions, or the chemical reactions involved at high pressure and high temperature (HP-HT) between different solids and liquids. This new tool allows laboratory studies before conducting further detailed experiments using more brilliant synchrotron X-ray sources or before kinetic studies. This device uses the diffraction of X-rays produced by a quasi-monochromatic micro-beam source operating at the silver radiation (λ(Ag)Kα 1, 2≈0.56 Å). The experimental set-up is based on a VX Paris-Edinburgh cell equipped with tungsten carbide or sintered diamond anvils and uses standard B-epoxy 5 or 7 mm gaskets. The diffracted signal coming from the compressed (and heated) sample is collected on an image plate. The pressure and temperature calibrations were performed by diffraction, using conventional calibrants (BN, NaCl and MgO) for determination of the pressure, and by crossing isochores of BN, NaCl, Cu or Au for the determination of the temperature. The first examples of studies performed with this new laboratory set-up are presented in the article: determination of the melting point of germanium and magnesium under HP-HT, synthesis of MgB2 or C-diamond and partial study of the P, T phase diagram of MgH2.

Dilation x-ray imager a new∕faster gated x-ray imager for the NIF.

PubMed

Nagel, S R; Hilsabeck, T J; Bell, P M; Bradley, D K; Ayers, M J; Barrios, M A; Felker, B; Smith, R F; Collins, G W; Jones, O S; Kilkenny, J D; Chung, T; Piston, K; Raman, K S; Sammuli, B; Hares, J D; Dymoke-Bradshaw, A K L

2012-10-01

As the yield on implosion shots increases it is expected that the peak x-ray emission reduces to a duration with a FWHM as short as 20 ps for ∼7 × 10(18) neutron yield. However, the temporal resolution of currently used gated x-ray imagers on the NIF is 40-100 ps. We discuss the benefits of the higher temporal resolution for the NIF and present performance measurements for dilation x-ray imager, which utilizes pulse-dilation technology [T. J. Hilsabeck et al., Rev. Sci. Instrum. 81, 10E317 (2010)] to achieve x-ray imaging with temporal gate times below 10 ps. The measurements were conducted using the COMET laser, which is part of the Jupiter Laser Facility at the Lawrence Livermore National Laboratory.

Alternative designs for space x-ray telescopes

NASA Astrophysics Data System (ADS)

Hudec, R.; Pína, L.; Maršíková, Veronika; Černá, Daniela; Inneman, A.; Tichý, V.

2017-11-01

The X-ray optics is a key element of space X-ray telescopes, as well as other X-ray imaging instruments. The grazing incidence X-ray lenses represent the important class of X-ray optics. Most of grazing incidence (reflective) X-ray imaging systems used in astronomy but also in other (laboratory) applications are based on the Wolter 1 (or modified) arrangement. But there are also other designs and configurations proposed, used and considered for future applications both in space and in laboratory. The Kirkpatrick-Baez (K-B) lenses as well as various types of Lobster-Eye optics and MCP/Micropore optics serve as an example. Analogously to Wolter lenses, the X-rays are mostly reflected twice in these systems to create focal images. Various future projects in X-ray astronomy and astrophysics will require large segments with multiple thin shells or foils. The large Kirkpatrick-Baez modules, as well as the large Lobster-Eye X-ray telescope modules in Schmidt arrangement may serve as examples. All related space projects will require high quality and light segmented shells (bent or flat foils) with high X-ray reflectivity and excellent mechanical stability. The Multi Foil Optics (MFO) approach represent a promising alternative for both LE and K-B X-ray optical modules. Several types of reflecting substrates may be considered for these applications, with emphasis on thin float glass sheets and, more recently, high quality silicon wafers. This confirms the importance of non-Wolter X-ray optics designs for the future. The alternative designs require novel reflective substrates which are also discussed in the paper.

Digital enhancement of X-rays for NDT

NASA Technical Reports Server (NTRS)

Butterfield, R. L.

1980-01-01

Report is "cookbook" for digital processing of industrial X-rays. Computer techniques, previously used primarily in laboratory and developmental research, have been outlined and codified into step by step procedures for enhancing X-ray images. Those involved in nondestructive testing should find report valuable asset, particularly is visual inspection is method currently used to process X-ray images.

Systematic and Performance Tests of the Hard X-ray Polarimeter X-Calibur

NASA Astrophysics Data System (ADS)

Endsley, Ryan; Beilicke, Matthias; Kislat, Fabian; Krawczynski, Henric; X-Calibur/InFOCuS

2015-01-01

X-ray polarimetry has great potential to reveal new astrophysical information about the emission processes of high energy sources such as black hole environments, X-ray binary systems, and active galactic nuclei. Here we present the results and conclusions of systematic and performance measurements of the hard X-ray polarimeter, X-Calibur. Designed to be flown on a balloon-borne X-ray telescope, X-Calibur will achieve unprecedented sensitivity and makes use of the fact that polarized X-rays preferentially Compton-scatter perpendicular to their E-field vector. Extensive laboratory measurements taken at Washington University and the Cornell High-Energy Synchrotron Source (CHESS) indicate that X-Calibur combines a detection efficiency on the order of unity with a high modulation factor of µ ≈ 0.5 averaged over the whole detector assembly, and with values up to µ ≈ 0.7 for select subsections of the polarimeter. Additionally, we are able to suppress background flux by more than two orders of magnitude by utilizing an active shield and scintillator coincidence. Comparing laboratory data with Monte Carlo simulations of both polarized and unpolarized hard X-ray beams illustrate that we have an exceptional understanding of the detector response.

Rietveld analysis of X-ray powder diffraction patterns as a potential tool for the identification of impact-deformed carbonate rocks

NASA Astrophysics Data System (ADS)

Huson, S. A.; Foit, F. F.; Watkinson, A. J.; Pope, M. C.

2009-12-01

Previous X-ray powder diffraction (XRD) studies revealed that shock deformed carbonates and quartz have broader XRD patterns than those of unshocked samples. Entire XRD patterns, single peak profiles and Rietveld refined parameters of carbonate samples from the Sierra Madera impact crater, west Texas, unshocked equivalent samples from 95 miles north of the crater and the Mission Canyon Formation of southwest Montana and western Wyoming were used to evaluate the use of X-ray powder diffraction as a potential tool for distinguishing impact deformed rocks from unshocked and tectonically deformed rocks. At Sierra Madera dolostone and limestone samples were collected from the crater rim (lower shock intensity) and the central uplift (higher shock intensity). Unshocked equivalent dolostone samples were collected from well cores drilled outside of the impact crater. Carbonate rocks of the Mission Canyon Formation were sampled along a transect across the tectonic front of the Sevier and Laramide orogenic belts. Whereas calcite subjected to significant shock intensities at the Sierra Madera impact crater can be differentiated from tectonically deformed calcite from the Mission Canyon Formation using Rietveld refined peak profiles, weakly shocked calcite from the crater rim appears to be indistinguishable from the tectonically deformed calcite. In contrast, Rietveld analysis readily distinguishes shocked Sierra Madera dolomite from unshocked equivalent dolostone samples from outside the crater and tectonically deformed Mission Canyon Formation dolomite.

Clay pigment structure characterisation as a guide for provenance determination--a comparison between laboratory powder micro-XRD and synchrotron radiation XRD.

PubMed

Švarcová, Silvie; Bezdička, Petr; Hradil, David; Hradilová, Janka; Žižak, Ivo

2011-01-01

Application of X-ray diffraction (XRD)-based techniques in the analysis of painted artworks is not only beneficial for indisputable identification of crystal constituents in colour layers, but it can also bring insight in material crystal structure, which can be affected by their geological formation, manufacturing procedure or secondary changes. This knowledge might be helpful for art historic evaluation of an artwork as well as for its conservation. By way of example of kaolinite, we show that classification of its crystal structure order based on XRD data is useful for estimation of its provenance. We found kaolinite in the preparation layer of a Gothic wall painting in a Czech church situated near Karlovy Vary, where there are important kaolin deposits. Comparing reference kaolin materials from eight various Czech deposits, we found that these can be differentiated just according to the kaolinite crystallinity. Within this study, we compared laboratory powder X-ray micro-diffraction (micro-XRD) with synchrotron radiation X-ray diffraction analysing the same real sample. We found that both techniques led to the same results.

Myoanatomy of the velvet worm leg revealed by laboratory-based nanofocus X-ray source tomography.

PubMed

Müller, Mark; de Sena Oliveira, Ivo; Allner, Sebastian; Ferstl, Simone; Bidola, Pidassa; Mechlem, Korbinian; Fehringer, Andreas; Hehn, Lorenz; Dierolf, Martin; Achterhold, Klaus; Gleich, Bernhard; Hammel, Jörg U; Jahn, Henry; Mayer, Georg; Pfeiffer, Franz

2017-11-21

X-ray computed tomography (CT) is a powerful noninvasive technique for investigating the inner structure of objects and organisms. However, the resolution of laboratory CT systems is typically limited to the micrometer range. In this paper, we present a table-top nanoCT system in conjunction with standard processing tools that is able to routinely reach resolutions down to 100 nm without using X-ray optics. We demonstrate its potential for biological investigations by imaging a walking appendage of Euperipatoides rowelli , a representative of Onychophora-an invertebrate group pivotal for understanding animal evolution. Comparative analyses proved that the nanoCT can depict the external morphology of the limb with an image quality similar to scanning electron microscopy, while simultaneously visualizing internal muscular structures at higher resolutions than confocal laser scanning microscopy. The obtained nanoCT data revealed hitherto unknown aspects of the onychophoran limb musculature, enabling the 3D reconstruction of individual muscle fibers, which was previously impossible using any laboratory-based imaging technique.

Phased Contrast X-Ray Imaging

ScienceCinema

Miller, Erin

2018-02-07

The Pacific Northwest National Laboratory is developing a range of technologies to broaden the field of explosives detection. Phased contrast X-ray imaging, which uses silicon gratings to detect distortions in the X-ray wave front, may be applicable to mail or luggage scanning for explosives; it can also be used in detecting other contraband, small-parts inspection, or materials characterization.

One-Step Hydrothermal Synthesis of Zeolite X Powder from Natural Low-Grade Diatomite.

PubMed

Yao, Guangyuan; Lei, Jingjing; Zhang, Xiaoyu; Sun, Zhiming; Zheng, Shuilin

2018-05-28

Zeolite X powder was synthesized using natural low-grade diatomite as the main source of Si but only as a partial source of Al via a simple and green hydrothermal method. The microstructure and surface properties of the obtained samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), wavelength dispersive X-ray fluorescence (XRF), calcium ion exchange capacity (CEC), thermogravimetric-differential thermal (TG-DTA) analysis, and N₂ adsorption-desorption technique. The influence of various synthesis factors, including aging time and temperature, crystallization time and temperature, Na₂O/SiO₂ and H₂O/Na₂O ratio on the CEC of zeolite, were systematically investigated. The as-synthesized zeolite X with binary meso-microporous structure possessed remarkable thermal stability, high calcium ion exchange capacity of 248 mg/g and large surface area of 453 m²/g. In addition, the calcium ion exchange capacity of zeolite X was found to be mainly determined by the crystallization degree. In conclusion, the synthesized zeolite X using diatomite as a cost-effective raw material in this study has great potential for industrial application such as catalyst support and adsorbent.

Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids

PubMed Central

2013-01-01

We report a strategy for structure determination of organic materials in which complete solid-state nuclear magnetic resonance (NMR) spectral data is utilized within the context of structure determination from powder X-ray diffraction (XRD) data. Following determination of the crystal structure from powder XRD data, first-principles density functional theory-based techniques within the GIPAW approach are exploited to calculate the solid-state NMR data for the structure, followed by careful scrutiny of the agreement with experimental solid-state NMR data. The successful application of this approach is demonstrated by structure determination of the 1:1 cocrystal of indomethacin and nicotinamide. The 1H and 13C chemical shifts calculated for the crystal structure determined from the powder XRD data are in excellent agreement with those measured experimentally, notably including the two-dimensional correlation of 1H and 13C chemical shifts for directly bonded 13C–1H moieties. The key feature of this combined approach is that the quality of the structure determined is assessed both against experimental powder XRD data and against experimental solid-state NMR data, thus providing a very robust validation of the veracity of the structure. PMID:24386493

Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids.

PubMed

Dudenko, Dmytro V; Williams, P Andrew; Hughes, Colan E; Antzutkin, Oleg N; Velaga, Sitaram P; Brown, Steven P; Harris, Kenneth D M

2013-06-13

We report a strategy for structure determination of organic materials in which complete solid-state nuclear magnetic resonance (NMR) spectral data is utilized within the context of structure determination from powder X-ray diffraction (XRD) data. Following determination of the crystal structure from powder XRD data, first-principles density functional theory-based techniques within the GIPAW approach are exploited to calculate the solid-state NMR data for the structure, followed by careful scrutiny of the agreement with experimental solid-state NMR data. The successful application of this approach is demonstrated by structure determination of the 1:1 cocrystal of indomethacin and nicotinamide. The 1 H and 13 C chemical shifts calculated for the crystal structure determined from the powder XRD data are in excellent agreement with those measured experimentally, notably including the two-dimensional correlation of 1 H and 13 C chemical shifts for directly bonded 13 C- 1 H moieties. The key feature of this combined approach is that the quality of the structure determined is assessed both against experimental powder XRD data and against experimental solid-state NMR data, thus providing a very robust validation of the veracity of the structure.

Real-time monitoring of laser powder bed fusion process using high-speed X-ray imaging and diffraction

DOE PAGES

Zhao, Cang; Fezzaa, Kamel; Cunningham, Ross W.; ...

2017-06-15

Here, we employ the high-speed synchrotron hard X-ray imaging and diffraction techniques to monitor the laser powder bed fusion (LPBF) process of Ti-6Al-4V in situ and in real time. We demonstrate that many scientifically and technologically significant phenomena in LPBF, including melt pool dynamics, powder ejection, rapid solidification, and phase transformation, can be probed with unprecedented spatial and temporal resolutions. In particular, the keyhole pore formation is experimentally revealed with high spatial and temporal resolutions. The solidification rate is quantitatively measured, and the slowly decrease in solidification rate during the relatively steady state could be a manifestation of the recalescencemore » phenomenon. The high-speed diffraction enables a reasonable estimation of the cooling rate and phase transformation rate, and the diffusionless transformation from β to α’ phase is evident. The data present here will facilitate the understanding of dynamics and kinetics in metal LPBF process, and the experiment platform established will undoubtedly become a new paradigm for future research and development of metal additive manufacturing.« less

Real-time monitoring of laser powder bed fusion process using high-speed X-ray imaging and diffraction

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

Zhao, Cang; Fezzaa, Kamel; Cunningham, Ross W.

Here, we employ the high-speed synchrotron hard X-ray imaging and diffraction techniques to monitor the laser powder bed fusion (LPBF) process of Ti-6Al-4V in situ and in real time. We demonstrate that many scientifically and technologically significant phenomena in LPBF, including melt pool dynamics, powder ejection, rapid solidification, and phase transformation, can be probed with unprecedented spatial and temporal resolutions. In particular, the keyhole pore formation is experimentally revealed with high spatial and temporal resolutions. The solidification rate is quantitatively measured, and the slowly decrease in solidification rate during the relatively steady state could be a manifestation of the recalescencemore » phenomenon. The high-speed diffraction enables a reasonable estimation of the cooling rate and phase transformation rate, and the diffusionless transformation from β to α’ phase is evident. The data present here will facilitate the understanding of dynamics and kinetics in metal LPBF process, and the experiment platform established will undoubtedly become a new paradigm for future research and development of metal additive manufacturing.« less

Electron paramagnetic resonance, scanning electron microscopy with energy dispersion X-ray spectrometry, X-ray powder diffraction, and NMR characterization of iron-rich fired clays.

PubMed

Presciutti, Federica; Capitani, Donatella; Sgamellotti, Antonio; Brunetti, Brunetto Giovanni; Costantino, Ferdinando; Viel, Stéphane; Segre, Annalaura

2005-12-01

The aim of this study is to clarify the structure of an iron-rich clay and the structural changes involved in the firing process as a preliminary step to get information on ancient ceramic technology. To this purpose, illite-rich clay samples fired at different temperatures were characterized using a multitechnique approach, i.e., by electron paramagnetic resonance, scanning electron microscopy with electron dispersion X-ray spectrometry, X-ray powder diffraction, magic angle spinning and multiple quantum magic angle spinning NMR. During firing, four main reaction processes occur: dehydration, dehydroxylation, structural breakdown, and recrystallization. When the results are combined from all characterization methods, the following conclusions could be obtained. Interlayer H2O is located close to aluminum in octahedral sites and is driven off at temperatures lower than 600 degrees C. Between 600 and 700 degrees C dehydroxylation occurs whereas, between 800 and 900 degrees C, the aluminum in octahedral sites disappears, due to the breakdown of the illite structure, and all iron present is oxidized to Fe3+. In samples fired at 1000 and 1100 degrees C iron clustering was observed as well as large single crystals of iron with the occurrence of ferro- or ferrimagnetic effects. Below 900 degrees C the aluminum in octahedral sites presents a continuous distribution of chemical shift, suggesting the presence of slightly distorted sites. Finally, over the whole temperature range, the presence of at least two tetrahedral aluminum sites was revealed, characterized by different values of the quadrupolar coupling constant.

Single shot near edge x-ray absorption fine structure spectroscopy in the laboratory

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

Mantouvalou, I., E-mail: ioanna.mantouvalou@tu-berlin.de; Witte, K.; Martyanov, W.

With the help of adapted off-axis reflection zone plates, near edge X-ray absorption fine structure spectra at the C and N K-absorption edge have been recorded using a single 1.2 ns long soft X-ray pulse. The transmission experiments were performed with a laser-produced plasma source in the laboratory rendering time resolved measurements feasible independent on large scale facilities. A resolving power of E/ΔE ∼ 950 at the respective edges could be demonstrated. A comparison of single shot spectra with those collected with longer measuring time proves that all features of the used reference samples (silicon nitrate and polyimide) can be resolved in 1.2 ns.more » Hence, investigations of radiation sensitive biological specimen become possible due to the high efficiency of the optical elements enabling low dose experiments.« less

42 CFR 410.32 - Diagnostic x-ray tests, diagnostic laboratory tests, and other diagnostic tests: Conditions.

Code of Federal Regulations, 2013 CFR

2013-10-01

... in the 80000 series of the Current Procedural Terminology published by the American Medical... & MEDICAID SERVICES, DEPARTMENT OF HEALTH AND HUMAN SERVICES MEDICARE PROGRAM SUPPLEMENTARY MEDICAL INSURANCE (SMI) BENEFITS Medical and Other Health Services § 410.32 Diagnostic x-ray tests, diagnostic laboratory...

42 CFR 410.32 - Diagnostic x-ray tests, diagnostic laboratory tests, and other diagnostic tests: Conditions.

Code of Federal Regulations, 2011 CFR

2011-10-01

... Procedural Terminology published by the American Medical Association. (vii) Diagnostic tests performed by a... & MEDICAID SERVICES, DEPARTMENT OF HEALTH AND HUMAN SERVICES MEDICARE PROGRAM SUPPLEMENTARY MEDICAL INSURANCE (SMI) BENEFITS Medical and Other Health Services § 410.32 Diagnostic x-ray tests, diagnostic laboratory...

42 CFR 410.32 - Diagnostic x-ray tests, diagnostic laboratory tests, and other diagnostic tests: Conditions.

Code of Federal Regulations, 2012 CFR

2012-10-01

... Procedural Terminology published by the American Medical Association. (vii) Diagnostic tests performed by a... & MEDICAID SERVICES, DEPARTMENT OF HEALTH AND HUMAN SERVICES MEDICARE PROGRAM SUPPLEMENTARY MEDICAL INSURANCE (SMI) BENEFITS Medical and Other Health Services § 410.32 Diagnostic x-ray tests, diagnostic laboratory...

42 CFR 410.32 - Diagnostic x-ray tests, diagnostic laboratory tests, and other diagnostic tests: Conditions.

Code of Federal Regulations, 2010 CFR

2010-10-01

... Procedural Terminology published by the American Medical Association. (3) Levels of supervision. Except where... & MEDICAID SERVICES, DEPARTMENT OF HEALTH AND HUMAN SERVICES MEDICARE PROGRAM SUPPLEMENTARY MEDICAL INSURANCE (SMI) BENEFITS Medical and Other Health Services § 410.32 Diagnostic x-ray tests, diagnostic laboratory...

Long duration X-ray drive hydrodynamics experiments relevant for laboratory astrophysics

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

Casner, A.; Martinez, D.; Smalyuk, V.

The advent of high-power lasers facilities such as the National Ignition Facility (NIF), and the Laser Megajoule (LMJ) in the near future, opens a new era in the field of High Energy Density Laboratory Astrophysics. These versatile laser facilities will provide unique platforms to study the rich physics of nonlinear and turbulent mixing flows. The extended laser pulse duration could be harnessed to accelerate targets over much larger distances and longer time periods than previously achieved. Here, we report on the first results acquired on NIF with the ablative Rayleigh–Taylor Instability (RTI) platform. A 20-ns X-ray drive is tailored tomore » accelerate planar modulated samples into the highly-nonlinear bubble merger regime. Based on the analogy between flames front and ablation front, highly nonlinear RTI measurements at ablation front can provide important insights into the initial deflagration stage of thermonuclear supernova of Type Ia. We also report on an innovative concept used to create even longer drive on multi-beam laser facilities. The multi-barrel hohlraum (Gattling Gun) approach consists, here, of three adjacent cavities, driven in succession in time. This novel concept has been validated on the Omega EP laser system. The three cavities were irradiated with three 6–10 ns pulse UV beams and a 30 ns, 90 eV X-ray radiation drive was measured with the time-resolved X-ray spectrometer μDMX. This concept is promising to investigate the pillar structures in the Eagle Nebula or for photoionization studies which require a steady light source of sufficient duration to recreate relevant physics.« less

Long duration X-ray drive hydrodynamics experiments relevant for laboratory astrophysics

DOE PAGES

Casner, A.; Martinez, D.; Smalyuk, V.; ...

2014-09-20

The advent of high-power lasers facilities such as the National Ignition Facility (NIF), and the Laser Megajoule (LMJ) in the near future, opens a new era in the field of High Energy Density Laboratory Astrophysics. These versatile laser facilities will provide unique platforms to study the rich physics of nonlinear and turbulent mixing flows. The extended laser pulse duration could be harnessed to accelerate targets over much larger distances and longer time periods than previously achieved. Here, we report on the first results acquired on NIF with the ablative Rayleigh–Taylor Instability (RTI) platform. A 20-ns X-ray drive is tailored tomore » accelerate planar modulated samples into the highly-nonlinear bubble merger regime. Based on the analogy between flames front and ablation front, highly nonlinear RTI measurements at ablation front can provide important insights into the initial deflagration stage of thermonuclear supernova of Type Ia. We also report on an innovative concept used to create even longer drive on multi-beam laser facilities. The multi-barrel hohlraum (Gattling Gun) approach consists, here, of three adjacent cavities, driven in succession in time. This novel concept has been validated on the Omega EP laser system. The three cavities were irradiated with three 6–10 ns pulse UV beams and a 30 ns, 90 eV X-ray radiation drive was measured with the time-resolved X-ray spectrometer μDMX. This concept is promising to investigate the pillar structures in the Eagle Nebula or for photoionization studies which require a steady light source of sufficient duration to recreate relevant physics.« less

Performance Characteristics of Waste Glass Powder Substituting Portland Cement in Mortar Mixtures

NASA Astrophysics Data System (ADS)

Kara, P.; Csetényi, L. J.; Borosnyói, A.

2016-04-01

In the present work, soda-lime glass cullet (flint, amber, green) and special glass cullet (soda-alkaline earth-silicate glass coming from low pressure mercury-discharge lamp cullet and incandescent light bulb borosilicate glass waste cullet) were ground into fine powders in a laboratory planetary ball mill for 30 minutes. CEM I 42.5N Portland cement was applied in mortar mixtures, substituted with waste glass powder at levels of 20% and 30%. Characterisation and testing of waste glass powders included fineness by laser diffraction particle size analysis, specific surface area by nitrogen adsorption technique, particle density by pycnometry and chemical analysis by X-ray fluorescence spectrophotometry. Compressive strength, early age shrinkage cracking and drying shrinkage tests, heat of hydration of mortars, temperature of hydration, X-ray diffraction analysis and volume stability tests were performed to observe the influence of waste glass powder substitution for Portland cement on physical and engineering properties of mortar mixtures.

Generation of High Brightness X-rays with the PLEIADES Thomson X-ray Source

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

Brown, W J; Anderson, S G; Barty, C P J

2003-05-28

The use of short laser pulses to generate high peak intensity, ultra-short x-ray pulses enables exciting new experimental capabilities, such as femtosecond pump-probe experiments used to temporally resolve material structural dynamics on atomic time scales. PLEIADES (Picosecond Laser Electron InterAction for Dynamic Evaluation of Structures) is a next generation Thomson scattering x-ray source being developed at Lawrence Livermore National Laboratory (LLNL). Ultra-fast picosecond x-rays (10-200 keV) are generated by colliding an energetic electron beam (20-100 MeV) with a high intensity, sub-ps, 800 nm laser pulse. The peak brightness of the source is expected to exceed 10{sup 20} photons/s/0.1% bandwidth/mm2/mrad2. Simulationsmore » of the electron beam production, transport, and final focus are presented. Electron beam measurements, including emittance and final focus spot size are also presented and compared to simulation results. Measurements of x-ray production are also reported and compared to theoretical calculations.« less

Characterization of monoclinic crystals in tablets by pattern-fitting procedure using X-ray powder diffraction data.

PubMed

Yamamura, Shigeo; Momose, Yasunori

2003-06-18

The purpose of this study is to characterize the monoclinic crystals in tablets by using X-ray powder diffraction data and to evaluate the deformation feature of crystals during compression. The monoclinic crystals of acetaminophen and benzoic acid were used as the samples. The observed X-ray diffraction intensities were fitted to the analytic expression, and the fitting parameters, such as the lattice parameters, the peak-width parameters, the preferred orientation parameter and peak asymmetric parameter were optimized by a non-linear least-squares procedure. The Gauss and March distribution functions were used to correct the preferred orientation of crystallites in the tablet. The March function performed better in correcting the modification of diffraction intensity by preferred orientation of crystallites, suggesting that the crystallites in the tablets had fiber texture with axial orientation. Although a broadening of diffraction peaks was observed in acetaminophen tablets with an increase of compression pressure, little broadening was observed in the benzoic tablets. These results suggest that "acetaminophen is a material consolidating by fragmentation of crystalline particles and benzoic acid is a material consolidating by plastic deformation then occurred rearrangement of molecules during compression". A pattern-fitting procedure is the superior method for characterizing the crystalline drugs of monoclinic crystals in the tablets, as well as orthorhombic isoniazid and mannitol crystals reported in the previous paper.

X-Ray Structure determination of the Glycine Cleavage System Protein H of Mycobacterium tuberculosis Using An Inverse Compton Synchrotron X-Ray Source

PubMed Central

Abendroth, Jan; McCormick, Michael S.; Edwards, Thomas E.; Staker, Bart; Loewen, Roderick; Gifford, Martin; Rifkin, Jeff; Mayer, Chad; Guo, Wenjin; Zhang, Yang; Myler, Peter; Kelley, Angela; Analau, Erwin; Hewitt, Stephen Nakazawa; Napuli, Alberto J.; Kuhn, Peter; Ruth, Ronald D.; Stewart, Lance J.

2010-01-01

Structural genomics discovery projects require ready access to both X-ray and NMR instrumentation which support the collection of experimental data needed to solve large numbers of novel protein structures. The most productive X-ray crystal structure determination laboratories make extensive frequent use of tunable synchrotron X-ray light to solve novel structures by anomalous diffraction methods. This requires that frozen cryo-protected crystals be shipped to large government-run synchrotron facilities for data collection. In an effort to eliminate the need to ship crystals for data collection, we have developed the first laboratory-scale synchrotron light source capable of performing many of the state-of-the-art synchrotron applications in X-ray science. This Compact Light Source is a first-in-class device that uses inverse Compton scattering to generate X-rays of sufficient flux, tunable wavelength and beam size to allow high-resolution X-ray diffraction data collection from protein crystals. We report on benchmarking tests of X-ray diffraction data collection with hen egg white lysozyme, and the successful high-resolution X-ray structure determination of the Glycine cleavage system protein H from Mycobacterium tuberculosis using diffraction data collected with the Compact Light Source X-ray beam. PMID:20364333

Thermal expansion of coesite determined by synchrotron powder X-ray diffraction

NASA Astrophysics Data System (ADS)

Kulik, Eleonora; Murzin, Vadim; Kawaguchi, Shogo; Nishiyama, Norimasa; Katsura, Tomoo

2018-05-01

Thermal expansion of synthetic coesite was studied with synchrotron powder X-ray diffraction in the temperature range of 100-1000 K. We determined the unit cell parameters of monoclinic coesite (a, b, c, and β) every 50 K in this temperature range. We observed that a and b parameters increase with increasing temperature, while c decreases. The β angle also decreases with temperature and approaches 120°. As a result, the unit cell volume expands by only 0.7% in this temperature range. Our measurements provide thermal expansion coefficients of coesite as a function of temperature: it increases from 3.4 × 10-6 K-1 at 100 K to 9.3 × 10-6 K-1 at 600 K and remains nearly constant above this temperature. The Suzuki model based on the zero-pressure Mie-Grüneisen equation of state was implemented to fit the unit cell volume data. The refined parameters are {V_0} = 546.30(2) Å3, Q = 7.20(12) × 106 J/mol and {θ D} = 1018(43) K, where {θ D} is the Debye temperature and {V_0} is the unit cell volume at 0 K with an assumption that {K^' } is equal to 1.8. The obtained Debye temperature is consistent with that determined in a previous study for heat capacity measurements.

X-ray diffraction studies of shocked lunar analogs

NASA Technical Reports Server (NTRS)

Hanss, R. E.

1979-01-01

The X-ray diffraction experiments on shocked rock and mineral analogs of particular significance to lunar geology are described. Materials naturally shocked by meteorite impact, nuclear-shocked, or artificially shocked in a flat plate accelerator were utilized. Four areas were outlined for investigation: powder diffractometer studies of shocked single crystal silicate minerals (quartz, orthoclase, oligoclase, pyroxene), powder diffractometer studies of shocked polycrystalline monomineralic samples (dunite), Debye-Scherrer studies of single grains of shocked granodiorite, and powder diffractometer studies of shocked whole rock samples. Quantitative interpretation of peak shock pressures experienced by materials found in lunar or terrestrial impact structures is presented.

Motion control system of MAX IV Laboratory soft x-ray beamlines

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

Sjöblom, Peter, E-mail: peter.sjoblom@maxlab.lu.se; Lindberg, Mirjam, E-mail: mirjam.lindberg@maxlab.lu.se; Forsberg, Johan, E-mail: johan.forsberg@maxlab.lu.se

2016-07-27

At the MAX IV Laboratory, five new soft x-ray beamlines are under development. The first is Species and it will be used to develop and set the standard of the control system, which will be common across the facility. All motion axes at MAX IV will be motorized using stepper motors steered by the IcePAP motion controller and a mixture of absolute and incremental encoders following a predefined coordinate system. The control system software is built in Tango and uses the Python-based Sardana framework. The user controls the entire beamline through a synoptic overview and Sardana is used to runmore » the scans.« less

X-ray diffraction results from Mars Science Laboratory: mineralogy of Rocknest at Gale crater.

PubMed

Bish, D L; Blake, D F; Vaniman, D T; Chipera, S J; Morris, R V; Ming, D W; Treiman, A H; Sarrazin, P; Morrison, S M; Downs, R T; Achilles, C N; Yen, A S; Bristow, T F; Crisp, J A; Morookian, J M; Farmer, J D; Rampe, E B; Stolper, E M; Spanovich, N

2013-09-27

The Mars Science Laboratory rover Curiosity scooped samples of soil from the Rocknest aeolian bedform in Gale crater. Analysis of the soil with the Chemistry and Mineralogy (CheMin) x-ray diffraction (XRD) instrument revealed plagioclase (~An57), forsteritic olivine (~Fo62), augite, and pigeonite, with minor K-feldspar, magnetite, quartz, anhydrite, hematite, and ilmenite. The minor phases are present at, or near, detection limits. The soil also contains 27 ± 14 weight percent x-ray amorphous material, likely containing multiple Fe(3+)- and volatile-bearing phases, including possibly a substance resembling hisingerite. The crystalline component is similar to the normative mineralogy of certain basaltic rocks from Gusev crater on Mars and of martian basaltic meteorites. The amorphous component is similar to that found on Earth in places such as soils on the Mauna Kea volcano, Hawaii.

Detection Limit of Smectite by Chemin IV Laboratory Instrument: Preliminary Implications for Chemin on the Mars Science Laboratory Mission

NASA Technical Reports Server (NTRS)

Archilles, Cherie; Ming, D. W.; Morris, R. V.; Blake, D. F.

2011-01-01

The CheMin instrument on the Mars Science Laboratory (MSL) is an miniature X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of detecting the mineralogical and elemental compositions of rocks, outcrops and soils on the surface of Mars. CheMin uses a microfocus-source Co X-ray tube, a transmission sample cell, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. CRISM and OMEGA have identified the presence of phyllosilicates at several locations on Mars including the four candidate MSL landing sites. The objective of this study was to conduct preliminary studies to determine the CheMin detection limit of smectite in a smectite/olivine mixed mineral system.

Structural properties of a family of hydrogen-bonded co-crystals formed between gemfibrozil and hydroxy derivatives of t-butylamine, determined directly from powder X-ray diffraction data

NASA Astrophysics Data System (ADS)

Cheung, Eugene Y.; David, Sarah E.; Harris, Kenneth D. M.; Conway, Barbara R.; Timmins, Peter

2007-03-01

We report the formation and structural properties of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine H 2NC(CH 3) 3-n(CH 2OH) n, with n=0, 1, 2 and 3. In each case, a 1:1 co-crystal is formed, with transfer of a proton from the carboxylic acid group of gemfibrozil to the amino group of the t-butylamine derivative. All of the co-crystal materials prepared are polycrystalline powders, and do not contain single crystals of suitable size and/or quality for single crystal X-ray diffraction studies. Structure determination of these materials has been carried out directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm technique for structure solution followed by Rietveld refinement. The structural chemistry of this series of co-crystal materials reveals well-defined structural trends within the first three members of the family ( n=0, 1, 2), but significantly contrasting structural properties for the member with n=3.

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

DOE PAGES

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit; ...

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials and in situ and operando diffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, overmore » a continuous range of diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. In addition, the design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

Fabrication and testing of a newly designed slit system for depth-resolved X-ray diffraction measurements

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

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit

2016-10-06

A new system of slits called `spiderweb slits' have been developed for depth-resolved powder or polycrystalline X-ray diffraction measurements. The slits act on diffracted X-rays to select a particular gauge volume of sample, while absorbing diffracted X-rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials andin situandoperandodiffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, over a continuous range ofmore » diffraction angles, and work for X-ray energies of tens to hundreds of kiloelectronvolts. The design is generated and optimized using ray-tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X-ray Powder Diffraction beamline at the National Synchrotron Light Source II.« less

A laboratory 8 keV transmission full-field x-ray microscope with a polycapillary as condenser for bright and dark field imaging.

PubMed

Baumbach, S; Kanngießer, B; Malzer, W; Stiel, H; Wilhein, T

2015-08-01

This article introduces a laboratory setup of a transmission full-field x-ray microscope at 8 keV photon energy. The microscope operates in bright and dark field imaging mode with a maximum field of view of 50 μm. Since the illumination geometry determines whether the sample is illuminated homogeneously and moreover, if different imaging methods can be applied, the condenser optic is one of the most significant parts. With a new type of x-ray condenser, a polycapillary optic, we realized bright field imaging and for the first time dark field imaging at 8 keV photon energy in a laboratory setup. A detector limited spatial resolution of 210 nm is measured on x-ray images of Siemens star test patterns.

Non Destructive 3D X-Ray Imaging of Nano Structures & Composites at Sub-30 NM Resolution, With a Novel Lab Based X-Ray Microscope

DTIC Science & Technology

2006-11-01

NON DESTRUCTIVE 3D X-RAY IMAGING OF NANO STRUCTURES & COMPOSITES AT SUB-30 NM RESOLUTION, WITH A NOVEL LAB BASED X- RAY MICROSCOPE S H Lau...article we describe a 3D x-ray microscope based on a laboratory x-ray source operating at 2.7, 5.4 or 8.0 keV hard x-ray energies. X-ray computed...tomography (XCT) is used to obtain detailed 3D structural information inside optically opaque materials with sub-30 nm resolution. Applications include

X-ray Diffraction from Membrane Protein Nanocrystals

PubMed Central

Hunter, M.S.; DePonte, D.P.; Shapiro, D.A.; Kirian, R.A.; Wang, X.; Starodub, D.; Marchesini, S.; Weierstall, U.; Doak, R.B.; Spence, J.C.H.; Fromme, P.

2011-01-01

Membrane proteins constitute >30% of the proteins in an average cell, and yet the number of currently known structures of unique membrane proteins is <300. To develop new concepts for membrane protein structure determination, we have explored the serial nanocrystallography method, in which fully hydrated protein nanocrystals are delivered to an x-ray beam within a liquid jet at room temperature. As a model system, we have collected x-ray powder diffraction data from the integral membrane protein Photosystem I, which consists of 36 subunits and 381 cofactors. Data were collected from crystals ranging in size from 100 nm to 2 μm. The results demonstrate that there are membrane protein crystals that contain <100 unit cells (200 total molecules) and that 3D crystals of membrane proteins, which contain <200 molecules, may be suitable for structural investigation. Serial nanocrystallography overcomes the problem of x-ray damage, which is currently one of the major limitations for x-ray structure determination of small crystals. By combining serial nanocrystallography with x-ray free-electron laser sources in the future, it may be possible to produce molecular-resolution electron-density maps using membrane protein crystals that contain only a few hundred or thousand unit cells. PMID:21190672

Characterization of Metal Powders Used for Additive Manufacturing.

PubMed

Slotwinski, J A; Garboczi, E J; Stutzman, P E; Ferraris, C F; Watson, S S; Peltz, M A

2014-01-01

Additive manufacturing (AM) techniques can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process.

Characterization of Metal Powders Used for Additive Manufacturing

PubMed Central

Slotwinski, JA; Garboczi, EJ; Stutzman, PE; Ferraris, CF; Watson, SS; Peltz, MA

2014-01-01

Additive manufacturing (AM) techniques1 can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process. PMID:26601040

Capillary Optics Based X-Ray Micro-Imaging Elemental Analysis

NASA Astrophysics Data System (ADS)

Hampai, D.; Dabagov, S. B.; Cappuccio, G.; Longoni, A.; Frizzi, T.; Cibin, G.

2010-04-01

A rapidly developed during the last few years micro-X-ray fluorescence spectrometry (μXRF) is a promising multi-elemental technique for non-destructive analysis. Typically it is rather hard to perform laboratory μXRF analysis because of the difficulty of producing an original small-size X-ray beam as well as its focusing. Recently developed for X-ray beam focusing polycapillary optics offers laboratory X-ray micro probes. The combination of polycapillary lens and fine-focused micro X-ray tube can provide high intensity radiation flux on a sample that is necessary in order to perform the elemental analysis. In comparison to a pinhole, an optimized "X-ray source-op tics" system can result in radiation density gain of more than 3 orders by the value. The most advanced way to get that result is to use the confocal configuration based on two X-ray lenses, one for the fluorescence excitation and the other for the detection of secondary emission from a sample studied. In case of X-ray capillary microfocusing a μXRF instrument designed in the confocal scheme allows us to obtain a 3D elemental mapping. In this work we will show preliminary results obtained with our prototype, a portable X-ray microscope for X-ray both imaging and fluorescence analysis; it enables μXRF elemental mapping simultaneously with X-ray imaging. A prototype of compact XRF spectrometer with a spatial resolution less than 100 μm has been designed.

A final report to the Laboratory Directed Research and Development committee on Project 93-ERP-075: ``X-ray laser propagation and coherence: Diagnosing fast-evolving, high-density laser plasmas using X-ray lasers``

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

Wan, A.S.; Cauble, R.; Da Silva, L.B.

1996-02-01

This report summarizes the major accomplishments of this three-year Laboratory Directed Research and Development (LDRD) Exploratory Research Project (ERP) entitled ``X-ray Laser Propagation and Coherence: Diagnosing Fast-evolving, High-density Laser Plasmas Using X-ray Lasers,`` tracking code 93-ERP-075. The most significant accomplishment of this project is the demonstration of a new laser plasma diagnostic: a soft x-ray Mach-Zehnder interferometer using a neonlike yttrium x-ray laser at 155 {angstrom} as the probe source. Detailed comparisons of absolute two-dimensional electron density profiles obtained from soft x-ray laser interferograms and profiles obtained from radiation hydrodynamics codes, such as LASNEX, will allow us to validate andmore » benchmark complex numerical models used to study the physics of laser-plasma interactions. Thus the development of soft x-ray interferometry technique provides a mechanism to probe the deficiencies of the numerical models and is an important tool for, the high-energy density physics and science-based stockpile stewardship programs. The authors have used the soft x-ray interferometer to study a number of high-density, fast evolving, laser-produced plasmas, such as the dynamics of exploding foils and colliding plasmas. They are pursuing the application of the soft x-ray interferometer to study ICF-relevant plasmas, such as capsules and hohlraums, on the Nova 10-beam facility. They have also studied the development of enhanced-coherence, shorter-pulse-duration, and high-brightness x-ray lasers. The utilization of improved x-ray laser sources can ultimately enable them to obtain three-dimensional holographic images of laser-produced plasmas.« less

Kinetic and radiation-hydrodynamic modeling of x-ray heating in laboratory photoionized plasmas

NASA Astrophysics Data System (ADS)

Mancini, Roberto

2017-06-01

In experiments performed at the Z facility of Sandia National Laboratories a cm-scale cell filled with neon gas was driven by the burst of broadband x-rays emitted at the collapse of a wire-array z-pinch turning the gas into a photoionized plasma. Transmission spectroscopy of a narrowband portion of the x-ray flux was used to diagnose the plasma. The data show a highly-ionized neon plasma with a rich line absorption spectrum that permits the extraction of the ionization distribution among Be-, Li-, He- and H-like ions. Analysis of the spectra produced atomic ground and low excited state areal densities in these ions, and from the ratio of first-excited to ground state populations in Li-like neon a temperature of 19±4eV was extracted to characterize the x-ray heating of the plasma. To interpret this observation, we have performed data-constrained view-factor calculations of the spectral distribution of the x-ray drive, self-consistent modeling of electron and atomic kinetics, and radiation-hydrodynamic simulations. For the conditions of the experiment, the electron distribution thermalizes quickly, has a negligible high-energy tail, and is very well approximated by a single Maxwellian distribution. Radiation-hydrodynamic simulations with either LTE or NLTE (i.e. non-equilibrium) atomic physics provide a more complete modeling of the experiment. We found that in order to compute electron temperatures consistent with observation inline non-equilibrium collisional-radiative neon atomic kinetics needs to be taken into account. We discuss the details of LTE and NLTE simulations, and the impact of atomic physics on the radiation heating and cooling rates that determine the plasma temperature. This work was sponsored in part by DOE Office of Science Grant DE-SC0014451, and the Z Facility Fundamental Science Program of SNL.

The soft x-ray beamline at Frascati Labs

NASA Astrophysics Data System (ADS)

Cinque, Gianfelice; Burattini, Emilio; Grilli, Antonio; Dabagov, Sultan

2005-08-01

DAΦNE-Light is the Synchrotron Radiation laboratory at the Laboratori Nazionali di Frascati (LNF)1. Three beamlines were commissioned since spring 2003 to exploit parasitically the intense photon emission from DAΦNE, the 0.5 1 GeV storage ring routinely circulating over 1 A of electrons. The soft X-ray beamline utilizes a wiggler source and, by a double-crystal fixed-exit monochromator, it is operational in the distinguishing energy window 1.5 - 4 keV range to be extended from the "water window" toward 6 keV. At present, the research activity is focused on X-ray Absorption Spectroscopy (XAS): precisely, X-ray Absorption Near Edge Spectroscopy (XANES) on the inner electronic levels of light elements and transition metals from Al to Ge and both d- and f-shells of higher Z atoms. Preliminary tests of X-ray imaging have been performed in view of applying different focusing optics, namely policapillary systems in trasmission and/or bent mica diffractor in back-reflection, for X-ray microscopy and spectromicroscopy experiments. The use of polycapillary systems (lenses, halflenses, capillaries) for studying features of radiation transportation by such structures (X-ray channelling, focusing, bending, etc.) has been planned.

Picosecond x-ray diagnostics for third and fourth generation synchrotron sources

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

DeCamp, Matthew

2016-03-30

In the DOE-EPSCoR State/National Laboratory partnership grant ``Picosecond x-ray diagnostics for third and fourth generation synchrotron sources'' Dr. DeCamp set forth a partnership between the University of Delaware and Argonne National Laboratory. This proposal aimed to design and implement a series of experiments utilizing, or improving upon, existing time-domain hard x-ray spectroscopies at a third generation synchrotron source. Specifically, the PI put forth three experimental projects to be explored in the grant cycle: 1) implementing a picosecond ``x-ray Bragg switch'' using a laser excited nano-structured metallic film, 2) designing a robust x-ray optical delay stage for x-ray pump-probe studies atmore » a hard x-ray synchrotron source, and 3) building/installing a laser based x-ray source at the Advanced Photon Source for two-color x-ray pump-probe studies.« less

X ray imaging microscope for cancer research

NASA Technical Reports Server (NTRS)

Hoover, Richard B.; Shealy, David L.; Brinkley, B. R.; Baker, Phillip C.; Barbee, Troy W., Jr.; Walker, Arthur B. C., Jr.

1991-01-01

The NASA technology employed during the Stanford MSFC LLNL Rocket X Ray Spectroheliograph flight established that doubly reflecting, normal incidence multilayer optics can be designed, fabricated, and used for high resolution x ray imaging of the Sun. Technology developed as part of the MSFC X Ray Microscope program, showed that high quality, high resolution multilayer x ray imaging microscopes are feasible. Using technology developed at Stanford University and at the DOE Lawrence Livermore National Laboratory (LLNL), Troy W. Barbee, Jr. has fabricated multilayer coatings with near theoretical reflectivities and perfect bandpass matching for a new rocket borne solar observatory, the Multi-Spectral Solar Telescope Array (MSSTA). Advanced Flow Polishing has provided multilayer mirror substrates with sub-angstrom (rms) smoothnesss for the astronomical x ray telescopes and x ray microscopes. The combination of these important technological advancements has paved the way for the development of a Water Window Imaging X Ray Microscope for cancer research.

Second metrology round-robin of APS, ESRF and SPring-8 laboratories of elliptical and spherical hard-x-ray mirrors.

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

Rommeveaux, A.; Assoufid, L.; Ohashi, H.

2007-01-01

The first series of metrology round-robin measurements carried out in 2005 at the APS, ESRF and SPring-8 metrology laboratories involving two flat x-ray mirrors and a cylindrical x-ray mirror has shown excellent agreement among the three facilities Long Trace Profilers (LTP) despite their architectural differences. Because of the growing interest in diffraction-limited hard x-ray K-B focusing mirrors, it was decided to extend the round robin measurements to spherical and aspheric x-ray mirrors. The strong surface slope variation of these mirrors presents a real challenge to LTP. As a result, new LTP measurement protocol has to be developed and implemented tomore » ensure measurement accuracy and consistency. In this paper, different measurement techniques and procedures will be described, the results will be discussed, and comparison will be extended to micro-stitching interferometry measurements performed at Osaka University, Japan.« less

Accretion and Outflows in X-ray Binaries: What's Really Going on During X-ray Quiescence

NASA Astrophysics Data System (ADS)

MacDonald, Rachel K. D.; Bailyn, Charles D.; Buxton, Michelle

2015-01-01

X-ray binaries, consisting of a star and a stellar-mass black hole, are wonderful laboratories for studying accretion and outflows. They evolve on timescales quite accessible to us, unlike their supermassive cousins, and allow the possibility of gaining a deeper understanding of these two common astrophysical processes. Different wavelength regimes reveal different aspects of the systems: radio emission is largely generated by outflows and jets, X-ray emission by inner accretion flows, and optical/infrared (OIR) emission by the outer disk and companion star. The search for relationships between these different wavelengths is thus an area of active research, aiming to reveal deeper connections between accretion and outflows.Initial evidence for a strong, tight correlation between radio and X-ray emission has weakened as further observations and newly-discovered sources have been obtained. This has led to discussions of multiple tracks or clusters, or the possibility that no overall relation exists for the currently-known population of X-ray binaries. Our ability to distinguish among these options is hampered by a relative lack of observations at lower luminosities, and especially of truly X-ray quiescent (non-outbursting) systems. Although X-ray binaries spend the bulk of their existence in quiescence, few quiescent sources have been observed and multiple observations of individual sources are largely nonexistent. Here we discuss new observations of the lowest-luminosity quiescent X-ray binary, A0620-00, and the place this object occupies in investigations of the radio/X-ray plane. For the first time, we also incorporate simultaneous OIR data with the radio and X-ray data.In December 2013 we took simultaneous observations of A0620-00 in the X-ray (Chandra), the radio (EVLA), and the OIR (SMARTS 1.3m). These X-ray and radio data allowed us to investigate similarities among quiescent X-ray binaries, and changes over time for this individual object, in the radio/X-ray

Capillary Discharge Soft X-ray Laser Experiments at Air Force Research Laboratory

NASA Astrophysics Data System (ADS)

Ruden, E. L.; Gale, D. G.

1997-11-01

The Air Force Research Laboratory (previously Phillips Laboratory) is presently attempting to reproduce the high gain laser results of J.J. Rocca's capillary discharge z-pinch pumped 46.9 nm Ne-like Ar laser. This poster presents progress to date at measuring our laser's intensity and gain. The capillary circuit consists of a low inductance 3 nH water capacitor discharged by a coaxial spark gap into a 12 cm long, 4 mm ID plastic capillary. The capillary is supplied with 39 kA of current with a 20 ns risetime. The principle radiation diagnostic consists of a VUV monochrometer coupled to a custom high speed vacuum X-ray diode with an aluminum cathode. The signal is recorded on a fast transient digitizer (Tektronix SCD 5000). The total detector system's analog bandwidth is about 3 GHz.

History of Chandra X-Ray Observatory

NASA Image and Video Library

1997-04-15

This photograph captures the installation of the Chandra X-Ray Observatory, formerly Advanced X-Ray Astrophysics Facility (AXAF), Advanced Charged-Coupled Device (CCD) Imaging Spectrometer (ACIS) into the Vacuum Chamber at the X-Ray Calibration Facility (XRCF) at Marshall Space Flight Center (MSFC). The AXAF was renamed Chandra X-Ray Observatory (CXO) in 1999. The CXO is the most sophisticated and the world's most powerful x-ray telescope ever built. It observes x-rays from high-energy regions of the universe, such as hot gas in the remnants of exploded stars. The ACIS is one of two focal plane instruments. As the name suggests, this instrument is an array of CCDs similar to those used in a camcorder. This instrument will be especially useful because it can make x-ray images and measure the energies of incoming x-rays. It is the instrument of choice for studying the temperature variation across x-ray sources, such as vast clouds of hot-gas intergalactic space. MSFC's XRCF is the world's largest, most advanced laboratory for simulating x-ray emissions from distant celestial objects. It produces a space-like environment in which components related to x-ray telescope imaging are tested and the quality of their performances in space is predicted. TRW, Inc. was the prime contractor for the development of the CXO and NASA's MSFC was responsible for its project management. The Smithsonian Astrophysical Observatory controls science and flight operations of the CXO for NASA from Cambridge, Massachusetts. The CXO was launched July 22, 1999 aboard the Space Shuttle Columbia (STS-93).

A laboratory 8 keV transmission full-field x-ray microscope with a polycapillary as condenser for bright and dark field imaging

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

Baumbach, S., E-mail: baumbach@rheinahrcampus.de; Wilhein, T.; Kanngießer, B.

2015-08-15

This article introduces a laboratory setup of a transmission full-field x-ray microscope at 8 keV photon energy. The microscope operates in bright and dark field imaging mode with a maximum field of view of 50 μm. Since the illumination geometry determines whether the sample is illuminated homogeneously and moreover, if different imaging methods can be applied, the condenser optic is one of the most significant parts. With a new type of x-ray condenser, a polycapillary optic, we realized bright field imaging and for the first time dark field imaging at 8 keV photon energy in a laboratory setup. A detectormore » limited spatial resolution of 210 nm is measured on x-ray images of Siemens star test patterns.« less

Kinetics of methane hydrate decomposition studied via in situ low temperature X-ray powder diffraction.

PubMed

Everett, S Michelle; Rawn, Claudia J; Keffer, David J; Mull, Derek L; Payzant, E Andrew; Phelps, Tommy J

2013-05-02

Gas hydrate is known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Based on results from the decomposition of three nominally similar methane hydrate samples, the kinetics of two regions, 180-200 and 230-260 K, within the overall decomposition range 140-260 K, were studied by in situ low temperature X-ray powder diffraction. The kinetic rate constants, k(a), and the reaction mechanisms, n, for ice formation from methane hydrate were determined by the Avrami model within each region, and activation energies, E(a), were determined by the Arrhenius plot. E(a) determined from the data for 180-200 K was 42 kJ/mol and for 230-260 K was 22 kJ/mol. The higher E(a) in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.

Kinetics of Methane Hydrate Decomposition Studied via in Situ Low Temperature X-ray Powder Diffraction

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

Everett, Susan M; Rawn, Claudia J; Keffer, David J.

Gas hydrates are known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice termed self-preservation or anomalous preservation. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Two regions of slowed decomposition for methane hydrate, 180 200 K and 230 260 K, were observed, and the kinetics were studied by in situ low temperature x-ray powder diffraction. The kinetic constants for ice formation from methane hydrate were determined by the Avrami model within each region and activation energies, Ea, were determined by the Arrhenius plot.more » Ea determined from the data for 180 200 K was 42 kJ/mol and for 230 260 K was 22 kJ/mol. The higher Ea in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.« less

Monitoring X-Ray Emission from X-Ray Bursters

NASA Technical Reports Server (NTRS)

Halpern, Jules P.; Kaaret, Philip

1999-01-01

The scientific goal of this project was to monitor a selected sample of x-ray bursters using data from the All-Sky Monitor (ASM) on the Rossi X-Ray Timing Explorer together with data from the Burst and Transient Source Experiment (BATSE) on the Compton Gamma-Ray Observatory to study the long-term temporal evolution of these sources in the x-ray and hard x-ray bands. The project was closely related to "Long-Term Hard X-Ray Monitoring of X-Ray Bursters", NASA project NAG5-3891, and and "Hard x-ray emission of x-ray bursters", NASA project NAG5-4633, and shares publications in common with both of these. The project involved preparation of software for use in monitoring and then the actual monitoring itself. These efforts have lead to results directly from the ASM data and also from Target of Opportunity Observations (TOO) made with the Rossi X-Ray Timing Explorer based on detection of transient hard x-ray outbursts with the ASM and BATSE.

New trends in space x-ray optics

NASA Astrophysics Data System (ADS)

Hudec, R.; Maršíková, V.; Pína, L.; Inneman, A.; Skulinová, M.

2017-11-01

The X-ray optics is a key element of various X-ray telescopes, X-ray microscopes, as well as other X-ray imaging instruments. The grazing incidence X-ray lenses represent the important class of X-ray optics. Most of grazing incidence (reflective) X-ray imaging systems used in astronomy but also in other (laboratory) applications are based on the Wolter 1 (or modified) arrangement. But there are also other designs and configurations proposed, used and considered for future applications both in space and in laboratory. The Kirkpatrick-Baez (K-B) lenses as well as various types of Lobster-Eye optics and MCP/Micropore optics serve as an example. Analogously to Wolter lenses, the X-rays are mostly reflected twice in these systems to create focal images. Various future projects in X-ray astronomy and astrophysics will require large segments with multiple thin shells or foils. The large Kirkpatrick-Baez modules, as well as the large Lobster-Eye X-ray telescope modules in Schmidt arrangement may serve as examples. All these space projects will require high quality and light segmented shells (bent or flat foils) with high X-ray reflectivity and excellent mechanical stability. The Multi Foil Optics (MFO) approach represent a promising alternative for both LE and K-B X-ray optical modules. Several types of reflecting substrates may be considered for these applications, with emphasis on thin float glass sheets and, more recently, high quality silicon wafers. This confirms the importance of non- Wolter X-ray optics designs for the future. Future large space X-ray telescopes (such as IXO) require precise and light-weight X-ray optics based on numerous thin reflecting shells. Novel approaches and advanced technologies are to be exploited and developed. In this contribution, we refer on results of tested X-ray mirror shells produced by glass thermal forming (GTF) and by shaping Si wafers. Both glass foils and Si wafers are commercially available, have excellent surface

X-ray irradiation of yeast cells

NASA Astrophysics Data System (ADS)

Masini, Alessandra; Batani, Dimitri; Previdi, Fabio; Conti, Aldo; Pisani, Francesca; Botto, Cesare; Bortolotto, Fulvia; Torsiello, Flavia; Turcu, I. C. Edmond; Allott, Ric M.; Lisi, Nicola; Milani, Marziale; Costato, Michele; Pozzi, Achille; Koenig, Michel

1997-10-01

Saccharomyces Cerevisiae yeast cells were irradiated using the soft X-ray laser-plasma source at Rutherford Laboratory. The aim was to produce a selective damage of enzyme metabolic activity at the wall and membrane level (responsible for fermentation) without interfering with respiration (taking place in mitochondria) and with nuclear and DNA activity. The source was calibrated by PIN diodes and X-ray spectrometers. Teflon stripes were chosen as targets for the UV laser, emitting X-rays at about 0.9 keV, characterized by a very large decay exponent in biological matter. X-ray doses to the different cell compartments were calculated following a Lambert-Bouguet-Beer law. After irradiation, the selective damage to metabolic activity at the membrane level was measured by monitoring CO2 production with pressure silicon detectors. Preliminary results gave evidence of pressure reduction for irradiated samples and non-linear response to doses. Also metabolic oscillations were evidenced in cell suspensions and it was shown that X-ray irradiation changed the oscillation frequency.

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.

MOXE: An X-ray all-sky monitor for Soviet Spectrum-X-Gamma Mission

NASA Technical Reports Server (NTRS)

Priedhorsky, W.; Fenimore, E. E.; Moss, C. E.; Kelley, R. L.; Holt, S. S.

1989-01-01

A Monitoring Monitoring X-Ray Equipment (MOXE) is being developed for the Soviet Spectrum-X-Gamma Mission. MOXE is an X-ray all-sky monitor based on array of pinhole cameras, to be provided via a collaboration between Goddard Space Flight Center and Los Alamos National Laboratory. The objectives are to alert other observers on Spectrum-X-Gamma and other platforms of interesting transient activity, and to synoptically monitor the X-ray sky and study long-term changes in X-ray binaries. MOXE will be sensitive to sources as faint as 2 milliCrab (5 sigma) in 1 day, and cover the 2 to 20 KeV band.

History of Chandra X-Ray Observatory

NASA Image and Video Library

1997-05-01

This photograph shows the Chandra X-Ray Observatory (CXO), formerly Advanced X-Ray Astrophysics Facility (AXAF), High Resolution Mirror Assembly (HRMA) being removed from the test structure in the X-Ray Calibration Facility (XRCF) at the Marshall Space Flight Center (MSFC). The AXAF was renamed CXO in 1999. The CXO is the most sophisticated and the world's most powerful x-ray telescope ever built. It observes x-rays from high-energy regions of the universe, such as hot gas in the remnants of exploded stars. The HRMA, the heart of the telescope system, is contained in the cylindrical "telescope" portion of the observatory. Since high-energy x-rays would penetrate a normal mirror, special cylindrical mirrors were created. The two sets of four nested mirrors resemble tubes within tubes. Incoming x-rays graze off the highly polished mirror surface and are furneled to the instrument section for detection and study. MSFC's XRCF is the world's largest, most advanced laboratory for simulating x-ray emissions from distant celestial objects. It produces a space-like environment in which components related to x-ray telescope imaging are tested and the quality of their performances in space is predicted. TRW, Inc. was the prime contractor for the development of the CXO and NASA's MSFC was responsible for its project management. The Smithsonian Astrophysical Observatory controls science and flight operations of the CXO for NASA from Cambridge, Massachusetts. The CXO was launched July 22, 1999 aboard the Space Shuttle Columbia (STS-93).

History of Chandra X-Ray Observatory

NASA Image and Video Library

1996-12-16

This is a photograph of the Chandra X-Ray Observatory (CXO), formerly Advanced X-Ray Astrophysics Facility (AXAF), High Resolution Mirror Assembly (HRMA) integration at the X-Ray Calibration Facility (XRCF) at the Marshall Space Flight Center (MSFC). The AXAF was renamed CXO in 1999. The CXO is the most sophisticated and the world's most powerful x-ray telescope ever built. It observes x-rays from high-energy regions of the universe, such as hot gas in the remnants of exploded stars. The HRMA, the heart of the telescope system, is contained in the cylindrical "telescope" portion of the observatory. Since high-energy x-rays would penetrate a normal mirror, special cylindrical mirrors were created. The two sets of four nested mirrors resemble tubes within tubes. Incoming x-rays graze off the highly polished mirror surface and are furneled to the instrument section for detection and study. MSFC's XRCF is the world's largest, most advanced laboratory for simulating x-ray emissions from distant celestial objects. It produces a space-like environment in which components related to x-ray telescope imaging are tested and the quality of their performances in space is predicted. TRW, Inc. was the prime contractor for the development of the CXO and NASA's MSFC was responsible for its project management. The Smithsonian Astrophysical Observatory controls science and flight operations of the CXO for NASA from Cambridge, Massachusetts. The CXO was launched July 22, 1999 aboard the Space Shuttle Columbia (STS-93).

History of Chandra X-Ray Observatory

NASA Image and Video Library

1997-12-16

This is a photograph of the Chandra X-Ray Observatory (CXO), formerly Advanced X-Ray Astrophysics Facility (AXAF), High Resolution Mirror Assembly (HRMA) integration at the X-Ray Calibration Facility (XRCF) at the Marshall Space Flight Center (MSFC). The AXAF was renamed CXO in 1999. The CXO is the most sophisticated and the world's most powerful x-ray telescope ever built. It observes x-rays from high-energy regions of the universe, such as hot gas in the remnants of exploded stars. The HRMA, the heart of the telescope system, is contained in the cylindrical "telescope" portion of the observatory. Since high-energy x-rays would penetrate a normal mirror, special cylindrical mirrors were created. The two sets of four nested mirrors resemble tubes within tubes. Incoming x-rays graze off the highly polished mirror surface and are furneled to the instrument section for detection and study. MSFC's XRCF is the world's largest, most advanced laboratory for simulating x-ray emissions from distant celestial objects. It produces a space-like environment in which components related to x-ray telescope imaging are tested and the quality of their performances in space is predicted. TRW, Inc. was the prime contractor for the development of the CXO and NASA's MSCF was responsible for its project management. The Smithsonian Astrophysical Observatory controls science and flight operations of the CXO for NASA from Cambridge, Massachusetts. The CXO was launched July 22, 1999 aboard the Space Shuttle Columbia (STS-93).

History of Chandra X-Ray Observatory

NASA Image and Video Library

1997-05-01

This photograph shows the Chandra X-ray Observatory (CXO), formerly Advanced X-Ray Astrophysics Facility (AXAF), High Resolution Mirror Assembly (HRMA) being removed from the test structure in the X-Ray Calibration Facility (XRCF) at the Marshall Space Flight Center (MSFC). The AXAF was renamed CXO in 1999. The CXO is the most sophisticated and the world's most powerful x-ray telescope ever built. It observes x-rays from high-energy regions of the universe, such as hot gas in the remnants of exploded stars. The HRMA, the heart of the telescope system, is contained in the cylindrical "telescope" portion of the observatory. Since high-energy x-rays would penetrate a normal mirror, special cylindrical mirrors were created. The two sets of four nested mirrors resemble tubes within tubes. Incoming x-rays graze off the highly polished mirror surface and are furneled to the instrument section for detection and study. MSFC's XRCF is the world's largest, most advanced laboratory for simulating x-ray emissions from distant celestial objects. It produces a space-like environment in which components related to x-ray telescope imaging are tested and the quality of their performances in space is predicted. TRW, Inc. was the prime contractor for the development of the CXO and NASA's MSFC was responsible for its project management. The Smithsonian Astrophysical Observatory controls science and flight operations of the CXO for NASA from Cambridge, Massachusetts. The CXO was launched July 22, 1999 aboard the Space Shuttle Columbia (STS-93).

Portable Soft X-Ray Laser

DTIC Science & Technology

1992-05-22

ABSTRACT (Maximum 200 worch) A carpact sOtt X-ray laser (SXL) can be designed combining results of Princeton Plasma Physics Laboratory ( PPPL ) and Rutherford...Appleton Laboratory (RAL). At PPPL , gain at 18.2nm was dem- onstrated in a carbon plasma pumped by a low energy laser, with no mag- netic field. The...Physics Laboratory ( PPPL ) and Rutherford Appleton Laboratory (RAL). In the PPPL experiment, gain at a wavelength of 18.2 nm was demonstrated in a

History of Chandra X-Ray Observatory

NASA Image and Video Library

2002-01-23

Leon Van Speybroeck of the Harvard-Smithsonian Center for Astrophysics in Cambridge Massachusetts was awarded the 2002 Bruno Rossi Prize of the High-Energy Astrophysics Division of the American Astronomy Society. The Rossi Prize is an arnual recognition of significant contributions in high-energy astrophysics in honor of the Massachusetts Institute of Technology's late Professor Bruno Rossi, an authority on cosmic ray physics and a pioneer in the field of x-ray astronomy. Van Speybroeck, who led the effort to design and make the x-ray mirrors for NASA's premier Chandra X-Ray Observatory, was recognized for a career of stellar achievements in designing precision x-ray optics. As Telescope Scientist for Chandra, he has worked for more than 20 years with a team that includes scientists and engineers from the Harvard-Smithsonian, NASA's Marshall Space Flight Center, TRW, Inc., Huhes-Danbury (now B.F. Goodrich Aerospace), Optical Coating Laboratories, Inc., and Eastman-Kodak on all aspects of the x-ray mirror assembly that is the heart of the observatory.

Coherent X-ray imaging across length scales

NASA Astrophysics Data System (ADS)

Munro, P. R. T.

2017-04-01

Contemporary X-ray imaging techniques span a uniquely wide range of spatial resolutions, covering five orders of magnitude. The evolution of X-ray sources, from the earliest laboratory sources through to highly brilliant and coherent free-electron lasers, has been key to the development of these imaging techniques. This review surveys the predominant coherent X-ray imaging techniques with fields of view ranging from that of entire biological organs, down to that of biomolecules. We introduce the fundamental principles necessary to understand the image formation for each technique as well as briefly reviewing coherent X-ray source development. We present example images acquired using a selection of techniques, by leaders in the field.

New Possibilities for Understanding Complex Metal Hydrides via Synchrotron X-ray Studies

NASA Astrophysics Data System (ADS)

Dobbins, Tabbetha

2008-03-01

Ultrasmall-angle x-ray scattering (USAXS) and X-ray absorption spectroscopy (XAS) are used for the study of chemical and morphological changes in metal hydride powder (e.g. NaAlH4) both before and after transition metal salt catalytic dopant additions by high energy ball milling. The variation in surface fractal dimension and particle size with milling time and dopant content were tracked. These studies show that dopant content level (e.g. 2 mol % and 4 mol %) and dopant type (i.e. TiCl2, TiCl3, VCl3, and ZrCl4) markedly affects NaAlH4 powder particle surface area (determined using USAXS surface fractal dimension). As well, the chemical reaction between the catalyst and hydride powder was further elucidated using XAS. Ti-metal reacts with the Al desorption product (from NaAlH4) to form TiAlx product phases. These studies were able to link powder particle surface area to catalytic doping and were able to link dopant chemical state with dehydrogenation reactant and product phases.

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

High Resolution X-ray Imaging

NASA Technical Reports Server (NTRS)

Cash, Webster

2002-01-01

NAG5-5020 covered a period of 7.5 years during which a great deal of progress was made in x-ray optical techniques under this grant. We survived peer review numerous times during the effort to keep the grant going. In 1994, when the grant started we were actively pursuing the application of spherical mirrors to improving x-ray telescopes. We had found that x-ray detectors were becoming rapidly more sophisticated and affordable, but that x-ray telescopes were only being improved through the intense application of money within the AXAF program. Clearly new techniques for the future were needed. We were successful in developing and testing at the HELSTF facility in New Mexico a four reflection coma-corrected telescope made from spheres. We were able to demonstrate 0.3 arcsecond resolution, almost to the diffraction limit of the system. The community as a whole was, at that time, not particularly interested in looking past AXAF (Chandra) and the effort needed to evolve. Since we had reached the diffraction limit using non-Wolter optics we then decided to see if we could build an x-ray interferometer in the laboratory. In the lab the potential for improved resolution was substantial. If synthetic aperture telescopes could be built in space, then orders of magnitude improvement would become feasible. In 1998 NASA, under the direction of Dr. Nick White of Goddard, started a study to assess the potential and feasibility of x-ray interferometry in space. My work became of central interest to the committee because it indicated that such was possible. In early 1999 we had the breakthrough that allowed us build a practical interferometer. By using flats and hooking up with the Marshall Space Flight Center facilities we were able to demonstrate fringes at 1.25keV on a one millimeter baseline. This actual laboratory demonstration provided the solid proof of concept that NASA needed.

Microstructural Examination of Oxidized Fe_(14-x) Nb5_x Alloy Produced from Powders Prepared by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Demirkıran, A. Şükran; Sen, Saduman; Ozdemir, Ozkan; Sen, Ugur

In the present study, ferrous niobium, ferrous boron and iron were used as starting powders. The mixture of the powders which were calculated to give the designed compositions was prepared by using planetary high energy ball mill. Mechanically alloyed powders were pressed and sintered at 1350°C for 120 min in Ar atmosphere. The cyclic oxidation experiments were carried out in an electrical furnace at 650, 750 and 850 °C in open atmosphere for 96 h. The specimens were periodically weighed for the determination of weight change. Before and after oxidation, the present phases of the samples were determined by X-ray diffraction analysis (XRD). The microstructural characterizations were realized using scanning electron microscopy (SEM) with EDS attachment.

Laboratory Measurements of X-Ray Emissions From Centimeter-Long Streamer Corona Discharges

NASA Astrophysics Data System (ADS)

da Silva, C. L.; Millan, R. M.; McGaw, D. G.; Yu, C. T.; Putter, A. S.; LaBelle, J.; Dwyer, J.

2017-11-01

We provide extensive evidence that runaway electron acceleration and subsequent bremsstrahlung X-ray emission are a common feature in negative electrical discharges with voltages as low as 100 kV, indicating that all negative lightning could potentially produce runaway electrons. Centimeter long streamer corona discharges produce bursts of X-ray radiation, emitted by a source highly compact in space and time, leading to photon pileup. Median photon burst energies vary between 33 and 96 keV in 100 kV discharges. Statistical analysis of 5,000+ discharges shows that X-rays are observed in as many as 60% of the triggers, depending on the configuration. X-ray detection is more frequent when streamers are not followed by a spark, the detector is oriented perpendicular to the gap, and a thicker anode is used. In an 8-cm-long gap, X-rays are produced when runaway electrons hit the anode, and the electron acceleration is not necessarily correlated with streamer collisions.

Laboratory implementation of edge illumination X-ray phase-contrast imaging with energy-resolved detectors

NASA Astrophysics Data System (ADS)

Diemoz, P. C.; Endrizzi, M.; Vittoria, F. A.; Hagen, C. K.; Kallon, G.; Basta, D.; Marenzana, M.; Delogu, P.; Vincenzi, A.; De Ruvo, L.; Spandre, G.; Brez, A.; Bellazzini, R.; Olivo, A.

2015-03-01

Edge illumination (EI) X-ray phase-contrast imaging (XPCI) has potential for applications in different fields of research, including materials science, non-destructive industrial testing, small-animal imaging, and medical imaging. One of its main advantages is the compatibility with laboratory equipment, in particular with conventional non-microfocal sources, which makes its exploitation in normal research laboratories possible. In this work, we demonstrate that the signal in laboratory implementations of EI can be correctly described with the use of the simplified geometrical optics. Besides enabling the derivation of simple expressions for the sensitivity and spatial resolution of a given EI setup, this model also highlights the EI's achromaticity. With the aim of improving image quality, as well as to take advantage of the fact that all energies in the spectrum contribute to the image contrast, we carried out EI acquisitions using a photon-counting energy-resolved detector. The obtained results demonstrate that this approach has great potential for future laboratory implementations of EI.

Advanced High Brilliance X-Ray Source

NASA Technical Reports Server (NTRS)

Gibson, Walter M.

1998-01-01

The possibility to dramatically increase the efficiency of laboratory based protein structure measurements through the use of polycapillary X-ray optics was investigated. This project initiated April 1, 1993 and concluded December 31, 1996 (including a no cost extension from June 31, 1996). This is a final report of the project. The basis for the project is the ability to collect X-rays from divergent electron bombardment laboratory X-ray sources and redirect them into quasiparallel or convergent (focused) beams. For example, a 0.1 radian (approx. 6 deg) portion of a divergent beam collected by a polycapillary collimator and transformed into a quasiparallel beam of 3 millradian (0.2 deg) could give a gain of 6(exp 2)/0.2(exp 2) x T for the intensity of a diffracted beam from a crystal with a 0.2 deg diffraction width. T is the transmission efficiency of the polycapillary diffraction optic, and for T=0.5, the gain would be 36/0.04 x O.5=45. In practice, the effective collection angle will depend on the source spot size, the input focal length of the optic (usually limited by the source spot-to-window distance on the x-ray tube) and the size of the crystal relative to the output diameter of the optic. The transmission efficiency, T, depends on the characteristics (fractional open area, surface roughness, shape and channel diameter) of the polycapillary optic and is typically in the range 0.2-0.4. These effects could substantially reduce the expected efficiency gain. During the course of this study, the possibility to use a weakly focused beam (0.5 deg convergence) was suggested which could give an additional 10-20 X efficiency gain for small samples . Weakly focused beams from double focusing mirrors are frequently used for macromolecular crystallography studies. Furthermore the crystals are typically oscillated by as much as 2 deg during each X-ray exposure in order to increase the reciprocal space (number of crystal planes) sampled and use of a slightly convergent

Quantitative measurement of indomethacin crystallinity in indomethacin-silica gel binary system using differential scanning calorimetry and X-ray powder diffractometry.

PubMed

Pan, Xiaohong; Julian, Thomas; Augsburger, Larry

2006-02-10

Differential scanning calorimetry (DSC) and X-ray powder diffractometry (XRPD) methods were developed for the quantitative analysis of the crystallinity of indomethacin (IMC) in IMC and silica gel (SG) binary system. The DSC calibration curve exhibited better linearity than that of XRPD. No phase transformation occurred in the IMC-SG mixtures during DSC measurement. The major sources of error in DSC measurements were inhomogeneous mixing and sampling. Analyzing the amount of IMC in the mixtures using high-performance liquid chromatography (HPLC) could reduce the sampling error. DSC demonstrated greater sensitivity and had less variation in measurement than XRPD in quantifying crystalline IMC in the IMC-SG binary system.

Laboratory X-ray Studies with Trapped Highly Charged Ions Using Synchrotrons and Free-electron Lasers

NASA Astrophysics Data System (ADS)

Crespo López-Urrutia, José R.

2018-06-01

Laboratory studies on highly charged ions (HCI) using electron beam ion traps (EBITs) can cover all charge states and chemical elements found in astrophysical sources. Since their introduction in 1986, a wealth of emission measurements from the optical to the x-ray range has been carried out by different groups. In most of the work, electron-impact excitation was the driving mechanism, and high resolution spectrometers were used for the diagnostic of the emitted radiation. Other recent studies included x-ray emission following charge exchange, a mechanism which is present in many astrophysical environments and can help explain some of the unknown spectral features at 3.55 keV.In the last decade, excitation and photoionization have also been investigated by exposing HCI trapped in an EBIT to intense, monochromatic radiation from free-electron lasers and synchrotron sources. Here, advanced monochromators in powerful undulator beamlines allowed us to work at photon energies from 50 eV to 15 keV while resolving the natural linewidths of x-ray transitions like the Kα complex of Fe up to the highest charge states, and to measure the oscillator strengths of, e. g., the neonlike Fe16+ spectrum. Photoionization studies have been performed for those species as well. Very recently, our novel compact EBIT with an off-axis electron gun allows for simultaneously using the photon beam downstream, enabling exact wavelength determinations referenced to HCI with accurately calculable transitions. We have performed a recalibration of the molecular and atomic oxygen soft x-ray absorption lines in the 500 eV range with an uncertainty estimate of 30 meV. This revealed a 600 meV calibration error that propagated through the literature for decades with the consequence of a 200 km/s misfit of the velocity in interstellar oxygen absorbers. Other possibilities for the compact EBIT are investigations of resonant photorecombination processes with excellent energy resolution. With the

Spiral chain structure of high pressure selenium-II{sup '} and sulfur-II from powder x-ray diffraction

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

Fujihisa, Hiroshi; Yamawaki, Hiroshi; Sakashita, Mami

2004-10-01

The structure of high pressure phases, selenium-II{sup '} (Se-II{sup '}) and sulfur-II (S-II), for {alpha}-Se{sub 8} (monoclinic Se-I) and {alpha}-S{sub 8} (orthorhombic S-I) was studied by powder x-ray diffraction experiments. Se-II{sup '} and S-II were found to be isostructural and to belong to the tetragonal space group I4{sub 1}/acd, which is made up of 16 atoms in the unit cell. The structure consisted of unique spiral chains with both 4{sub 1} and 4{sub 3} screws. The results confirmed that the structure sequence of the pressure-induced phase transitions for the group VIb elements depended on the initial molecular form. The chemicalmore » bonds of the phases are also discussed from the interatomic distances that were obtained.« less

Laboratory and In-Flight In-Situ X-ray Imaging and Scattering Facility for Materials, Biotechnology and Life Sciences

NASA Technical Reports Server (NTRS)

2003-01-01

We propose a multifunctional X-ray facility for the Materials, Biotechnology and Life Sciences Programs to visualize formation and behavior dynamics of materials, biomaterials, and living organisms, tissues and cells. The facility will combine X-ray topography, phase micro-imaging and scattering capabilities with sample units installed on the goniometer. This should allow, for the first time, to monitor under well defined conditions, in situ, in real time: creation of imperfections during growth of semiconductors, metal, dielectric and biomacromolecular crystals and films, high-precision diffraction from crystals within a wide range of temperatures and vapor, melt, solution conditions, internal morphology and changes in living organisms, tissues and cells, diffraction on biominerals, nanotubes and particles, radiation damage, also under controlled formation/life conditions. The system will include an ultrabright X-ray source, X-ray mirror, monochromator, image-recording unit, detectors, and multipurpose diffractometer that fully accommodate and integrate furnaces and samples with other experimental environments. The easily adjustable laboratory and flight versions will allow monitoring processes under terrestrial and microgravity conditions. The flight version can be made available using a microsource combined with multilayer or capillary optics.

Advances toward submicron resolution optics for x-ray instrumentation and applications

NASA Astrophysics Data System (ADS)

Cordier, Mark; Stripe, Benjamin; Yun, Wenbing; Lau, S. H.; Lyon, Alan; Reynolds, David; Lewis, Sylvia J. Y.; Chen, Sharon; Semenov, Vladimir A.; Spink, Richard I.; Seshadri, Srivatsan

2017-08-01

Sigray's axially symmetric x-ray optics enable advanced microanalytical capabilities for focusing x-rays to microns-scale to submicron spot sizes, which can potentially unlock many avenues for laboratory micro-analysis. The design of these optics allows submicron spot sizes even at low x-ray energies, enabling research into low atomic number elements and allows increased sensitivity of grazing incidence measurements and surface analysis. We will discuss advances made in the fabrication of these double paraboloidal mirror lenses designed for use in laboratory x-ray applications. We will additionally present results from as-built paraboloids, including surface figure error and focal spot size achieved to-date.

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.

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.

Synchrotron powder X-ray diffraction and structural analysis of Eu0.5La0.5FBiS2-x Se x

NASA Astrophysics Data System (ADS)

Nagasaka, K.; Jinno, G.; Miura, O.; Miura, A.; Moriyoshi, C.; Kuroiwa, Y.; Mizuguchi, Y.

2017-07-01

Eu0.5La0.5FBiS2-x Se x is a new BiS2-based superconductor system. In Eu0.5La0.5FBiS2-x Se x , electron carriers are doped to the BiS2 layer by the substitution of Eu by La. Bulk superconductivity in this system is induced by increasing the in-plane chemical pressure, which is controlled by the Se concentration (x). In this study, we have analysed the crystal structure of Eu0.5La0.5FBiS2-x Se x using synchrotron powder diffraction and the Rietveld refinement. The precise determination of the structural parameters and thermal factors suggest that the emergence of bulk superconductivity in Eu0.5La0.5FBiS2-x Se x is achieved by the enhanced in-plane chemical pressure and the decrease in in-plane disorder.

Structure of N-(5-ethyl-[1,3,4]-thiadiazole-2-yl)toluenesulfonamide by combined X-ray powder diffraction, 13C solid-state NMR and molecular modelling.

PubMed

Hangan, Adriana; Borodi, Gheorghe; Filip, Xenia; Tripon, Carmen; Morari, Cristian; Oprean, Luminita; Filip, Claudiu

2010-12-01

The crystal structure solution of the title compound is determined from microcrystalline powder using a multi-technique approach that combines X-ray powder diffraction (XRPD) data analysis based on direct-space methods with information from (13)C solid-state NMR (SSNMR), and molecular modelling using the GIPAW (gauge including projector augmented-wave) method. The space group is Pbca with one molecule in the asymmetric unit. The proposed methodology proves very useful for unambiguously characterizing the supramolecular arrangement adopted by the N-(5-ethyl-[1,3,4]-thiadiazole-2-yl)toluenesulfonamide molecules in the crystal, which consists of extended double strands held together by C-H···π non-covalent interactions.

Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

2004-01-01

A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

A novel synthesis of polymeric CO via useful hard X-ray photochemistry

NASA Astrophysics Data System (ADS)

Pravica, Michael; Sneed, Daniel; Smith, Quinlan; Billinghurst, Brant; May, Tim; White, Melanie; Dziubek, Kamil

2016-12-01

We report on the synchrotron hard X-ray-induced decomposition of strontium oxalate (SrC2O4) pressurized to 7 GPa inside a diamond anvil cell (DAC). After some 4 h of irradiation in a white X-ray synchrotron beam, a dark reddish/brown region formed in the area of irradiation which was surrounded by a yellowish brown remainder in the rest of the sample. Upon depressurization of the sample to ambient conditions, the reacted/decomposed sample was recoverable as a dark brown/red and yellow waxy solid. Synchrotron infrared spectroscopy confirmed the strong presence of CO2 even under ambient conditions with the sample exposed to air and other strongly absorbing regions, suggesting that the sample may likely be polymerized CO (in part) with dispersed CO2 and SrO trapped within the polymer. These results will have significant implications in the ability to readily produce and trap CO2 in situ via irradiation of a simple powder for useful hard X-ray photochemistry and in the ability to easily manufacture polymeric CO (via loading of powders in a DAC or high volume press) without the need for the dangerous and complex loading of toxic CO. A novel means of X-ray-induced polymerization under extreme conditions has also been demonstrated.

Global Properties of X-Ray Flashes and X-Ray-Rich Gamma-Ray Bursts Observed by Swift

NASA Astrophysics Data System (ADS)

Sakamoto, Takanori; Yamazaki, Ryo; Barthelmy, Scott; Gehrels, Neil; Osborne, Julian; Hullinger, Derek; Sato, Goro; Barbier, Louis; Cummings, Jay; Fenimore, Ed; Krimm, Hans; Lamb, Don; Markwardt, Craig; Palmer, David; Parsons, Ann; Stamatikos, Michael; Tueller, Jack

Takanori Sakamoto, Taka.Sakamoto@nasa.gov NASA Goddard Space Flight Center, Greenbelt, Maryland, United States Ryo Yamazaki, ryo@theo.phys.sci.hiroshima-u.ac.jp Hiroshima University, Higashi-Hiroshima, Japan Scott Barthelmy, scott@milkyway.gsfc.nasa.gov NASA GSFC, Greenbelt, Maryland, United States Neil Gehrels, gehrels@milkyway.gsfc.nasa.gov NASA Goddard Space Flight Center, Greenbelt, Maryland, United States Julian Osborne, julo@star.le.ac.uk University of Leicester, Leicester, United Kingdom Derek Hullinger, derek.hullinger@gmail.com Moxtek, Inc, Orem, Utah, United States Goro Sato, Goro.Sato@nasa.gov Goddard Space Flight Center, Greenbelt, Maryland, United States Louis Barbier, lmb@milkyway.gsfc.nasa.gov Goddard Space Flight Center, Greenbelt, Maryland, United States Jay Cummings, jayc@milkyway.gsfc.nasa.gov Goddard Space Flight Center, Greenbelt, Maryland, United States Ed Fenimore, efenimore@lanl.gov Los Alamos National Laboratory, Los Alamos, California, United States Hans Krimm, hans.krimm@nasa.gov Goddard Space Flight Center, Greenbelt, Maryland, United States Don Lamb, d-lamb@uchicago.edu University of Chicago, Chicago, Illinois, United States Craig Markwardt, Craig.Markwardt@nasa.gov Goddard Space Flight Center, Greenbelt, Maryland, United States David Palmer, palmer@lanl.gov Los Alamos National Laboratory, Los Alamos, California, United States Ann Parsons, Ann.M.Parsons@nasa.gov Goddard Space Flight Center, Greenbelt, Maryland, United States Michael Stamatikos, michael@milkyway.gsfc.nasa.gov Goddard Space Flight Center, Greenbelt, Maryland, United States Jack Tueller, jack.tueller@nasa.gov Goddard Space Flight Center, Greenbelt, Maryland, United States We present the spectral and temporal characteristics of the prompt emission and X-ray afterglow emission of X-ray flashes (XRFs) and X-ray-rich gamma-ray bursts (XRRs) detected and observed by Swift between December 2004 and September 2006. We compare these characteristics to a sample of conventional

X-ray diffraction study of elemental thulium to 86 GPa

NASA Astrophysics Data System (ADS)

Pravica, Michael; Romano, Edward; Quine, Zachary; Pravica, Walter

2006-03-01

We have studied the structures and equation of state of elemental thulium up to 86 GPa in a diamond anvil cell using angular-dispersive x-ray powder diffraction methods at the Advanced Photon Source. This is part of a study of phase transitions in the lanthanide-series metals using cyclohexane as a quasi-hydrostatic medium. We present evidence of a series of phase transitions that appear to follow the anticipated hcp ->Sm-type -> dhcp -> distorted fcc sequence of transitions and show the equation of state derived from the x-ray fit data.

Femtosecond profiling of shaped x-ray pulses

NASA Astrophysics Data System (ADS)

Hoffmann, M. C.; Grguraš, I.; Behrens, C.; Bostedt, C.; Bozek, J.; Bromberger, H.; Coffee, R.; Costello, J. T.; DiMauro, L. F.; Ding, Y.; Doumy, G.; Helml, W.; Ilchen, M.; Kienberger, R.; Lee, S.; Maier, A. R.; Mazza, T.; Meyer, M.; Messerschmidt, M.; Schorb, S.; Schweinberger, W.; Zhang, K.; Cavalieri, A. L.

2018-03-01

Arbitrary manipulation of the temporal and spectral properties of x-ray pulses at free-electron lasers would revolutionize many experimental applications. At the Linac Coherent Light Source at Stanford National Accelerator Laboratory, the momentum phase-space of the free-electron laser driving electron bunch can be tuned to emit a pair of x-ray pulses with independently variable photon energy and femtosecond delay. However, while accelerator parameters can easily be adjusted to tune the electron bunch phase-space, the final impact of these actuators on the x-ray pulse cannot be predicted with sufficient precision. Furthermore, shot-to-shot instabilities that distort the pulse shape unpredictably cannot be fully suppressed. Therefore, the ability to directly characterize the x-rays is essential to ensure precise and consistent control. In this work, we have generated x-ray pulse pairs via electron bunch shaping and characterized them on a single-shot basis with femtosecond resolution through time-resolved photoelectron streaking spectroscopy. This achievement completes an important step toward future x-ray pulse shaping techniques.

Femtosecond profiling of shaped x-ray pulses

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

Hoffmann, M. C.; Grguras, I.; Behrens, C.

Arbitrary manipulation of the temporal and spectral properties of x-ray pulses at free-electron lasers would revolutionize many experimental applications. At the Linac Coherent Light Source at Stanford National Accelerator Laboratory, the momentum phase-space of the free-electron laser driving electron bunch can be tuned to emit a pair of x-ray pulses with independently variable photon energy and femtosecond delay. However, while accelerator parameters can easily be adjusted to tune the electron bunch phase-space, the final impact of these actuators on the x-ray pulse cannot be predicted with sufficient precision. Furthermore, shot-to-shot instabilities that distort the pulse shape unpredictably cannot be fullymore » suppressed. Therefore, the ability to directly characterize the x-rays is essential to ensure precise and consistent control. In this work, we have generated x-ray pulse pairs via electron bunch shaping and characterized them on a single-shot basis with femtosecond resolution through time-resolved photoelectron streaking spectroscopy. Furthermore, this achievement completes an important step toward future x-ray pulse shaping techniques.« less

Femtosecond profiling of shaped x-ray pulses

DOE PAGES

Hoffmann, M. C.; Grguras, I.; Behrens, C.; ...

2018-03-26

Arbitrary manipulation of the temporal and spectral properties of x-ray pulses at free-electron lasers would revolutionize many experimental applications. At the Linac Coherent Light Source at Stanford National Accelerator Laboratory, the momentum phase-space of the free-electron laser driving electron bunch can be tuned to emit a pair of x-ray pulses with independently variable photon energy and femtosecond delay. However, while accelerator parameters can easily be adjusted to tune the electron bunch phase-space, the final impact of these actuators on the x-ray pulse cannot be predicted with sufficient precision. Furthermore, shot-to-shot instabilities that distort the pulse shape unpredictably cannot be fullymore » suppressed. Therefore, the ability to directly characterize the x-rays is essential to ensure precise and consistent control. In this work, we have generated x-ray pulse pairs via electron bunch shaping and characterized them on a single-shot basis with femtosecond resolution through time-resolved photoelectron streaking spectroscopy. Furthermore, this achievement completes an important step toward future x-ray pulse shaping techniques.« less

Structural Transitions in Nanosized Zn0.97Al0.03O Powders under High Pressure Analyzed by in Situ Angle-Dispersive X-ray Diffraction

PubMed Central

Lin, Chih-Ming; Liu, Hsin-Tzu; Zhong, Shi-Yao; Hsu, Chia-Hung; Chiu, Yi-Te; Tai, Ming-Fong; Juang, Jenh-Yih; Chuang, Yu-Chun; Liao, Yen-Fa

2016-01-01

Nanosized aluminum-doped zinc oxide Zn1−xAlxO (AZO) powders (AZO-NPs) with x = 0.01, 0.03, 0.06, 0.09 and 0.11 were synthesized by chemical precipitation method. The thermogravimetric analysis (TGA) indicated that the precursors were converted to oxides from hydroxides near 250 °C, which were then heated to 500 °C for subsequent thermal processes to obtain preliminary powders. The obtained preliminary powders were then calcined at 500 °C for three hours. The structure and morphology of the products were measured and characterized by angle-dispersive X-ray diffraction (ADXRD) and scanning electron microscopy (SEM). ADXRD results showed that AZO-NPs with Al content less than 11% exhibited würtzite zinc oxide structure and there was no other impurity phase in the AZO-NPs, suggesting substitutional doping of Al on Zn sites. The Zn0.97Al0.03O powders (A3ZO-NPs) with grain size of about 21.4 nm were used for high-pressure measurements. The in situ ADXRD measurements revealed that, for loading run, the pressure-induced würtzite (B4)-to-rocksalt (B1) structural phase transition began at 9.0(1) GPa. Compared to the predicted phase-transition pressure of ~12.7 GPa for pristine ZnO nanocrystals of similar grain size (~21.4 nm), the transition pressure for the present A3ZO-NPs exhibited a reduction of ~3.7 GPa. The significant reduction in phase-transition pressure is attributed to the effects of highly selective site occupation, namely Zn2+ and Al3+, were mainly found in tetrahedral and octahedral sites, respectively. PMID:28773683

Quantitative Measurements of X-ray Intensity

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

Haugh, M. J., Schneider, M.

This chapter describes the characterization of several X-ray sources and their use in calibrating different types of X-ray cameras at National Security Technologies, LLC (NSTec). The cameras are employed in experimental plasma studies at Lawrence Livermore National Laboratory (LLNL), including the National Ignition Facility (NIF). The sources provide X-rays in the energy range from several hundred eV to 110 keV. The key to this effort is measuring the X-ray beam intensity accurately and traceable to international standards. This is accomplished using photodiodes of several types that are calibrated using radioactive sources and a synchrotron source using methods and materials thatmore » are traceable to the U.S. National Institute of Standards and Technology (NIST). The accreditation procedures are described. The chapter begins with an introduction to the fundamental concepts of X-ray physics. The types of X-ray sources that are used for device calibration are described. The next section describes the photodiode types that are used for measuring X-ray intensity: power measuring photodiodes, energy dispersive photodiodes, and cameras comprising photodiodes as pixel elements. Following their description, the methods used to calibrate the primary detectors, the power measuring photodiodes and the energy dispersive photodiodes, as well as the method used to get traceability to international standards are described. The X-ray source beams can then be measured using the primary detectors. The final section then describes the use of the calibrated X-ray beams to calibrate X-ray cameras. Many of the references are web sites that provide databases, explanations of the data and how it was generated, and data calculations for specific cases. Several general reference books related to the major topics are included. Papers expanding some subjects are cited.« less

Popular Berkeley Lab X-ray Data Booklet reissued

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

Robinson, Art

2001-03-02

X-ray scientists and synchrotron-radiation users who have been patiently waiting for an updated version of the popular X-Ray Data Booklet last published in 1986 by the Center for X-Ray Optics at the Lawrence Berkeley National Laboratory can breathe a sigh of relief. The venerable ''little orange book'' has now been reissued under the auspices of CXRO and the Advanced Light Source (ALS) with an April printing of 10,000 paper copies and the posting of a Web edition at http://xdb.lbl.gov.

Results from a Grazing Incidence X-Ray Interferometer

NASA Technical Reports Server (NTRS)

Joy, Marshall K.; Shipley, Ann; Cash, Webster; Carter, James

2000-01-01

A prototype grazing incidence interferometer has been built and tested at EUV and X-ray wavelengths using a 120 meter long vacuum test facility at Marshall Space Flight Center. We describe the design and construction of the interferometer, the EUV and x-ray sources, the detector systems, and compare the interferometric fringe measurements with theoretical predictions. We also describe the next-generation grazing incidence system which is designed to provide laboratory demonstration of key technologies that will be needed for a space-based x-ray interferometer.

Kinetic Modeling of Ultraintense X-ray Laser-Matter Interactions

NASA Astrophysics Data System (ADS)

Royle, Ryan; Sentoku, Yasuhiko; Mancini, Roberto

2016-10-01

Hard x-ray free-electron lasers (XFELs) have had a profound impact on the physical, chemical, and biological sciences. They can produce millijoule x-ray laser pulses just tens of femtoseconds in duration with more than 1012 photons each, making them the brightest laboratory x-ray sources ever produced by several orders of magnitude. An XFEL pulse can be intensified to 1020 W/cm2 when focused to submicron spot sizes, making it possible to isochorically heat solid matter well beyond 100 eV. These characteristics enable XFELs to create and probe well-characterized warm and hot dense plasmas of relevance to HED science, planetary science, laboratory astrophysics, relativistic laser plasmas, and fusion research. Several newly developed atomic physics models including photoionization, Auger ionization, and continuum-lowering have been implemented in a particle-in-cell code, PICLS, which self-consistently solves the x-ray transport, to enable the simulation of the non-LTE plasmas created by ultraintense x-ray laser interactions with solid density matter. The code is validated against the results of several recent experiments and is used to simulate the maximum-intensity x-ray heating of solid iron targets. This work was supported by DOE/OFES under Contract No. DE-SC0008827.

Three-dimensional x-ray diffraction nanoscopy

NASA Astrophysics Data System (ADS)

Nikulin, Andrei Y.; Dilanian, Ruben A.; Zatsepin, Nadia A.; Muddle, Barry C.

2008-08-01

A novel approach to x-ray diffraction data analysis for non-destructive determination of the shape of nanoscale particles and clusters in three-dimensions is illustrated with representative examples of composite nanostructures. The technique is insensitive to the x-rays coherence, which allows 3D reconstruction of a modal image without tomographic synthesis and in-situ analysis of large (over a several cubic millimeters) volume of material with a spatial resolution of few nanometers, rendering the approach suitable for laboratory facilities.

Order-disorder-reorder process in thermally treated dolomite samples: a combined powder and single-crystal X-ray diffraction study

NASA Astrophysics Data System (ADS)

Zucchini, A.; Comodi, P.; Katerinopoulou, A.; Balic-Zunic, T.; McCammon, C.; Frondini, F.

2012-04-01

A combined powder and single-crystal X-ray diffraction analysis of dolomite [CaMg(CO3)2] heated to 1,200°C at 3 GPa was made to study the order-disorder-reorder process. The order/disorder transition is inferred to start below 1,100°C, and complete disorder is attained at approximately 1,200°C. Twinned crystals characterized by high internal order were found in samples annealed over 1,100°C, and their fraction was found to increase with temperature. Evidences of twinning domains combined with probable remaining disordered portions of the structure imply that reordering processes occur during the quench. Twin domains are hereby proposed as a witness to thermally induced intra-layer-type cation disordering.

X-ray microtomography of porous media at BNL

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

Dowd, B.

This session is comprised of pertinent information about the historical aspects, current status of research, technical achievements, and future plans in X-ray computed microtomography at Brookhaven National Laboratories. An explanation with specifications and diagrams of X-ray instrumentation is provided. Several high resolution 3-D color images of reservoir rock drill cores and other materials are included.

Lab-based x-ray nanoCT imaging

NASA Astrophysics Data System (ADS)

Müller, Mark; Allner, Sebastian; Ferstl, Simone; Dierolf, Martin; Tuohimaa, Tomi; Pfeiffer, Franz

2017-03-01

Due to the recent development of transmission X-ray tubes with very small focal spot sizes, laboratory-based CT imaging with sub-micron resolutions is nowadays possible. We recently developed a novel X-ray nanoCT setup featuring a prototype nanofocus X-ray source and a single-photon counting detector. The system is based on mere geometrical magnification and can reach resolutions of 200 nm. To demonstrate the potential of the nanoCT system for biomedical applications we show high resolution nanoCT data of a small piece of human tooth comprising coronal dentin. The reconstructed CT data clearly visualize the dentin tubules within the tooth piece.

Characterization of powdered fish heads for bone graft biomaterial applications.

PubMed

Oteyaka, Mustafa Ozgür; Unal, Hasan Hüseyin; Bilici, Namık; Taşçı, Eda

2013-01-01

The aim of this study was to define the chemical composition, morphology and crystallography of powdered fish heads of the species Argyrosomus regius for bone graft biomaterial applications. Two sizes of powder were prepared by different grinding methods; Powder A (coarse, d50=68.5 µm) and Powder B (fine, d50=19.1 µm). Samples were analyzed using X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), thermogravimetry (TG), and energy dispersive X-ray spectroscopy (EDS). The powder was mainly composed of aragonite (CaCO3) and calcite (CaCO3). The XRD pattern of Powder A and B matched standard aragonite and calcite patterns. In addition, the calcium oxide (CaO) phase was found after the calcination of Powder A. Thermogravimetry analysis confirmed total mass losses of 43.6% and 47.3% in Powders A and B, respectively. The microstructure of Powder A was mainly composed of different sizes and tubular shape, whereas Powder B showed agglomerated particles. The high quantity of CaO and other oxides resemble the chemical composition of bone. In general, the powder can be considered as bone graft after transformation to hydroxyapatite phase.

X-ray intensity and source size characterizations for the 25 kV upgraded Manson source at Sandia National Laboratories

NASA Astrophysics Data System (ADS)

Loisel, G.; Lake, P.; Gard, P.; Dunham, G.; Nielsen-Weber, L.; Wu, M.; Norris, E.

2016-11-01

At Sandia National Laboratories, the x-ray generator Manson source model 5 was upgraded from 10 to 25 kV. The purpose of the upgrade is to drive higher characteristics photon energies with higher throughput. In this work we present characterization studies for the source size and the x-ray intensity when varying the source voltage for a series of K-, L-, and M-shell lines emitted from Al, Y, and Au elements composing the anode. We used a 2-pinhole camera to measure the source size and an energy dispersive detector to monitor the spectral content and intensity of the x-ray source. As the voltage increases, the source size is significantly reduced and line intensity is increased for the three materials. We can take advantage of the smaller source size and higher source throughput to effectively calibrate the suite of Z Pulsed Power Facility crystal spectrometers.

A comparative study of the use of powder X-ray diffraction, Raman and near infrared spectroscopy for quantification of binary polymorphic mixtures of piracetam.

PubMed

Croker, Denise M; Hennigan, Michelle C; Maher, Anthony; Hu, Yun; Ryder, Alan G; Hodnett, Benjamin K

2012-04-07

Diffraction and spectroscopic methods were evaluated for quantitative analysis of binary powder mixtures of FII(6.403) and FIII(6.525) piracetam. The two polymorphs of piracetam could be distinguished using powder X-ray diffraction (PXRD), Raman and near-infrared (NIR) spectroscopy. The results demonstrated that Raman and NIR spectroscopy are most suitable for quantitative analysis of this polymorphic mixture. When the spectra are treated with the combination of multiplicative scatter correction (MSC) and second derivative data pretreatments, the partial least squared (PLS) regression model gave a root mean square error of calibration (RMSEC) of 0.94 and 0.99%, respectively. FIII(6.525) demonstrated some preferred orientation in PXRD analysis, making PXRD the least preferred method of quantification. Copyright © 2012 Elsevier B.V. All rights reserved.

Ultrafast X-Ray Coherent Control

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

Reis, David

2009-05-01

This main purpose of this grant was to develop the nascent eld of ultrafast x-ray science using accelerator-based sources, and originally developed from an idea that a laser could modulate the di racting properties of a x-ray di racting crystal on a fast enough time scale to switch out in time a shorter slice from the already short x-ray pulses from a synchrotron. The research was carried out primarily at the Advanced Photon Source (APS) sector 7 at Argonne National Laboratory and the Sub-Picosecond Pulse Source (SPPS) at SLAC; in anticipation of the Linac Coherent Light Source (LCLS) x-ray freemore » electron laser that became operational in 2009 at SLAC (all National User Facilities operated by BES). The research centered on the generation, control and measurement of atomic-scale dynamics in atomic, molecular optical and condensed matter systems with temporal and spatial resolution . It helped develop the ultrafast physics, techniques and scienti c case for using the unprecedented characteristics of the LCLS. The project has been very successful with results have been disseminated widely and in top journals, have been well cited in the eld, and have laid the foundation for many experiments being performed on the LCLS, the world's rst hard x-ray free electron laser.« less

X-Ray Diffraction on Mars: Scientific Discoveries Made by the CheMin Instrument

NASA Technical Reports Server (NTRS)

Rampe, E. B.; Blake, D. F.; Ming, D. W.; Bristow, T. F.

2017-01-01

The Mars Science Laboratory Curiosity landed in Gale crater in August 2012 with the goal to identify and characterize habitable environments on Mars. Curiosity has been studying a series of sedimentary rocks primarily deposited in fluviolacustrine environments approximately 3.5 Ga. Minerals in the rocks and soils on Mars can help place further constraints on these ancient aqueous environments, including pH, salinity, and relative duration of liquid water. The Chemistry and Mineralogy (CheMin) X-ray diffraction and X-ray fluorescence instrument on Curiosity uses a Co X-ray source and charge-coupled device detector in transmission geometry to collect 2D Debye-Scherrer ring patterns of the less than 150 micron size fraction of drilled rock powders or scooped sediments. With an angular range of approximately 2.52deg 20 and a 20 resolution of approximately 0.3deg, mineral abundances can be quantified with a detection limit of approximately 1-2 wt. %. CheMin has returned quantitative mineral abundances from 16 mudstone, sandstone, and aeolian sand samples so far. The mineralogy of these samples is incredibly diverse, suggesting a variety of depositional and diagenetic environments and different source regions for the sediments. Results from CheMin have been essential for reconstructing the geologic history of Gale crater and addressing the question of habitability on ancient Mars.

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

Solid-state synthesis of nano-sized Ba(Ti1- x Sn x )O3 powders and dielectric properties of corresponding ceramics

NASA Astrophysics Data System (ADS)

Ansaree, Md. Jawed; Kumar, Upendra; Upadhyay, Shail

2017-06-01

Powders of a few compositions of solid solution BaTi1- x Sn x O3 ( x = 0.0, 0.1, 0.2, 0.3 and 0.40) have been synthesized at 800 °C for 8 h using Ba(NO3)2, TiO2 and SnCl4·5H2O as starting materials. The thermogravimetric (TG) and differential scanning calorimetric (DSC) analysis of mixture in the stoichiometric proportion for sample BaTi0.80Sn0.20O3 have been carried out to understand the formation of solid solutions. Single-phase pure compounds (except x = 0.40) of the samples have been obtained at a lower calcination temperature (800 °C) than that of those reported in the literature for traditional solid-state synthesis making use of oxides and or carbonates as starting material (≥1200 °C). Tetragonal symmetry for compositions x = 0.0 and 0.10, cubic for x = 0.2 and 0.30 were found by X-ray diffraction (XRD) analysis. The transmission electron microscopic (TEM) analysis confirmed that calcined powders have a particle size between 30 and 50 nm. Ceramics of these powders were prepared by sintering at 1350 °C for 4 h. Properties of ceramics obtained in this work have been compared with properties reported in the literature.

Demonstration of Laser Plasma X-Ray Source with X-Ray Collimator Final Report CRADA No. TC-1564-99

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

Lane, S. M.; Forber, R. A.

2017-09-28

This collaborative effort between the University of California, Lawrence Livermore National Laboratory (LLNL) and JMAR Research, Inc. (JRI), was to demonstrate that LLNL x-ray collimators can effectively increase the wafer throughput of JRI's laser based x-ray lithography systems. The technical objectives were expected to be achieved by completion of the following tasks, which are separated into two task lists by funding source. The organization (LLNL or JMAR) having primary responsibility is given parenthetically for each task.

High Resolution X-ray Imaging

NASA Technical Reports Server (NTRS)

Cash, Webster

2002-01-01

NAG5-5020 covered a period of 7.5 years during which a great deal of progress was made in x-ray optical techniques under this grant. We survived peer review numerous times during the effort to keep the grant going. In 1994, when the grant started we were actively pursuing the application of spherical mirrors to improving x-ray telescopes. We had found that x-ray detectors were becoming rapidly more sophisticated and affordable, but that x-ray telescopes were only being improved through the intense application of money within the AXAF program. Clearly new techniques for the future were needed. We were successful in developing and testing at the HELSTF facility in New Mexico a four reflection coma-corrected telescope made from spheres. We were able to demonstrate 0.3 arcsecond resolution, almost to the diffraction limit of the system. The community as a whole was, at that time, not particularly interested in looking past AXAF (Chandra) and the effort needed to evolve. Since we had reached the diffraction limit using non-Wolter optics we then decided to see if we could build an x-ray interferometer in the laboratory. In the lab the potential for improved resolution was substantial. If synthetic aperture telescopes could be built in space, then orders of magnitude improvement would become feasible. In 1998 NASA, under the direction of Dr Nick White of Goddard, started a study to assess the potential and feasibility of x-ray interferometry in space. My work became of central interest to the committee because it indicated that such was possible. In early 1999 we had the breakthrough that allowed us build a practical interferometer. By using flats and hooking up with the Marshall Space Flight Center facilities we were able to demonstrate fringes at 1.25keV on a one millimeter baseline. This actual laboratory demonstration provided the solid proof of concept that NASA needed. As the year progressed the future of x-ray astronomy jelled around the Maxim program. Maxim is a

A novel synthesis of polymeric CO via useful hard X-ray photochemistry

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

Pravica, Michael; Sneed, Daniel; Smith, Quinlan

We report on the synchrotron hard X-ray-induced decomposition of strontium oxalate (SrC 2O 4) pressurized to 7 GPa inside a diamond anvil cell (DAC). After some 4 h of irradiation in a white X-ray synchrotron beam, a dark reddish/brown region formed in the area of irradiation which was surrounded by a yellowish brown remainder in the rest of the sample. Upon depressurization of the sample to ambient conditions, the reacted/decomposed sample was recoverable as a dark brown/red and yellow waxy solid. Synchrotron infrared spectroscopy confirmed the strong presence of CO 2 even under ambient conditions with the sample exposed tomore » air and other strongly absorbing regions, suggesting that the sample may likely be polymerized CO (in part) with dispersed CO 2 and SrO trapped within the polymer. These results will have significant implications in the ability to readily produce and trap CO 2 in situ via irradiation of a simple powder for useful hard X-ray photochemistry and in the ability to easily manufacture polymeric CO (via loading of powders in a DAC or high volume press) without the need for the dangerous and complex loading of toxic CO. As a result, a novel means of X-ray-induced polymerization under extreme conditions has also been demonstrated.« less

A novel synthesis of polymeric CO via useful hard X-ray photochemistry

DOE PAGES

Pravica, Michael; Sneed, Daniel; Smith, Quinlan; ...

2016-03-30

We report on the synchrotron hard X-ray-induced decomposition of strontium oxalate (SrC 2O 4) pressurized to 7 GPa inside a diamond anvil cell (DAC). After some 4 h of irradiation in a white X-ray synchrotron beam, a dark reddish/brown region formed in the area of irradiation which was surrounded by a yellowish brown remainder in the rest of the sample. Upon depressurization of the sample to ambient conditions, the reacted/decomposed sample was recoverable as a dark brown/red and yellow waxy solid. Synchrotron infrared spectroscopy confirmed the strong presence of CO 2 even under ambient conditions with the sample exposed tomore » air and other strongly absorbing regions, suggesting that the sample may likely be polymerized CO (in part) with dispersed CO 2 and SrO trapped within the polymer. These results will have significant implications in the ability to readily produce and trap CO 2 in situ via irradiation of a simple powder for useful hard X-ray photochemistry and in the ability to easily manufacture polymeric CO (via loading of powders in a DAC or high volume press) without the need for the dangerous and complex loading of toxic CO. As a result, a novel means of X-ray-induced polymerization under extreme conditions has also been demonstrated.« less

A hard X-ray nanoprobe beamline for nanoscale microscopy

PubMed Central

Winarski, Robert P.; Holt, Martin V.; Rose, Volker; Fuesz, Peter; Carbaugh, Dean; Benson, Christa; Shu, Deming; Kline, David; Stephenson, G. Brian; McNulty, Ian; Maser, Jörg

2012-01-01

The Hard X-ray Nanoprobe Beamline (or Nanoprobe Beamline) is an X-ray microscopy facility incorporating diffraction, fluorescence and full-field imaging capabilities designed and operated by the Center for Nanoscale Materials and the Advanced Photon Source at Sector 26 of the Advanced Photon Source at Argonne National Laboratory. This facility was constructed to probe the nanoscale structure of biological, environmental and material sciences samples. The beamline provides intense focused X-rays to the Hard X-ray Nanoprobe (or Nanoprobe) which incorporates Fresnel zone plate optics and a precision laser sensing and control system. The beamline operates over X-ray energies from 3 to 30 keV, enabling studies of most elements in the periodic table, with a particular emphasis on imaging transition metals. PMID:23093770

A hard X-ray nanoprobe beamline for nanoscale microscopy.

PubMed

Winarski, Robert P; Holt, Martin V; Rose, Volker; Fuesz, Peter; Carbaugh, Dean; Benson, Christa; Shu, Deming; Kline, David; Stephenson, G Brian; McNulty, Ian; Maser, Jörg

2012-11-01

The Hard X-ray Nanoprobe Beamline (or Nanoprobe Beamline) is an X-ray microscopy facility incorporating diffraction, fluorescence and full-field imaging capabilities designed and operated by the Center for Nanoscale Materials and the Advanced Photon Source at Sector 26 of the Advanced Photon Source at Argonne National Laboratory. This facility was constructed to probe the nanoscale structure of biological, environmental and material sciences samples. The beamline provides intense focused X-rays to the Hard X-ray Nanoprobe (or Nanoprobe) which incorporates Fresnel zone plate optics and a precision laser sensing and control system. The beamline operates over X-ray energies from 3 to 30 keV, enabling studies of most elements in the periodic table, with a particular emphasis on imaging transition metals.

History of Chandra X-Ray Observatory

NASA Image and Video Library

1997-03-16

This photo shows the High Resolution Camera (HRC) for the Chandra X-Ray Observatory (CXO), formerly Advanced X-Ray Astrophysics Facility (AXAF), being integrated with the High Resolution Mirror Assembly (HRMA) in Marshall Space Flight Center's (MSFC's) 24-foot Vacuum Chamber at the X-Ray Calibration Facility (XRCF). The AXAF was renamed CXO in 1999. The CXO is the most sophisticated and the world's most poweful x-ray telescope ever built. It observes x-rays from high-energy regions of the universe, such as hot gas in the remnants of exploded stars. The HRC is one of the two instruments used at the focus of CXO, where it will detect x-rays reflected from an assembly of eight mirrors. The unique capabilities of the HRC stem from the close match of its imaging capability to the focusing of the mirrors. When used with CXO mirrors, the HRC makes images that reveal detail as small as one-half an arc second. This is equivalent to the ability to read a newspaper at a distance of 1 kilometer. MSFC's XRCF is the world's largest, most advanced laboratory for simulating x-ray emissions from distant celestial objects. It produces a space-like environment in which components relatedto x-ray telescope imaging are tested and the quality of their performances in space is predicted. TRW, Inc. was the prime contractor for the development of the CXO and NASA's MSFC was responsible for its project management. The Smithsonian Astrophysical Observatory controls science and flight operations of the CXO for NASA from Cambridge, Massachusetts. The CXO was launched July 22, 1999 aboard the Space Shuttle Columbia (STS-93).

History of Chandra X-Ray Observatory

NASA Image and Video Library

1997-03-16

This photo shows the High Resolution Camera (HRC) for the Chandra X-Ray Observatory (CXO), formerly Advanced X-Ray Astrophysics Facility (AXAF), being integrated with the High Resolution Mirror Assembly (HRMA) in Marshall Space Flight Center's (MSFC's) 24-foot Vacuum Chamber at the X-Ray Calibration Facility (XRCF). The AXAF was renamed CXO in 1999. The CXO is the most sophisticated and the world's most powerful x-ray telescope ever built. It observes x-rays from high-energy regions of the universe, such as hot gas in the remnants of exploded stars. The HRC is one of the two instruments used at the focus of CXO, where it will detect x-rays reflected from an assembly of eight mirrors. The unique capabilities of the HRC stem from the close match of its imaging capability to the focusing of the mirrors. When used with CXO mirrors, the HRC makes images that reveal detail as small as one-half an arc second. This is equivalent to the ability to read a newspaper at a distance of 1 kilometer. MSFC's XRCF is the world's largest, most advanced laboratory for simulating x-ray emissions from distant celestial objects. It produces a space-like environment in which components related to x-ray telescope imaging are tested and the quality of their performances in space is predicted. TRW, Inc. was the prime contractor for the development of the CXO and NASA's MSFC was responsible for its project management. The Smithsonian Astrophysical Observatory controls science and flight operations of the CXO for NASA from Cambridge, Massachusetts. The CXO was launched July 22, 1999 aboard the Space Shuttle Columbia (STS-93).

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

Laboratory x-ray micro-computed tomography: a user guideline for biological samples

PubMed Central

2017-01-01

Abstract Laboratory x-ray micro–computed tomography (micro-CT) is a fast-growing method in scientific research applications that allows for non-destructive imaging of morphological structures. This paper provides an easily operated “how to” guide for new potential users and describes the various steps required for successful planning of research projects that involve micro-CT. Background information on micro-CT is provided, followed by relevant setup, scanning, reconstructing, and visualization methods and considerations. Throughout the guide, a Jackson's chameleon specimen, which was scanned at different settings, is used as an interactive example. The ultimate aim of this paper is make new users familiar with the concepts and applications of micro-CT in an attempt to promote its use in future scientific studies. PMID:28419369

Use of X-Ray Fluorescence in a Laboratory for the Treatment of Uranium Ores; UTILISATION DE LA FLUORESCENCE DANS UN LABORATOIRE DE TRAITEMENTS DE MINERAIS D'URANIUM

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

Guillet, H.

1960-01-01

A brief description is given of some aspects of the experience gained over a year during which x-ray fluorescence was used at the laberatory of the present Section Autonome d'Etudes, Recherches et Applications Chimiques of the Commissariat a l'Energie Atomique. A standard is tested daily to ensure reproducibility. The observations made during the months from Dec. 1958 to May 1959 are described. In acid leaching of uranium ores, the residues are analyzed by x-ray fluorescence directly in powder form. Fixation and elution of vanadium on ion-exchange resin were also studied. (auth)

X-Ray Diffraction on NIF

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

Eggert, J H; Wark, J

2012-02-15

The National Ignition Facility (NIF) is currently a 192 beam, 1.6 MJ laser. NIF Ramp-Compression Experiments have already made the relevant exo-planet pressure range from 1 to 50 Mbar accessible. We Proposed to Study Carbon Phases by X-Ray Diffraction on NIF. Just a few years ago, ultra-high pressure phase diagrams for materials were very 'simple'. New experiments and theories point out surprising and decidedly complex behavior at the highest pressures considered. High pressures phases of aluminum are also predicted to be complex. Recent metadynamics survey of carbon proposed a dynamic pathway among multiple phases. We need to develop diagnostics andmore » techniques to explore this new regime of highly compressed matter science. X-Ray Diffraction - Understand the phase diagram/EOS/strength/texture of materials to 10's of Mbar. Strategy and physics goals: (1) Powder diffraction; (2) Begin with diamond; (3) Continue with metals etc.; (4) Explore phase diagrams; (5) Develop liquid diffraction; and (6) Reduce background/improve resolution.« less

Fabrication of high-resolution x-ray diffractive optics at King's College London

NASA Astrophysics Data System (ADS)

Charalambous, Pambos S.; Anastasi, Peter A. F.; Burge, Ronald E.; Popova, Katia

1995-09-01

The fabrication of high resolution x-ray diffractive optics, and Fresnel zone plates (ZPs) in particular, is a very demanding multifaceted technological task. The commissioning of more (and brighter) synchrotron radiation sources, has increased the number of x-ray imaging beam lines world wide. The availability of cheaper and more effective laboratory x-ray sources, has further increased the number of laboratories involved in x-ray imaging. The result is an ever increasing demand for x-ray optics with a very wide range of specifications, reflecting the particular type of x-ray imaging performed at different laboratories. We have been involved in all aspects of high resolution nanofabrication for a number of years, and we have explored many different methods of lithography, which, although unorthodox, open up possibilities, and increase our flexibility for the fabrication of different diffractive optical elements, as well as other types of nanostructures. The availability of brighter x-ray sources, means that the diffraction efficiency of the ZPs is becoming of secondary importance, a trend which will continue in the future. Resolution, however, is important and will always remain so. Resolution is directly related to the accuracy af pattern generation, as well as the ability to draw fine lines. This is the area towards which we have directed most of our efforts so far.

In-Line Phase-Contrast X-ray Imaging and Tomography for Materials Science

PubMed Central

Mayo, Sheridan C.; Stevenson, Andrew W.; Wilkins, Stephen W.

2012-01-01

X-ray phase-contrast imaging and tomography make use of the refraction of X-rays by the sample in image formation. This provides considerable additional information in the image compared to conventional X-ray imaging methods, which rely solely on X-ray absorption by the sample. Phase-contrast imaging highlights edges and internal boundaries of a sample and is thus complementary to absorption contrast, which is more sensitive to the bulk of the sample. Phase-contrast can also be used to image low-density materials, which do not absorb X-rays sufficiently to form a conventional X-ray image. In the context of materials science, X-ray phase-contrast imaging and tomography have particular value in the 2D and 3D characterization of low-density materials, the detection of cracks and voids and the analysis of composites and multiphase materials where the different components have similar X-ray attenuation coefficients. Here we review the use of phase-contrast imaging and tomography for a wide variety of materials science characterization problems using both synchrotron and laboratory sources and further demonstrate the particular benefits of phase contrast in the laboratory setting with a series of case studies. PMID:28817018

In-Line Phase-Contrast X-ray Imaging and Tomography for Materials Science.

PubMed

Mayo, Sheridan C; Stevenson, Andrew W; Wilkins, Stephen W

2012-05-24

X-ray phase-contrast imaging and tomography make use of the refraction of X-rays by the sample in image formation. This provides considerable additional information in the image compared to conventional X-ray imaging methods, which rely solely on X-ray absorption by the sample. Phase-contrast imaging highlights edges and internal boundaries of a sample and is thus complementary to absorption contrast, which is more sensitive to the bulk of the sample. Phase-contrast can also be used to image low-density materials, which do not absorb X-rays sufficiently to form a conventional X-ray image. In the context of materials science, X-ray phase-contrast imaging and tomography have particular value in the 2D and 3D characterization of low-density materials, the detection of cracks and voids and the analysis of composites and multiphase materials where the different components have similar X-ray attenuation coefficients. Here we review the use of phase-contrast imaging and tomography for a wide variety of materials science characterization problems using both synchrotron and laboratory sources and further demonstrate the particular benefits of phase contrast in the laboratory setting with a series of case studies.

High-spatial-resolution nanoparticle x-ray fluorescence tomography

NASA Astrophysics Data System (ADS)

Larsson, Jakob C.; Vâgberg, William; Vogt, Carmen; Lundström, Ulf; Larsson, Daniel H.; Hertz, Hans M.

2016-03-01

X-ray fluorescence tomography (XFCT) has potential for high-resolution 3D molecular x-ray bio-imaging. In this technique the fluorescence signal from targeted nanoparticles (NPs) is measured, providing information about the spatial distribution and concentration of the NPs inside the object. However, present laboratory XFCT systems typically have limited spatial resolution (>1 mm) and suffer from long scan times and high radiation dose even at high NP concentrations, mainly due to low efficiency and poor signal-to-noise ratio. We have developed a laboratory XFCT system with high spatial resolution (sub-100 μm), low NP concentration and vastly decreased scan times and dose, opening up the possibilities for in-vivo small-animal imaging research. The system consists of a high-brightness liquid-metal-jet microfocus x-ray source, x-ray focusing optics and an energy-resolving photon-counting detector. By using the source's characteristic 24 keV line-emission together with carefully matched molybdenum nanoparticles the Compton background is greatly reduced, increasing the SNR. Each measurement provides information about the spatial distribution and concentration of the Mo nanoparticles. A filtered back-projection method is used to produce the final XFCT image.

X-Rays

MedlinePlus

X-rays are a type of radiation called electromagnetic waves. X-ray imaging creates pictures of the inside of ... different amounts of radiation. Calcium in bones absorbs x-rays the most, so bones look white. Fat ...

X-ray intensity and source size characterizations for the 25 kV upgraded Manson source at Sandia National Laboratories

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

Loisel, G., E-mail: gploise@sandia.gov; Lake, P.; Gard, P.

2016-11-15

At Sandia National Laboratories, the x-ray generator Manson source model 5 was upgraded from 10 to 25 kV. The purpose of the upgrade is to drive higher characteristics photon energies with higher throughput. In this work we present characterization studies for the source size and the x-ray intensity when varying the source voltage for a series of K-, L-, and M-shell lines emitted from Al, Y, and Au elements composing the anode. We used a 2-pinhole camera to measure the source size and an energy dispersive detector to monitor the spectral content and intensity of the x-ray source. As themore » voltage increases, the source size is significantly reduced and line intensity is increased for the three materials. We can take advantage of the smaller source size and higher source throughput to effectively calibrate the suite of Z Pulsed Power Facility crystal spectrometers.« less

Laboratory Measurements of Solar-Wind/Comet X-Ray Emission and Charge Exchange Cross Sections

NASA Technical Reports Server (NTRS)

Chutjian, A.; Cadez, I.; Greenwood, J. B.; Mawhorter, R. J.; Smith, S. J.; Lozano, J.

2002-01-01

The detection of X-rays from comets such as Hyakutake, Hale-Bopp, d Arrest, and Linear as they approach the Sun has been unexpected and exciting. This phenomenon, moreover, should be quite general, occurring wherever a fast solar or stellar wind interacts with neutrals in a comet, a planetary atmosphere, or a circumstellar cloud. The process is, O(+8) + H2O --> O(+7*) + H2O(+), where the excited O(+7*) ions are the source of the X-ray emissions. Detailed modeling has been carried out of X-ray emissions in charge-transfer collisions of heavy solar-wind Highly Charged Ions (HCIs) and interstellar/interplanetary neutral clouds. In the interplanetary medium the solar wind ions, including protons, can charge exchange with interstellar H and He. This can give rise to a soft X-ray background that could be correlated with the long-term enhancements seen in the low-energy X-ray spectrum of ROSAT. Approximately 40% of the soft X-ray background detected by Exosat, ROSAT, Chandra, etc. is due to Charge Exchange (CXE): our whole heliosphere is glowing in the soft X-ray due to CXE.

Defect Control of the WC Hardmetal by Mixing Recycled WC Nano Powder and Tungsten Powder

NASA Astrophysics Data System (ADS)

Hur, Man Gyu; Shin, Mi Kyung; Kim, Deug Joong; Yoon, Dae Ho

2018-03-01

Tungsten metal powder was added to recycled WC nano powder to control the macro and micro defects of WC hardmetal. The macro and micro defects caused by the excess carbon in the recycled WC powder were markedly removed after the addition of tungsten metal powder ranging from 2 to 6 wt%. The density and hardness of the WC hardmetals also increased due to the removal of defects after adding the tungsten metal powder. The density and hardness of WC hardmetals with the addition of W metal powder ranged from 8 to 12 wt% increased linearly as the W metal powder content increased due to the formation of a new (Co- and W-rich WC) composition. The surface morphology of the WC hardmetals was observed via field emission scanning electron microscopy, and a quantitative elemental analysis was conducted via X-ray fluorescence spectrometry and energy dispersive X-ray analysis. The density and hardness of the WC hardmetals were respectively measured using an analytical balance and a Vikers hardness tester. The effect on the defects in the recycled WC hardmetals through the addition of the tungsten metal powder was discussed in detail.

A wavelet transform algorithm for peak detection and application to powder x-ray diffraction data.

PubMed

Gregoire, John M; Dale, Darren; van Dover, R Bruce

2011-01-01

Peak detection is ubiquitous in the analysis of spectral data. While many noise-filtering algorithms and peak identification algorithms have been developed, recent work [P. Du, W. Kibbe, and S. Lin, Bioinformatics 22, 2059 (2006); A. Wee, D. Grayden, Y. Zhu, K. Petkovic-Duran, and D. Smith, Electrophoresis 29, 4215 (2008)] has demonstrated that both of these tasks are efficiently performed through analysis of the wavelet transform of the data. In this paper, we present a wavelet-based peak detection algorithm with user-defined parameters that can be readily applied to the application of any spectral data. Particular attention is given to the algorithm's resolution of overlapping peaks. The algorithm is implemented for the analysis of powder diffraction data, and successful detection of Bragg peaks is demonstrated for both low signal-to-noise data from theta-theta diffraction of nanoparticles and combinatorial x-ray diffraction data from a composition spread thin film. These datasets have different types of background signals which are effectively removed in the wavelet-based method, and the results demonstrate that the algorithm provides a robust method for automated peak detection.

Small angle x-ray scattering with edge-illumination

NASA Astrophysics Data System (ADS)

Modregger, Peter; Cremona, Tiziana P.; Benarafa, Charaf; Schittny, Johannes C.; Olivo, Alessandro; Endrizzi, Marco

2016-08-01

Sensitivity to sub-pixel sample features has been demonstrated as a valuable capability of phase contrast x-ray imaging. Here, we report on a method to obtain angular-resolved small angle x-ray scattering distributions with edge-illumination- based imaging utilizing incoherent illumination from an x-ray tube. Our approach provides both the three established image modalities (absorption, differential phase and scatter strength), plus a number of additional contrasts related to unresolved sample features. The complementarity of these contrasts is experimentally validated by using different materials in powder form. As a significant application example we show that the extended complementary contrasts could allow the diagnosis of pulmonary emphysema in a murine model. In support of this, we demonstrate that the properties of the retrieved scattering distributions are consistent with the expectation of increased feature sizes related to pulmonary emphysema. Combined with the simplicity of implementation of edge-illumination, these findings suggest a high potential for exploiting extended sub-pixel contrasts in the diagnosis of lung diseases and beyond.

Laboratory Scale X-ray Fluorescence Tomography: Instrument Characterization and Application in Earth and Environmental Science.

PubMed

Laforce, Brecht; Vermeulen, Bram; Garrevoet, Jan; Vekemans, Bart; Van Hoorebeke, Luc; Janssen, Colin; Vincze, Laszlo

2016-03-15

A new laboratory scale X-ray fluorescence (XRF) imaging instrument, based on an X-ray microfocus tube equipped with a monocapillary optic, has been developed to perform XRF computed tomography experiments with both higher spatial resolution (20 μm) and a better energy resolution (130 eV @Mn-K(α)) than has been achieved up-to-now. This instrument opens a new range of possible applications for XRF-CT. Next to the analytical characterization of the setup by using well-defined model/reference samples, demonstrating its capabilities for tomographic imaging, the XRF-CT microprobe has been used to image the interior of an ecotoxicological model organism, Americamysis bahia. This had been exposed to elevated metal (Cu and Ni) concentrations. The technique allowed the visualization of the accumulation sites of copper, clearly indicating the affected organs, i.e. either the gastric system or the hepatopancreas. As another illustrative application, the scanner has been employed to investigate goethite spherules from the Cretaceous-Paleogene boundary, revealing the internal elemental distribution of these valuable distal ejecta layer particles.

Fabrication of imaging X-ray optics

NASA Astrophysics Data System (ADS)

Catura, R. C.; Joki, E. G.; Brookover, W. J.

The design, fabrication, and performance of optics for X-ray astronomy and laboratory applications are described and illustrated with diagrams, drawings, graphs, photographs, and sample images. Particular attention is given to the Wolter I telescope developed for spectroscopic observation of 8-30-A cosmic X-ray sources from a rocketborne X-ray Objective Grating Spectrometer; this instrument employs three nested paraboloid-hyperboloid mirrors of 5083 Al alloy, figured by diamond turning and covered with a thin coating of acrylic lacquer prior to deposition of a 40-nm-thick layer of Sn. In calibration tests at NASA Marshall, the FWHM of the line-spread function at 1.33 nm was found to be 240 microns, corresponding to 21 arcsec. Also presented are the results of reflectivity measurements on C and W multilayers sputtered on Si and fusion glass substrates.

Performance of the PRAXyS X-Ray Polarimeter

NASA Technical Reports Server (NTRS)

Iwakiri, W. B.; Black, J. K.; Cole, R.; Enoto, T.; Hayato, A.; Hill, J. E.; Jahoda, Keith M.; Kaaret, P.; Kitaguchi, T.; Kubota, M.

2016-01-01

The performance of the Time Projection Chamber (TPC) polarimeter for the Polarimeter for Relativistic Astrophysical X-ray Sources (PRAXyS) Small Explorer was evaluated using polarized and unpolarized X-ray sources. The PRAXyS mission will enable exploration of the universe through X-ray polarimetry in the 2-10 keV energy band. We carried out performance tests of the polarimeter at the Brookhaven National Laboratory, National Synchrotron Light Source (BNL-NSLS) and at NASA's Goddard Space Flight Center. The polarimeter was tested with linearly polarized, monochromatic X-rays at 11 different energies between 2.5 and 8.0 keV. At maximum sensitivity, the measured modulation factors at 2.7, 4.5 and 8.0 keV are 27%, 43% and 59%, respectively and the measured angle of polarization is consistent with the expected value at all energies. Measurements with a broadband, unpolarized X-ray source placed a limit of less than 1% on false polarization in the PRAXyS polarimeter.

Performance of the PRAXyS X-ray polarimeter

NASA Astrophysics Data System (ADS)

Iwakiri, W. B.; Black, J. K.; Cole, R.; Enoto, T.; Hayato, A.; Hill, J. E.; Jahoda, K.; Kaaret, P.; Kitaguchi, T.; Kubota, M.; Marlowe, H.; McCurdy, R.; Takeuchi, Y.; Tamagawa, T.

2016-12-01

The performance of the Time Projection Chamber (TPC) polarimeter for the Polarimeter for Relativistic Astrophysical X-ray Sources (PRAXyS) Small Explorer was evaluated using polarized and unpolarized X-ray sources. The PRAXyS mission will enable exploration of the universe through X-ray polarimetry in the 2-10 keV energy band. We carried out performance tests of the polarimeter at the Brookhaven National Laboratory, National Synchrotron Light Source (BNL-NSLS) and at NASA's Goddard Space Flight Center. The polarimeter was tested with linearly polarized, monochromatic X-rays at 11 different energies between 2.5 and 8.0 keV. At maximum sensitivity, the measured modulation factors at 2.7, 4.5 and 8.0 keV are 27%, 43% and 59%, respectively and the measured angle of polarization is consistent with the expected value at all energies. Measurements with a broadband, unpolarized X-ray source placed a limit of less than 1% on false polarization in the PRAXyS polarimeter.

Testing the limits of sensitivity in a solid-state structural investigation by combined X-ray powder diffraction, solid-state NMR, and molecular modelling.

PubMed

Filip, Xenia; Borodi, Gheorghe; Filip, Claudiu

2011-10-28

A solid state structural investigation of ethoxzolamide is performed on microcrystalline powder by using a multi-technique approach that combines X-ray powder diffraction (XRPD) data analysis based on direct space methods with information from (13)C((15)N) solid-state Nuclear Magnetic Resonance (SS-NMR) and molecular modeling. Quantum chemical computations of the crystal were employed for geometry optimization and chemical shift calculations based on the Gauge Including Projector Augmented-Wave (GIPAW) method, whereas a systematic search in the conformational space was performed on the isolated molecule using a molecular mechanics (MM) approach. The applied methodology proved useful for: (i) removing ambiguities in the XRPD crystal structure determination process and further refining the derived structure solutions, and (ii) getting important insights into the relationship between the complex network of non-covalent interactions and the induced supra-molecular architectures/crystal packing patterns. It was found that ethoxzolamide provides an ideal case study for testing the accuracy with which this methodology allows to distinguish between various structural features emerging from the analysis of the powder diffraction data. This journal is © the Owner Societies 2011

Design Considerations of a Virtual Laboratory for Advanced X-ray Sources

NASA Astrophysics Data System (ADS)

Luginsland, J. W.; Frese, M. H.; Frese, S. D.; Watrous, J. J.; Heileman, G. L.

2004-11-01

The field of scientific computation has greatly advanced in the last few years, resulting in the ability to perform complex computer simulations that can predict the performance of real-world experiments in a number of fields of study. Among the forces driving this new computational capability is the advent of parallel algorithms, allowing calculations in three-dimensional space with realistic time scales. Electromagnetic radiation sources driven by high-voltage, high-current electron beams offer an area to further push the state-of-the-art in high fidelity, first-principles simulation tools. The physics of these x-ray sources combine kinetic plasma physics (electron beams) with dense fluid-like plasma physics (anode plasmas) and x-ray generation (bremsstrahlung). There are a number of mature techniques and software packages for dealing with the individual aspects of these sources, such as Particle-In-Cell (PIC), Magneto-Hydrodynamics (MHD), and radiation transport codes. The current effort is focused on developing an object-oriented software environment using the Rational© Unified Process and the Unified Modeling Language (UML) to provide a framework where multiple 3D parallel physics packages, such as a PIC code (ICEPIC), a MHD code (MACH), and a x-ray transport code (ITS) can co-exist in a system-of-systems approach to modeling advanced x-ray sources. Initial software design and assessments of the various physics algorithms' fidelity will be presented.

High-resolution short-exposure small-animal laboratory x-ray phase-contrast tomography

NASA Astrophysics Data System (ADS)

Larsson, Daniel H.; Vågberg, William; Yaroshenko, Andre; Yildirim, Ali Önder; Hertz, Hans M.

2016-12-01

X-ray computed tomography of small animals and their organs is an essential tool in basic and preclinical biomedical research. In both phase-contrast and absorption tomography high spatial resolution and short exposure times are of key importance. However, the observable spatial resolutions and achievable exposure times are presently limited by system parameters rather than more fundamental constraints like, e.g., dose. Here we demonstrate laboratory tomography with few-ten μm spatial resolution and few-minute exposure time at an acceptable dose for small-animal imaging, both with absorption contrast and phase contrast. The method relies on a magnifying imaging scheme in combination with a high-power small-spot liquid-metal-jet electron-impact source. The tomographic imaging is demonstrated on intact mouse, phantoms and excised lungs, both healthy and with pulmonary emphysema.

XAP, a program for deconvolution and analysis of complex X-ray spectra

USGS Publications Warehouse

Quick, James E.; Haleby, Abdul Malik

1989-01-01

The X-ray analysis program (XAP) is a spectral-deconvolution program written in BASIC and specifically designed to analyze complex spectra produced by energy-dispersive X-ray analytical systems (EDS). XAP compensates for spectrometer drift, utilizes digital filtering to remove background from spectra, and solves for element abundances by least-squares, multiple-regression analysis. Rather than base analyses on only a few channels, broad spectral regions of a sample are reconstructed from standard reference spectra. The effects of this approach are (1) elimination of tedious spectrometer adjustments, (2) removal of background independent of sample composition, and (3) automatic correction for peak overlaps. Although the program was written specifically to operate a KEVEX 7000 X-ray fluorescence analytical system, it could be adapted (with minor modifications) to analyze spectra produced by scanning electron microscopes, electron microprobes, and probes, and X-ray defractometer patterns obtained from whole-rock powders.

Cation ordering/disordering kinetics in Ba3CoNb2O9: An in situ study using synchrotron x-ray powder diffraction

NASA Astrophysics Data System (ADS)

Mallinson, P. M.; Claridge, J. B.; Rosseinsky, M. J.; Ibberson, R. M.; Wright, J. P.; Fitch, A. N.; Price, T.; Iddles, D. M.

2007-11-01

In situ synchrotron x-ray powder diffraction has been used to study the kinetics of cation ordering and disordering in the microwave dielectric electroceramic Ba3CoNb2O9 with a time resolution of 15s. The method enables the order/disorder temperature (To /d) in this material of 1430°C to be directly observed. The changes in the rate and degree of cation ordering and in the growth of ordered domains between samples ordered from standard precursor material and then subsequently reordered following an annealing period above To /d show that small changes in precursor order state and phase assemblage strongly influence the final domain size.

X-ray Pulsar Navigation Algorithms and Testbed for SEXTANT

NASA Technical Reports Server (NTRS)

Winternitz, Luke M. B.; Hasouneh, Monther A.; Mitchell, Jason W.; Valdez, Jennifer E.; Price, Samuel R.; Semper, Sean R.; Yu, Wayne H.; Ray, Paul S.; Wood, Kent S.; Arzoumanian, Zaven;

Final Report on X-ray Yields from OMEGA II Targets

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

Fournier, K B; May, M J; MacLaren, S A

2007-06-20

We present details about X-ray yields measured with Lawrence Livermore National Laboratory (LLNL) and Sandia National Laboratories (SNL) diagnostics in soft and moderately hard X-ray bands from laser-driven, doped-aerogel targets shot on 07/14/06 during the OMEGA II test series. Yields accurate to {+-}25% in the 5-15 keV band are measured with Livermore's HENWAY spectrometer. Yields in the sub-keV to 3.2 keV band are measured with LLNL's DANTE diagnostic, the DANTE yields are accurate to 10-15%. SNL ran a PCD-based diagnostic that also measured X-ray yields in the spectral region above 4 keV, and also down to the sub-keV range. Themore » PCD and HENWAY and DANTE numbers are compared. The time histories of the moderately hard (h{nu} > 4 keV) X-ray signals are measured with LLNL's H11 PCD, and from two SNL PCDs with comparable filtration. There is general agreement between the H11 PCD and SNL PCD measured FWHM except for two of the shorter-laser-pulse shots, which is shown not to be due to analysis techniques. The recommended X-ray waveform is that from the SNL PCD p66k10, which was recorded on a fast, high-bandwidth TDS 6804 oscilloscope. X-ray waveforms from target emission in two softer spectral bands are also shown; the X-ray emissions have increasing duration as the spectral content gets softer.« less

Atomic Data in X-Ray Astrophysics

NASA Technical Reports Server (NTRS)

Brickhouse, N. S.

2000-01-01

With the launches of the Chandra X-ray Observatory (CXO) and the X-ray Multimirror Mission (XMM) and the upcoming launch of the Japanese mission ASTRO-E, high resolution X-ray spectroscopy of cosmic sources has begun. Early, deep observations of three stellar coronal sources will provide not only invaluable calibration data, but will also give us benchmarks for the atomic data under collisional equilibrium conditions. Analysis of the Chandra X-ray Observatory data, and data from other telescopes taken simultaneously, for these stars is ongoing as part of the Emission Line Project. Goals of the Emission Line Project are: (1) to determine and verify accurate and robust diagnostics and (2) to identify and prioritize issues in fundamental spectroscopy which will require further theoretical and/or laboratory work. The Astrophysical Plasma Emission Database will be described in some detail, as it is introducing standardization and flexibility into X-ray spectral modeling. Spectral models of X-ray astrophysical plasmas can be generally classified as dominated by either collisional ionization or by X-ray photoionization. While the atomic data needs for spectral models under these two types of ionization are significantly different, there axe overlapping data needs, as I will describe. Early results from the Emission Line Project benchmarks are providing an invaluable starting place, but continuing work to improve the accuracy and completeness of atomic data is needed. Additionally, we consider the possibility that some sources will require that both collisional ionization and photoionization be taken into account, or that time-dependent ionization be considered. Thus plasma spectral models of general use need to be computed over a wide range of physical conditions.

From Relativistic Electrons to X-ray Phase Contrast Imaging

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

Lumpkin, A. H.; Garson, A. B.; Anastasio, M. A.

2017-10-09

We report the initial demonstrations of the use of single crystals in indirect x-ray imaging for x-ray phase contrast imaging at the Washington University in St. Louis Computational Bioimaging Laboratory (CBL). Based on single Gaussian peak fits to the x-ray images, we observed a four times smaller system point spread function (21 μm (FWHM)) with the 25-mm diameter single crystals than the reference polycrystalline phosphor’s 80-μm value. Potential fiber-optic plate depth-of-focus aspects and 33-μm diameter carbon fiber imaging are also addressed.

Ellipsoidal and parabolic glass capillaries as condensers for x-ray microscopes.

PubMed

Zeng, Xianghui; Duewer, Fred; Feser, Michael; Huang, Carson; Lyon, Alan; Tkachuk, Andrei; Yun, Wenbing

2008-05-01

Single-bounce ellipsoidal and paraboloidal glass capillary focusing optics have been fabricated for use as condenser lenses for both synchrotron and tabletop x-ray microscopes in the x-ray energy range of 2.5-18 keV. The condenser numerical apertures (NAs) of these devices are designed to match the NA of x-ray zone plate objectives, which gives them a great advantage over zone plate condensers in laboratory microscopes. The fabricated condensers have slope errors as low as 20 murad rms. These capillaries provide a uniform hollow-cone illumination with almost full focusing efficiency, which is much higher than what is available with zone plate condensers. Sub-50 nm resolution at 8 keV x-ray energy was achieved by utilizing this high-efficiency condenser in a laboratory microscope based on a rotating anode generator.

Refractive Optics for Hard X-ray Transmission Microscopy

NASA Astrophysics Data System (ADS)

Simon, M.; Ahrens, G.; Last, A.; Mohr, J.; Nazmov, V.; Reznikova, E.; Voigt, A.

2011-09-01

For hard x-ray transmission microscopy at photon energies higher than 15 keV we design refractive condenser and imaging elements to be used with synchrotron light sources as well as with x-ray tube sources. The condenser lenses are optimized for low x-ray attenuation—resulting in apertures greater than 1 mm—and homogeneous intensity distribution on the detector plane, whereas the imaging enables high-resolution (<100 nm) full-field imaging. To obtain high image quality at reasonable exposure times, custom-tailored matched pairs of condenser and imaging lenses are being developed. The imaging lenses (compound refractive lenses, CRLs) are made of SU-8 negative resist by deep x-ray lithography. SU-8 shows high radiation stability. The fabrication technique enables high-quality lens structures regarding surface roughness and arrangement precision with arbitrary 2D geometry. To provide point foci, crossed pairs of lenses are used. Condenser lenses have been made utilizing deep x-ray lithographic patterning of thick SU-8 layers, too, whereas in this case, the aperture is limited due to process restrictions. Thus, in terms of large apertures, condenser lenses made of structured and rolled polyimide film are more attractive. Both condenser types, x-ray mosaic lenses and rolled x-ray prism lenses (RXPLs), are considered to be implemented into a microscope setup. The x-ray optical elements mentioned above are characterized with synchrotron radiation and x-ray laboratory sources, respectively.

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

The Imaging X-ray Polarimetry Explorer (IXPE)

NASA Astrophysics Data System (ADS)

Weisskopf, Martin C.; Ramsey, Brian; O'Dell, Stephen; Tennant, Allyn; Elsner, Ronald; Soffitta, Paolo; Bellazzini, Ronaldo; Costa, Enrico; Kolodziejczak, Jeffrey; Kaspi, Victoria; Muleri, Fabio; Marshall, Herman; Matt, Giorgio; Romani, Roger

2016-07-01

The Imaging X-ray Polarimetry Explorer (IXPE) expands observation space by simultaneously adding polarization measurements to the array of source properties currently measured (energy, time, and location). IXPE will thus open new dimensions for understanding how X-ray emission is produced in astrophysical objects, especially systems under extreme physical conditions—such as neutron stars and black holes. Polarization singularly probes physical anisotropies—ordered magnetic fields, aspheric matter distributions, or general relativistic coupling to black-hole spin—that are not otherwise measurable. Hence, IXPE complements all other investigations in high-energy astrophysics by adding important and relatively unexplored information to the parameter space for studying cosmic X-ray sources and processes, as well as for using extreme astrophysical environments as laboratories for fundamental physics.

Titration of a Solid Acid Monitored by X-Ray Diffraction

ERIC Educational Resources Information Center

Dungey, Keenan E.; Epstein, Paul

2007-01-01

An experiment is described to introduce students to an important class of solid-state reactions while reinforcing concepts of titration by using a pH meter and a powder X-ray diffractometer. The experiment was successful in teaching students the abstract concepts of solid-state structure and diffraction by applying the diffraction concepts learned…

Copper doped TiO2 nanoparticles characterized by X-ray absorption spectroscopy, total scattering, and powder diffraction--a benchmark structure-property study.

PubMed

Lock, Nina; Jensen, Ellen M L; Mi, Jianli; Mamakhel, Aref; Norén, Katarina; Qingbo, Meng; Iversen, Bo B

2013-07-14

Metal functionalized nanoparticles potentially have improved properties e.g. in catalytic applications, but their precise structures are often very challenging to determine. Here we report a structural benchmark study based on tetragonal anatase TiO2 nanoparticles containing 0-2 wt% copper. The particles were synthesized by continuous flow synthesis under supercritical water-isopropanol conditions. Size determination using synchrotron PXRD, TEM, and X-ray total scattering reveals 5-7 nm monodisperse particles. The precise dopant structure and thermal stability of the highly crystalline powders were characterized by X-ray absorption spectroscopy and multi-temperature synchrotron PXRD (300-1000 K). The combined evidence reveals that copper is present as a dopant on the particle surfaces, most likely in an amorphous oxide or hydroxide shell. UV-VIS spectroscopy shows that copper presence at concentrations higher than 0.3 wt% lowers the band gap energy. The particles are unaffected by heating to 600 K, while growth and partial transformation to rutile TiO2 occur at higher temperatures. Anisotropic unit cell behavior of anatase is observed as a consequence of the particle growth (a decreases and c increases).

LABORATORY EVALUATION OF SIX NEW/MODIFIED PORTABLE X-RAY FLUORESCENCE SPECTROMETERS FOR THE MEASUREMENT OF LEAD IN CHARACTERIZED PAINT FILMS AND RESEARCH MATERIAL BOARDS (APPENDICES)

EPA Science Inventory

A laboratory study was performed in 1994-1995 to identify and estimate the influence of key characteristics for evaluating the performance of portable X-ray fluorescence (XRF) spectrometers. Six new/modified spectrometers, including HNU SEFA-Pb, Metorex X-MET, Niton X-L, Radiat...

Laboratory Simulation of Frozen Methanol Under X-ray Radiation Field: Relevancies to Astrophysical Ices

NASA Astrophysics Data System (ADS)

Andrade, Diana; Rocco, Maria Luiza M.; Boechat-Roberty, Heloisa Maria

The origin of complex organic molecules detected in comets, meteorites, star-forming regions and other environments are currently subject of discussion. Depending on the environment, it is dominated by X-rays, UV photons as well as by charged particles, electrons and ions with high or low energies. Every particle will promote a different fragmentation in the molecule and different phenomena in the ice, favoring the formation of an ion species rather than another. To predict the chemical evolution and to quantify the complex organics incorporated into grains or desorbed to the gas phase, it is necessary to establish the main formation route, which can be tested in the laboratories. In this way, the study of the effects of different ionization agents on the ices becomes crucial. Methanol (CH3 OH), the simplest organic alcohol, is an important precursor of more complex prebiotic species and is found abundantly in icy mantles on interstellar and protostellar dust grains. This molecule has been detected through infrared spectroscopy in some astrophysics environments as W33A and RAFGL 7009. Additionally, methanol has been found in comets, as Hale-Bopp, and other solar system bodies, such as the centaur 5145 Pholus. All of these astronomical environments are subjected to some form of ionizing agents such as cosmic rays, electrons and photons (e.g. stellar radiation field). In this work, synchrotron radiation from the Brazilian Synchrotron Light Laboratory at the O 1s-edge was employed to perform desorption experiments on the frozen methanol. The desorp-tion rates (desorbed ion per incident photon) of the most intense ions desorbed from methanol due soft X-ray bombardment are estimated. The desorption rates are critical parameters for modeling the chemistry of interstellar clouds. Moreover, a comparison among our results and literature using different ionization agents and different phases (photons at 292 eV and elec-trons at 70 eV in gaseous phase and heavy ions around 65

A Compact X-Ray System for Support of High Throughput Crystallography

NASA Technical Reports Server (NTRS)

Ciszak, Ewa; Gubarev, Mikhail; Gibson, Walter M.; Joy, Marshall K.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

Standard x-ray systems for crystallography rely on massive generators coupled with optics that guide X-ray beams onto the crystal sample. Optics for single-crystal diffractometry include total reflection mirrors, polycapillary optics or graded multilayer monochromators. The benefit of using polycapillary optic is that it can collect x-rays over tile greatest solid angle, and thus most efficiently, utilize the greatest portion of X-rays emitted from the Source, The x-ray generator has to have a small anode spot, and thus its size and power requirements can be substantially reduced We present the design and results from the first high flux x-ray system for crystallography that combine's a microfocus X-ray generator (40microns FWHM Spot size at a power of 45 W) and a collimating, polycapillary optic. Diffraction data collected from small test crystals with cell dimensions up to 160A (lysozyme and thaumatin) are of high quality. For example, diffraction data collected from a lysozyme crystal at RT yielded R=5.0% for data extending to 1.70A. We compare these results with measurements taken from standard crystallographic systems. Our current microfocus X-ray diffraction system is attractive for supporting crystal growth research in the standard crystallography laboratory as well as in remote, automated crystal growth laboratory. Its small volume, light-weight, and low power requirements are sufficient to have it installed in unique environments, i.e.. on-board International Space Station.

X-ray beamsplitter

DOEpatents

Ceglio, Natale M.; Stearns, Daniel S.; Hawryluk, Andrew M.; Barbee, Jr., Troy W.

1989-01-01

An x-ray beamsplitter which splits an x-ray beam into two coherent parts by reflecting and transmitting some fraction of an incident beam has applications for x-ray interferometry, x-ray holography, x-ray beam manipulation, and x-ray laser cavity output couplers. The beamsplitter is formed of a wavelength selective multilayer thin film supported by a very thin x-ray transparent membrane. The beamsplitter resonantly transmits and reflects x-rays through thin film interference effects. A thin film is formed of 5-50 pairs of alternate Mo/Si layers with a period of 20-250 A. The support membrane is 10-200 nm of silicon nitride or boron nitride. The multilayer/support membrane structure is formed across a window in a substrate by first forming the structure on a solid substrate and then forming a window in the substrate to leave a free-standing structure over the window.

Search for Hard X-Ray Emission from the Soft X-Ray Transient Aquila X-1

NASA Astrophysics Data System (ADS)

Harmon, B. A.; Zhang, S. N.; Paciesas, W. S.; Tavani, M.; Kaaret, P.; Ford, E.

1994-12-01

We are investigating the possibility of hard x-ray emission from the recurrent soft x-ray transient and x-ray burst source Aquila X-1 (Aql X-1). Outbursts of this source are relatively frequent with a spacing of ~ 4-10 months (Kitamoto, S. et al. 1993, ApJ, 403, 315). The recent detections of hard tails (\\(>\\)20 keV) in low luminosity x-ray bursters (Barret, D. & Vedrenne, G. 1994, ApJ Supp. S. 92, 505) suggest that neutron star transient systems such as Aql X-1 can produce hard x-ray emission which is detectable by BATSE. We are correlating reported optical and soft x-ray observations since 1991 of Aql X-1 with BATSE observations in order to search for hard x-ray emission episodes, and to study their temporal and spectral evolution. We will present preliminary results of this search in the 20-1000 keV band using the Earth occultation technique applied to the large area detectors. If this work is successful, we hope to alert the astronomical community for the next Aql X-1 outburst expected in 1995. Simultaneous x-ray/hard x-ray and optical observations of Aql X-1 during outburst would be of great importance for the modeling of soft x-ray transients and related systems.

Use of capillary optics as a beam intensifier for a Compton x-ray source.

PubMed

Tompkins, P A; Abreu, C C; Carroll, F E; Xiao, Q F; MacDonald, C A

1994-11-01

The use of Kumakhov capillary optics will significantly enhance the performance of near-monochromatic, Compton backscattered x-ray programs. The Vanderbilt University Medical Free-Electron Laser Center is developing the capability to create these tunable x rays for medical imaging. The present transport has only reflection optics, and the beam is quite large in diameter at the laboratory. Low loss collimation of this beam would allow higher x-ray intensities after transport. This article describes experimental and computer simulation results which predict the expected performance for a multifiber Kumakhov collimator for use in the x-ray beam transport. Estimates from our research are that a multifiber optic formed of individual polycapillary fibers could be used to capture the full 7 mrad of the Vanderbilt x-ray beam and collimate it to a 1-2 mrad divergence with approximately 40%-50% transmission efficiency. This optic should increase the x-ray intensity at the laboratory level by a factor of > or = 5 by decreasing the beam divergence and subsequent spot size. Additionally, analysis of monolithic optics of fused multicapillary fibers predicts an increase in the intensity of the x rays at the laboratory by a factor of 55. These optics can have tapered channels that greatly decrease their exit divergence. This will greatly enhance the capabilities of this unique x-ray source. This article reports the initial results from a collaboration between Vanderbilt, The Center for X-Ray Optics at University at Albany, SUNY, and X-Ray Optical Systems in Albany, NY.

Talbot-Lau x-ray interferometry for high energy density plasma diagnostic.

PubMed

Stutman, D; Finkenthal, M

2011-11-01

High resolution density diagnostics are difficult in high energy density laboratory plasmas (HEDLP) experiments due to the scarcity of probes that can penetrate above solid density plasmas. Hard x-rays are one possible probe for such dense plasmas. We study the possibility of applying an x-ray method recently developed for medical imaging, differential phase-contrast with Talbot-Lau interferometers, for the diagnostic of electron density and small-scale hydrodynamic instabilities in HEDLP experiments. The Talbot method uses micro-periodic gratings to measure the refraction and ultra-small angle scatter of x-rays through an object and is attractive for HEDLP diagnostic due to its capability to work with incoherent and polychromatic x-ray sources such as the laser driven backlighters used for HEDLP radiography. Our paper studies the potential of the Talbot method for HEDLP diagnostic, its adaptation to the HEDLP environment, and its extension of high x-ray energy using micro-periodic mirrors. The analysis is illustrated with experimental results obtained using a laboratory Talbot interferometer. © 2011 American Institute of Physics

Buckskin Drill Hole and CheMin X-ray Diffraction

NASA Image and Video Library

2015-12-17

The graph at right presents information from the NASA Curiosity Mars rover's onboard analysis of rock powder drilled from the "Buckskin" target location, shown at left. X-ray diffraction analysis of the Buckskin sample inside the rover's Chemistry and Mineralogy (CheMin) instrument revealed the presence of a silica-containing mineral named tridymite. This is the first detection of tridymite on Mars. Peaks in the X-ray diffraction pattern are from minerals in the sample, and every mineral has a diagnostic set of peaks that allows identification. The image of Buckskin at left was taken by the rover's Mars Hand Lens Imager (MAHLI) camera on July 30, 2015, and is also available at PIA19804. http://photojournal.jpl.nasa.gov/catalog/PIA20271

Small-Size High-Current Generators for X-Ray Backlighting

NASA Astrophysics Data System (ADS)

Chaikovsky, S. A.; Artyomov, A. P.; Zharova, N. V.; Zhigalin, A. S.; Lavrinovich, I. V.; Oreshkin, V. I.; Ratakhin, N. A.; Rousskikh, A. G.; Fedunin, A. V.; Fedushchak, V. F.; Erfort, A. A.

2017-12-01

The paper deals with the soft X-ray backlighting based on the X-pinch as a powerful tool for physical studies of fast processes. Proposed are the unique small-size pulsed power generators operating as a low-inductance capacitor bank. These pulse generators provide the X-pinch-based soft X-ray source (hν = 1-10 keV) of micron size at 2-3 ns pulse duration. The small size and weight of pulse generators allow them to be transported to any laboratory for conducting X-ray backlighting of test objects with micron space resolution and nanosecond exposure time. These generators also allow creating synchronized multi-frame radiographic complexes with frame delay variation in a broad range.

X-ray beamsplitter

DOEpatents

Ceglio, N.M.; Stearns, D.G.; Hawryluk, A.M.; Barbee, T.W. Jr.

1987-08-07

An x-ray beamsplitter which splits an x-ray beam into two coherent parts by reflecting and transmitting some fraction of an incident beam has applications for x-ray interferometry, x-ray holography, x-ray beam manipulation, and x-ray laser cavity output couplers. The beamsplitter is formed of a wavelength selective multilayer thin film supported by a very thin x-ray transparent membrane. The beamsplitter resonantly transmits and reflects x-rays through thin film interference effects. A thin film is formed of 5--50 pairs of alternate Mo/Si layers with a period of 20--250 A. The support membrane is 10--200 nm of silicon nitride or boron nitride. The multilayer/support membrane structure is formed across a window in a substrate by first forming the structure on a solid substrate and then forming a window in the substrate to leave a free-standing structure over the window. 6 figs.

Simulating x-ray telescopes with McXtrace: a case study of ATHENA's optics

NASA Astrophysics Data System (ADS)

Ferreira, Desiree D. M.; Knudsen, Erik B.; Westergaard, Niels J.; Christensen, Finn E.; Massahi, Sonny; Shortt, Brian; Spiga, Daniele; Solstad, Mathias; Lefmann, Kim

2016-07-01

We use the X-ray ray-tracing package McXtrace to simulate the performance of X-ray telescopes based on Silicon Pore Optics (SPO) technologies. We use as reference the design of the optics of the planned X-ray mission Advanced Telescope for High ENergy Astrophysics (ATHENA) which is designed as a single X-ray telescope populated with stacked SPO substrates forming mirror modules to focus X-ray photons. We show that is possible to simulate in detail the SPO pores and qualify the use of McXtrace for in-depth analysis of in-orbit performance and laboratory X-ray test results.

X-ray Measurements of Laser Irradiated Foam Filled Liners

NASA Astrophysics Data System (ADS)

Patankar, Siddharth; Mariscal, Derek; Goyon, Clement; Baker, Kevin; MacLaren, Stephan; Hammer, Jim; Baumann, Ted; Amendt, Peter; Menapace, Joseph; Berger, Bob; Afeyan, Bedros; Tabak, Max; Dixit, Sham; Kim, Sung Ho; Moody, John; Jones, Ogden

2016-10-01

Low-density foam liners are being investigated as sources of efficient x-rays. Understanding the laser-foam interaction is key to modeling and optimizing foam composition and density for x-ray production with reduced backscatter. We report on the experimental results of laser-irradiated foam liners filled with SiO2 and Ta2O5 foams at densities between 2 to 30mg/cc. The foam liners consist of polyimide tubes filled with low-density foams and sealed with a gold foil at one end. The open end of the tube is driven with 250J of 527nm laser light in a 2ns 2-step pulse using the Jupiter Laser Facility at LLNL. A full aperture backscatter system is used to diagnose the coupled energy and losses. A streaked x-ray camera and filtered x-ray pinhole cameras are used to measure laser penetration into the low-density foam for different mass densities. A HOPG crystal spectrometer is used to estimate a thermal electron temperature. Comparisons with beam propagation and x-ray emission simulations are presented. This work was performed under the auspices of the U.S. Department of Energy by the Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344, with funding support from the Laboratory Directed Research and Development Program under project 15.

Estimation of Crystallinity of Nifedipine-Polyvinylpyrrolidone Solid Dispersion by Usage of Terahertz Time-Domain Spectroscopy and of X-Ray Powder Diffractometer.

PubMed

Takeuchi, Issei; Shimakura, Kemmaro; Kuroda, Hideki; Nakajima, Takehisa; Goto, Satoru; Makino, Kimiko

2015-12-01

Crystalline state of pharmaceutical materials is of great importance in preparation of pharmaceutics, because their physicochemical properties affect bioavailability, quality of products, therapeutic level and manufacturing process. In this study, we have estimated time-dependent changes of nifedipine in nifedipine-polyvinylpyrrolidone (PVP) solid dispersion by measuring terahertz time-domain spectroscopy (THz-TDS) and by X-ray powder diffractometry (XRPD), and compared their correlativity. Crystallinity of nifedipine-PVP solid dispersion was changed by storing the amorphous sample at 25°C-75°C and relative humidity of over 80% for 0.25-24.00 h. To compare the results of two types of measurements, we have used a general method of linear regression analysis. Crystallinities estimated using THz-TDS were plotted on the x-axis and that of XRPD were on the y-axis. From the result of the calculation, the correlativity of them was confirmed. THz-TDS has the capability of becoming the replacement of XRPD. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

[Particle size determination by radioisotope x-ray absorptiometry with sedimentation method].

PubMed

Matsui, Y; Furuta, T; Miyagawa, S

1976-09-01

The possibility of radioisotope X-ray absorptiometry to determine the particle size of powder in conjunction with sedimentation was investigated. The experimental accuracy was primarily determined by Cow and X-ray intensity. where Co'=weight concentration of the particle in the suspension w'=(micron/rho)l/(mu/rho)s-rhol/rhos rho; density micron/rho; mass absorption coefficient, suffix l and s indicate dispersion and particle, respectively. The radiosiotopes, Fe-55, Pu-238 and Cd-109 have high w-values over the wide range of the atomic number. However, a source of high micron value such as Fe-55 is not suitable because the optimal X-ray transmission length, Lopt is decided by the expression, micronlLopt approximately 2/(1+C'ow') by using Cd-109 AgKX-ray source, the weight size distribution of particles from the heavy elements such as PbO2 to light elements such as Al2O3 or flyash was determined.

Two-dimensional single crystal diamond refractive x-ray lens

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

Antipov, S., E-mail: s.antipov@euclidtechlabs.com; Baryshev, S. V.; Butler, J. E.

2016-07-27

The next generation light sources such as diffraction-limited storage rings and high repetition rate x-ray free-electron lasers will generate x-ray beams with significantly increased brilliance. These future machines will require X-ray optical components that are capable of handling higher instantaneous and average power densities while tailoring the properties of the x-ray beams for a variety of scientific experiments. Single crystal diamond is one of the best bulk materials for this application, because it is radiation hard, has a suitable uniform index of refraction and the best available thermal properties. In this paper we report on fabrication and experimental testing ofmore » a two-dimensional (2D) single crystal diamond compound refractive X-ray lenses (CRL). These lenses were manufactured using femto-second laser cutting and tested at the Advanced Photon Source of Argonne National Laboratory.« less

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.

High-resolution short-exposure small-animal laboratory x-ray phase-contrast tomography

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

Larsson, Daniel H.; Vågberg, William; Yaroshenko, Andre

X-ray computed tomography of small animals and their organs is an essential tool in basic and preclinical biomedical research. In both phase-contrast and absorption tomography high spatial resolution and short exposure times are of key importance. However, the observable spatial resolutions and achievable exposure times are presently limited by system parameters rather than more fundamental constraints like, e.g., dose. Here we demonstrate laboratory tomography with few-ten μm spatial resolution and few-minute exposure time at an acceptable dose for small-animal imaging, both with absorption contrast and phase contrast. The method relies on a magnifying imaging scheme in combination with a high-powermore » small-spot liquid-metal-jet electron-impact source. Lastly, the tomographic imaging is demonstrated on intact mouse, phantoms and excised lungs, both healthy and with pulmonary emphysema.« less

High-resolution short-exposure small-animal laboratory x-ray phase-contrast tomography

DOE PAGES

Larsson, Daniel H.; Vågberg, William; Yaroshenko, Andre; ...

2016-12-13

X-ray computed tomography of small animals and their organs is an essential tool in basic and preclinical biomedical research. In both phase-contrast and absorption tomography high spatial resolution and short exposure times are of key importance. However, the observable spatial resolutions and achievable exposure times are presently limited by system parameters rather than more fundamental constraints like, e.g., dose. Here we demonstrate laboratory tomography with few-ten μm spatial resolution and few-minute exposure time at an acceptable dose for small-animal imaging, both with absorption contrast and phase contrast. The method relies on a magnifying imaging scheme in combination with a high-powermore » small-spot liquid-metal-jet electron-impact source. Lastly, the tomographic imaging is demonstrated on intact mouse, phantoms and excised lungs, both healthy and with pulmonary emphysema.« less

X-Ray Optics at NASA Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

O'Dell, Stephen L.; Atkins, Carolyn; Broadway, David M.; Elsner, Ronald F.; Gaskin, Jessica A.; Gubarev, Mikhail V.; Kilaru, Kiranmayee; Kolodziejczak, Jeffery J.; Ramsey, Brian D.; Roche, Jacqueline M.;

Real-time X-ray Diffraction: Applications to Materials Characterization

NASA Technical Reports Server (NTRS)

Rosemeier, R. G.

1984-01-01

With the high speed growth of materials it becomes necessary to develop measuring systems which also have the capabilities of characterizing these materials at high speeds. One of the conventional techniques of characterizing materials was X-ray diffraction. Film, which is the oldest method of recording the X-ray diffraction phenomenon, is not quite adequate in most circumstances to record fast changing events. Even though conventional proportional counters and scintillation counters can provide the speed necessary to record these changing events, they lack the ability to provide image information which may be important in some types of experiment or production arrangements. A selected number of novel applications of using X-ray diffraction to characterize materials in real-time are discussed. Also, device characteristics of some X-ray intensifiers useful in instantaneous X-ray diffraction applications briefly presented. Real-time X-ray diffraction experiments with the incorporation of image X-ray intensification add a new dimension in the characterization of materials. The uses of real-time image intensification in laboratory and production arrangements are quite unlimited and their application depends more upon the ingenuity of the scientist or engineer.

X-Ray Polarization from High Mass X-Ray Binaries

NASA Technical Reports Server (NTRS)

Kallman, T.; Dorodnitsyn, A.; Blondin, J.

2015-01-01

X-ray astronomy allows study of objects which may be associated with compact objects, i.e. neutron stars or black holes, and also may contain strong magnetic fields. Such objects are categorically non-spherical, and likely non-circular when projected on the sky. Polarization allows study of such geometric effects, and X-ray polarimetry is likely to become feasible for a significant number of sources in the future. A class of potential targets for future X-ray polarization observations is the high mass X-ray binaries (HMXBs), which consist of a compact object in orbit with an early type star. In this paper we show that X-ray polarization from HMXBs has a distinct signature which depends on the source inclination and orbital phase. The presence of the X-ray source displaced from the star creates linear polarization even if the primary wind is spherically symmetric whenever the system is viewed away from conjunction. Direct X-rays dilute this polarization whenever the X-ray source is not eclipsed; at mid-eclipse the net polarization is expected to be small or zero if the wind is circularly symmetric around the line of centers. Resonance line scattering increases the scattering fraction, often by large factors, over the energy band spanned by resonance lines. Real winds are not expected to be spherically symmetric, or circularly symmetric around the line of centers, owing to the combined effects of the compact object gravity and ionization on the wind hydrodynamics. A sample calculation shows that this creates polarization fractions ranging up to tens of percent at mid-eclipse.

A laboratory means to produce tough aluminum sheet from powder

NASA Technical Reports Server (NTRS)

Singleton, O. R.; Royster, D. M.; Thomas, J. R.

1990-01-01

The rapid solidification of aluminum alloys as powder and the subsequent fabrication processes can be used to develop and tailor alloys to satisfy specific aerospace design requirements, including high strength and toughness. Laboratory procedures to produce aluminum powder-metallurgy (PM) materials are efficient but require evidence that the laboratory methods used can produce a product with superior properties. This paper describes laboratory equipment and procedures which can be used to produce tough aluminum PM sheet. The processing of a 2124 + 0.9 percent Zr aluminum alloy powder is used as an example. The fully hardened sheet product is evaluated in terms of properties and microstructure. The key features of the vacuum hot press pressing operation used to consolidate the powder are described. The 2124 + 0.9 percent Zr - T8 temper aluminum sheet produced was both strong (460-490 MPa yield strength) and tough (Kahn Tear unit-propagation- energy values over three times those typical for ingot metallurgy 2024-T81). Both the longitudinal and longitudinal-transverse directions of the sheet were tested. The microstructure was well refined with subgrains of one or two micrometers. Fine dispersoids of Al3Zr in the precipitate free regions adjacent to boundaries are believed to contribute to the improved toughness.

16th National School on Neutron and X-ray Scattering

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

Chakoumakos, Bryan; Achilles, Cherie; Cybulskis, Viktor

Students talk about their experience at the 16th National School on Neutron and X-ray Scattering, or NXS 2014. Jointly conducted by Oak Ridge and Argonne national laboratories, NXS immerses graduate students in national user facilities to learn in a hands-on environment how to use neutrons and X-rays in their research.

16th National School on Neutron and X-ray Scattering

ScienceCinema

Chakoumakos, Bryan; Achilles, Cherie; Cybulskis, Viktor; Gilbert, Ian

2018-02-14

Students talk about their experience at the 16th National School on Neutron and X-ray Scattering, or NXS 2014. Jointly conducted by Oak Ridge and Argonne national laboratories, NXS immerses graduate students in national user facilities to learn in a hands-on environment how to use neutrons and X-rays in their research.

X-ray rocking curve measurements of bent crystals. [used in High Resolution Spectrometer in Advanced X-ray Astrophysics Facility

NASA Technical Reports Server (NTRS)

Hakim, M. B.; Muney, W. S.; Fowler, W. B.; Woodgate, B. E.

1988-01-01

A three-crystal laboratory X-ray spectrometer is used to measure the Bragg reflection from concave cylindrically curved crystals to be used in the high-resolution X-ray spectrometer of the NASA Advanced X-ray Astrophysics Facility (AXAF). The first two crystals, in the dispersive (1.1) arrangement, select a narrow collimated monochromatic beam in the Cu K-alpha(1) line at 1.5 A (8.1 keV), which illuminates the test crystal. The angular centroids of rocking curves measured along the surface provide a measure of the conformity of the crystal to the desired radius of curvature. Individual and combined rocking-curve widths and areas provide a measure of the resolution and efficiency at 1.54 A. The crystals analyzed included LiF(200), PET, and acid phthalates such as TAP.

Be/X-ray Binary Science for Future X-ray Timing Missions

NASA Technical Reports Server (NTRS)

Wilson-Hodge, Colleen A.

2011-01-01

For future missions, the Be/X-ray binary community needs to clearly define our science priorities for the future to advocate for their inclusion in future missions. In this talk, I will describe current designs for two potential future missions and Be X-ray binary science enabled by these designs. The Large Observatory For X-ray Timing (LOFT) is an X-ray timing mission selected in February 2011 for the assessment phase from the 2010 ESA M3 call for proposals. The Advanced X-ray Timing ARray (AXTAR) is a NASA explorer concept X-ray timing mission. This talk is intended to initiate discussions of our science priorities for the future.

Abdomen X-Ray (Radiography)

MedlinePlus

... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Abdomen Abdominal x-ray uses a ... of an abdominal x-ray? What is abdominal x-ray? An x-ray (radiograph) is a noninvasive ...

Microwave Kinetic Inductance Detectors: Large Format X-ray Spectral Imagers for the Next Generation of X-ray Telescopes

NASA Astrophysics Data System (ADS)

Eckart, Megan E.; Mazin, B. A.; Bumble, B.; Golwala, S. R.; Zmuidzinas, J.; Day, P. K.; Harrison, F. A.

2006-09-01

Microwave Kinetic Inductance Detectors (MKIDs) have the potential to provide megapixel imagers with few eV spectral resolution for future X-ray missions such as Gen-X. MKIDs offer the advantage over many other cryogenic detector technologies that they can be easily multiplexed, so that arrays with many thousand pixels are readily achievable. In addition, the readout electronics can be operated at room temperature, a significant advantage for space applications. MKIDs exploit the dependence of surface impedance of a superconductorwith the quasiparticle density. Quasiparticles are created by absorption of X-rays, with number proportional to the X-ray energy. The impedance change may be sensitively measured using a thin-film resonant circuit. The practical application of MKIDs for photon detection requires a method of efficiently coupling the photon energy to the MKID. To apply the MKID scheme to X-ray detection we pattern tantalum strips with aluminum MKIDs attached at each end. An incident X-ray is absorbed in the Ta and creates millions of quasiparticle excitations, which diffuse to each end of the strip, finally entering the Al resonators where they are trapped and sensed. Simultaneous monitoring of the signal at both ends of the strip allow position and energy determination for each photon. We have demonstrated working strip detectors in the laboratory, and will present our measurements of the quasiparticle diffusion constant and the quasiparticle lifetime in tantalum, the aluminum quasiparticle lifetime, and the energy resolution of the detector. We will also discuss ideas for future detector designs and suggest ultimate performance goals for X-ray astronomy applications.

LABORATORY EVALUATION OF SIX NEW/MODIFIED PORTABLE X-RAY FLUORESCENCE SPECTROMETERS FOR THE MEASUREMENT OF LEAD IN CHARACTERIZED PAINT FILMS AND RESEARCH MATERIAL BOARDS (TECHNICAL REPORT)

EPA Science Inventory

A laboratory study was performed in 1994-1995 to identify and estimate the influence of key characteristics for evaluating the performance of portable X-ray fluorescence (XRF) spectrometers. Six new/modified spectrometers, including HNU SEFA-Pb, Metorex X-MET, Niton X-L, Radiat...

A search for X-ray polarization in cosmic X-ray sources. [binary X-ray sources and supernovae remnants

NASA Technical Reports Server (NTRS)

Hughes, J. P.; Long, K. S.; Novick, R.

1983-01-01

Fifteen strong X-ray sources were observed by the X-ray polarimeters on board the OSO-8 satellite from 1975 to 1978. The final results of this search for X-ray polarization in cosmic sources are presented in the form of upper limits for the ten sources which are discussed elsewhere. These limits in all cases are consistent with a thermal origin for the X-ray emission.

X-Ray Emission from the Soft X-Ray Transient Aquila X-1

NASA Technical Reports Server (NTRS)

Tavani, Marco

1998-01-01

Aquila X-1 is the most prolific of soft X-ray transients. It is believed to contain a rapidly spinning neutron star sporadically accreting near the Eddington limit from a low-mass companion star. The interest in studying the repeated X-ray outbursts from Aquila X-1 is twofold: (1) studying the relation between optical, soft and hard X-ray emission during the outburst onset, development and decay; (2) relating the spectral component to thermal and non-thermal processes occurring near the magnetosphere and in the boundary layer of a time-variable accretion disk. Our investigation is based on the BATSE monitoring of Aquila X-1 performed by our group. We observed Aquila X-1 in 1997 and re-analyzed archival information obtained in April 1994 during a period of extraordinary outbursting activity of the source in the hard X-ray range. Our results allow, for the first time for this important source, to obtain simultaneous spectral information from 2 keV to 200 keV. A black body (T = 0.8 keV) plus a broken power-law spectrum describe accurately the 1994 spectrum. Substantial hard X-ray emission is evident in the data, confirming that the accretion phase during sub-Eddington limit episodes is capable of producing energetic hard emission near 5 x 10(exp 35) ergs(exp -1). A preliminary paper summarizes our results, and a more comprehensive account is being written. We performed a theoretical analysis of possible emission mechanisms, and confirmed that a non-thermal emission mechanism triggered in a highly sheared magnetosphere at the accretion disk inner boundary can explain the hard X-ray emission. An anticorrelation between soft and hard X-ray emission is indeed prominently observed as predicted by this model.

Quantitative X-ray Differential Interference Contrast Microscopy

NASA Astrophysics Data System (ADS)

Nakamura, Takashi

Full-field soft x-ray microscopes are widely used in many fields of sciences. Advances in nanofabrication technology enabled short wavelength focusing elements with significantly improved spatial resolution. In the soft x-ray spectral region, samples as small as 12 nm can be resolved using micro zone-plates as the objective lens. In addition to conventional x-ray microscopy in which x-ray absorption difference provides the image contrast, phase contrast mechanisms such as differential phase contrast (DIC) and Zernike phase contrast have also been demonstrated These phase contrast imaging mechanisms are especially attractive at the x-ray wavelengths where phase contrast of most materials is typically 10 times stronger than the absorption contrast. With recent progresses in plasma-based x- ray sources and increasing accessibility to synchrotron user facilities, x-ray microscopes are quickly becoming standard measurement equipment in the laboratory. To further the usefulness of x-ray DIC microscopy this thesis explicitly addresses three known issues with this imaging modality by introducing new techniques and devices First, as opposed to its visible-light counterpart, no quantitative phase imaging technique exists for x-ray DIC microscopy. To address this issue, two nanoscale x-ray quantitative phase imaging techniques, using exclusive OR (XOR) patterns and zone-plate doublets, respectively, are proposed. Unlike existing x-ray quantitative phase imaging techniques such as Talbot interferometry and ptychography, no dedicated experimental setups or stringent illumination coherence are needed for quantitative phase retrieval. Second, to the best of our knowledge, no quantitative performance characterization of DIC microscopy exists to date. Therefore the imaging system's response to sample's spatial frequency is not known In order to gain in-depth understanding of this imaging modality, performance of x-ray DIC microscopy is quantified using modulation transfer function

X-ray investigations related to the shock history of the Shergotty achondrite

NASA Technical Reports Server (NTRS)

Horz, F.; Hanss, R.; Serna, C.

1986-01-01

The shock stress suffered by naturally shocked materials from the Shergotty achondrite was studied using X-ray diffraction techniques and experimentally shocked augite and enstatite as standards. The Shergotty pyroxenes revealed the formation of continuous diffraction rings, line broadening, preferred orientation of small scale diffraction domains, and other evidence of substantial lattice disorders. As disclosed by the application of Debye-Scherrer techniques, they are hybrids between single crystals and fine-grained random powders. The pyroxene lattice is very resistant to shock damage on smaller scales. While measurable lattice disaggregation and progressive fragmentation occur below 25 GPa, little additional damage is suffered from application of pressures between 30 to 60 GPa, making pressure calibration of naturally shocked pyroxenes via X-ray methods difficult. Powder diffractometer scans on pure maskelynite fractions of Shergotty revealed small amounts of still coherently diffracting plagioclase, which may contribute to the high refractive indices of the diaplectic feldspar glasses of Shergotty.

Pulsed supercritical synthesis of anatase TiO₂ nanoparticles in a water-isopropanol mixture studied by in situ powder X-ray diffraction.

PubMed

Rostgaard Eltzholtz, Jakob; Tyrsted, Christoffer; Ørnsbjerg Jensen, Kirsten Marie; Bremholm, Martin; Christensen, Mogens; Becker-Christensen, Jacob; Brummerstedt Iversen, Bo

2013-03-21

A new step in supercritical nanoparticle synthesis, the pulsed supercritical synthesis reactor, is investigated in situ using synchrotron powder X-ray diffraction (PXRD) to understand the formation of nanoparticles in real time. This eliminates the common problem of transferring information gained during in situ studies to subsequent laboratory reactor conditions. As a proof of principle, anatase titania nanoparticles were synthesized in a 50/50 mixture of water and isopropanol near and above the critical point of water (P = 250 bar, T = 300, 350, 400, 450, 500 and 550 °C). The evolution of the reaction product was followed by sequentially recording PXRD patterns with a time resolution of less than two seconds. The crystallite size of titania is found to depend on both temperature and residence time, and increasing either parameter leads to larger crystallites. A simple adjustment of either temperature or residence time provides a direct method for gram scale production of anatase nanoparticles of average crystallite sizes between 7 and 35 nm, thus giving the option of synthesizing tailor-made nanoparticles. Modeling of the in situ growth curves using an Avrami growth model gave an activation energy of 66(19) kJ mol(-1) for the initial crystallization. The in situ PXRD data also provide direct information about the size dependent macrostrain in the nanoparticles and with decreasing crystallite size the unit cell contracts, especially along the c-direction. This agrees well with previous ex situ results obtained for hydrothermal synthesis of titania nanoparticles.

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.

"X-Ray Transients in Star-Forming Regions" and "Hard X-Ray Emission from X-Ray Bursters"

NASA Technical Reports Server (NTRS)

Halpern, Jules P.; Kaaret, Philip

1999-01-01

This grant funded work on the analysis of data obtained with the Burst and Transient Experiment (BATSE) on the Compton Gamma-Ray Observatory. The goal of the work was to search for hard x-ray transients in star forming regions using the all-sky hard x-ray monitoring capability of BATSE. Our initial work lead to the discovery of a hard x-ray transient, GRO J1849-03. Follow-up observations of this source made with the Wide Field Camera on BeppoSAX showed that the source should be identified with the previously known x-ray pulsar GS 1843-02 which itself is identified with the x-ray source X1845-024 originally discovered with the SAS-3 satellite. Our identification of the source and measurement of the outburst recurrence time, lead to the identification of the source as a Be/X-ray binary with a spin period of 94.8 s and an orbital period of 241 days. The funding was used primarily for partial salary and travel support for John Tomsick, then a graduate student at Columbia University. John Tomsick, now Dr. Tomsick, received his Ph.D. from Columbia University in July 1999, based partially on results obtained under this investigation. He is now a postdoctoral research scientist at the University of California, San Diego.

Formation and Evolution of X-ray Binaries

NASA Astrophysics Data System (ADS)

Fragkos, Anastasios

X-ray binaries - mass-transferring binary stellar systems with compact object accretors - are unique astrophysical laboratories. They carry information about many complex physical processes such as star formation, compact object formation, and evolution of interacting binaries. My thesis work involves the study of the formation and evolution of Galactic and extra-galacticX-ray binaries using both detailed and realistic simulation tools, and population synthesis techniques. I applied an innovative analysis method that allows the reconstruction of the full evolutionary history of known black hole X-ray binaries back to the time of compact object formation. This analysis takes into account all the available observationally determined properties of a system, and models in detail four of its evolutionary evolutionary phases: mass transfer through the ongoing X-ray phase, tidal evolution before the onset of Roche-lobe overflow, motion through the Galactic potential after the formation of the black hole, and binary orbital dynamics at the time of core collapse. Motivated by deep extra-galactic Chandra survey observations, I worked on population synthesis models of low-mass X-ray binaries in the two elliptical galaxies NGC3379 and NGC4278. These simulations were targeted at understanding the origin of the shape and normalization of the observed X-ray luminosity functions. In a follow up study, I proposed a physically motivated prescription for the modeling of transient neutron star low-mass X-ray binary properties, such as duty cycle, outburst duration and recurrence time. This prescription enabled the direct comparison of transient low-mass X-ray binary population synthesis models to the Chandra X-ray survey of the two ellipticals NGC3379 and NGC4278. Finally, I worked on population synthesismodels of black holeX-ray binaries in the MilkyWay. This work was motivated by recent developments in observational techniques for the measurement of black hole spin magnitudes in

Lumbosacral spine x-ray

MedlinePlus

X-ray - lumbosacral spine; X-ray - lower spine ... The test is done in a hospital x-ray department or your health care provider's office by an x-ray technician. You will be asked to lie on the x-ray ...

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.

Discovery and development of x-ray diffraction

NASA Astrophysics Data System (ADS)

Jeong, Yeuncheol; Yin, Ming; Datta, Timir

2013-03-01

In 1912 Max Laue at University of Munich reasoned x-rays to be short wavelength electromagnetic waves and figured interference would occur when scattered off crystals. Arnold Sommerfeld, W. Wien, Ewald and others, raised objections to Laue's idea, but soon Walter Friedrich succeeded in recording x-ray interference patterns off copper sulfate crystals. But the Laue-Ewald's 3-dimensional formula predicted excess spots. Fewer spots were observed. William Lawrence Bragg then 22 year old studying at Cambridge University heard the Munich results from father William Henry Brag, physics professor at Univ of Leeds. Lawrence figured the spots are 2-d interference of x-ray wavelets reflecting off successive atomic planes and derived a simple eponymous equation, the Bragg equation d*sin(theta) = n*lamda. 1913 onward the Braggs dominated the crystallography. Max Laue was awarded the physics Nobel in 1914 and the Braggs shared the same in 1915. Starting with Rontgen's first ever prize in 1901, the importance of x-ray techniques is evident from the four out of a total 16 physics Nobels between 1901-1917. We will outline the historical back ground and importance of x-ray diffraction giving rise to techniques that even in 2013, remain work horses in laboratories all over the globe.

Toward a fourth-generation x-ray source.

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

Monction, D. E.

1999-05-19

The field of synchrotron radiation research has grown rapidly over the last 25 years due to both the push of the accelerator and magnet technology that produces the x-ray beams and the pull of the extraordinary scientific research that is possible with them. Three successive generations of synchrotrons radiation facilities have resulted in beam brilliances 11 to 12 orders of magnitude greater than the standard laboratory x-ray tube. However, greater advances can be easily imagined given the fact that x-ray beams from present-day facilities do not exhibit the coherence or time structure so familiar with the optical laser. Theoretical workmore » over the last ten years or so has pointed to the possibility of generating hard x-ray beams with laser-like characteristics. The concept is based on self-amplified spontaneous emission (SASE) in flee-electron lasers. A major facility of this type based upon a superconducting linac could produce a cost-effective facility that spans wave-lengths from the ultraviolet to the hard x-ray regime, simultaneously servicing large numbers experimenters from a wide range of disciplines. As with each past generation of synchrotrons facilities, immense new scientific opportunities would result from fourth-generation sources.« less

Oxidized nanocrystalline Fe-Cu pseudoalloy subjected to high pressure and electrodischarge pulses: Mössbauer and x-ray investigations

NASA Astrophysics Data System (ADS)

Gavriliuk, A. G.; Voitkovsky, V. S.; Sidorov, V. A.; Filonenko, V. P.; Tsiok, O. B.; Khvostantsev, L. G.

1998-05-01

Nanocrystalline Fe15Cu85 pseudoalloy has been subjected to pulsed heating up to 1500 K at high pressure (8 GPa). Two regimes were studied: the direct heating using electrodischarge through the sample and indirect heating with the use of cylindrical heater around the sample. The temperature and time conditions in both types of experiments were adjusted to be equivalent. The discharge parameters (stored energy, discharge time, and magnitude of current pulse) were sufficient to move defects by conduction electrons, but insufficient to melt the sample. The properties of treated samples were studied using Mössbauer absorption spectra and x-ray diffraction for three types of samples: (a) primary powder treated by high pressure up to 8 GPa, (b) powder subjected to indirect pulsed heating at 8 GPa, (c) powder treated by electrical pulses at 8 GPa. The x-ray diffraction pattern of primary powder exhibits peaks of copper, iron, and copper oxide (CuO). The Mössbauer spectrum of primary powder exhibits six peaks of alpha iron and some peaks near zero velocity due to the small iron clusters in the copper matrix and ultrafine clusters of paramagnetic phase x-Fe2O3. The transformation of CuO to Cu2O takes place in the course of indirect heating, the Mössbauer spectrum being almost unchanged. The direct electrodischarge heating causes the appearance of new magnetic phase with the magnetic field on iron nucleus 505 kOe, which corresponds to α-Fe2O3. The formation of α-Fe2O3 was confirmed by x-ray diffraction. At the same time the transformation of CuO to Cu2O is incomplete. These experiments demonstrate that high density current pulses, causing the electron wind, can be a useful tool to influence the structure of nanocrystalline powder.

SEXTANT - Station Explorer for X-Ray Timing and Navigation Technology

NASA Technical Reports Server (NTRS)

Mitchell, Jason; Hasouneh, Monther; Winternitz, Luke; Valdez, Jennifer; Price, Sam; Semper, Sean; Yu, Wayne; Gaebler, John; Ray, Paul; Wood, Kent;

Quantitative analysis of packed and compacted granular systems by x-ray microtomography

NASA Astrophysics Data System (ADS)

Fu, Xiaowei; Milroy, Georgina E.; Dutt, Meenakshi; Bentham, A. Craig; Hancock, Bruno C.; Elliott, James A.

2005-04-01

The packing and compaction of powders are general processes in pharmaceutical, food, ceramic and powder metallurgy industries. Understanding how particles pack in a confined space and how powders behave during compaction is crucial for producing high quality products. This paper outlines a new technique, based on modern desktop X-ray tomography and image processing, to quantitatively investigate the packing of particles in the process of powder compaction and provide great insights on how powder densify during powder compaction, which relate in terms of materials properties and processing conditions to tablet manufacture by compaction. A variety of powder systems were considered, which include glass, sugar, NaCl, with a typical particle size of 200-300 mm and binary mixtures of NaCl-Glass Spheres. The results are new and have been validated by SEM observation and numerical simulations using discrete element methods (DEM). The research demonstrates that XMT technique has the potential in further investigating of pharmaceutical processing and even verifying other physical models on complex packing.

The UCSD high energy X-ray timing experiment cosmic ray particle anticoincidence detector

NASA Technical Reports Server (NTRS)

Hink, P. L.; Rothschild, R. E.; Pelling, M. R.; Macdonald, D. R.; Gruber, D. E.

1991-01-01

The HEXTE, part of the X-Ray Timing Explorer (XTE), is designed to make high sensitivity temporal and spectral measurements of X-rays with energies between 15 and 250 keV using NaI/CsI phoswich scintillation counters. To achieve the required sensitivity it is necessary to provide anticoincidence of charged cosmic ray particles incident upon the instrument, some of which interact to produce background X-rays. The proposed cosmic ray particle anticoincidence shield detector for HEXTE uses a novel design based on plastic scintillators and wavelength-shifter bars. It consists of five segments, each with a 7 mm thick plastic scintillator, roughly 50 cm x 50 cm in size, coupled to two wavelength-shifter bars viewed by 1/2 inch photomultiplier tubes. These segments are configured into a five-sided, box-like structure around the main detector system. Results of laboratory testing of a model segment, and calculations of the expected performance of the flight segments and particle anticoincidence detector system are presented to demonstrate that the above anticoincidence detector system satisfies its scientific requirements.

Laboratory Measurements Of Charge-exchange Produced X-ray Emission From K-shell Transitions In Hydrogenic And Helium-like Fe

NASA Astrophysics Data System (ADS)

Brown, Gregory V.; Beiersdorfer, P.; Boyce, K. R.; Chen, H.; Gu, M. F.; Kelley, R. L.; Kilbourne, C. A.; Porter, F. S.; Thorn, D.; Wargelin, B.

2006-09-01

We have used a microcalorimeter and solid state detectors to measure x-ray emission produced by charge exchange reactions between bare and hydrogenic Fe colliding with neutral helium, hydrogen, and nitrogen gas. We show the measured spectral signature produced by different neutral donors and compare our results to theory where available. We also compare our results to measurements of the Fe K line emission from the Galactic Center measured by the XIS on the Suzaku x-ray observatory. This comparison shows that charge exchange recombination between highly charged ions (either cosmic rays or thermal ions) and neutral gas is probably not the dominant source of diffuse line emission in the Galactic Center. This work was performed under the auspices of the U.S. Department of Energy by University of California, Lawrence Livermore National Laboratory under Contract W-7405-Eng-48, and is also supported by NASA APRA grants to LLNL, GSFC, Harvard-Smithsonian CfA, and Stanford University.

Remote analysis of planetary soils: X-ray diffractometer development

NASA Technical Reports Server (NTRS)

Gregory, J. C.

1973-01-01

A system is described suitable for remote low power mineralogical analysis of lunar, planetary, or asteroid soils. It includes an X-ray diffractometer, fluorescence spectrometer, and sample preparation system. A one Curie Fe-55 source provides a monochromatic X-ray beam of 5.9 keV. Seeman-Bohlin or focusing geometry is employed in the camera, allowing peak detection to proceed simultaneously at all angles and obviating the need for moving parts. The detector system is an array of 500-600 proportional counters with a wire-spacing of 1 mm. An electronics unit comprising preamplifier, postamplifier, window discriminators, and storage flipflops requiring only 3.5 milliwatts was designed and tested. Total instrument power is less than 5 watts. Powder diffraction patterns using a flat breadboard multiwire counter were recorded.

Polymer X-ray refractive nano-lenses fabricated by additive technology.

PubMed

Petrov, A K; Bessonov, V O; Abrashitova, K A; Kokareva, N G; Safronov, K R; Barannikov, A A; Ershov, P A; Klimova, N B; Lyatun, I I; Yunkin, V A; Polikarpov, M; Snigireva, I; Fedyanin, A A; Snigirev, A

2017-06-26

The present work demonstrates the potential applicability of additive manufacturing to X-Ray refractive nano-lenses. A compound refractive lens with a radius of 5 µm was produced by the two-photon polymerization induced lithography. It was successfully tested at the X-ray microfocus laboratory source and a focal spot of 5 μm was measured. An amorphous nature of polymer material combined with the potential of additive technologies may result in a significantly enhanced focusing performance compared to the best examples of modern X-ray compound refractive lenses.

Heats of immersion of titania powders in primer solutions

NASA Technical Reports Server (NTRS)

Siriwardane, R.; Wightman, J. P.

1983-01-01

The oxide layer present on titanium alloys can play an important role in determining the strength and durability of adhesive bonds. Here, three titania powders in different crystalline phases, rutile-R1, anatase-A1, and anatase-A2, are characterized by several techniques. These include microelectrophoresis, X-ray diffractometry, surface area pore volume analysis, X-ray photoelectron spectroscopy, and measurements of the heats of immersion. Of the three powders, R1 has the highest heat of immersion in water, while the interaction between water and A1 powder is low. Experimental data also suggest a specific preferential interaction of polyphenylquinoxaline with anatase.

Sequential x-ray diffraction topography at 1-BM x-ray optics testing beamline at the advanced photon source

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

Stoupin, Stanislav, E-mail: sstoupin@aps.anl.gov; Shvyd’ko, Yuri; Trakhtenberg, Emil

2016-07-27

We report progress on implementation and commissioning of sequential X-ray diffraction topography at 1-BM Optics Testing Beamline of the Advanced Photon Source to accommodate growing needs of strain characterization in diffractive crystal optics and other semiconductor single crystals. The setup enables evaluation of strain in single crystals in the nearly-nondispersive double-crystal geometry. Si asymmetric collimator crystals of different crystallographic orientations were designed, fabricated and characterized using in-house capabilities. Imaging the exit beam using digital area detectors permits rapid sequential acquisition of X-ray topographs at different angular positions on the rocking curve of a crystal under investigation. Results on sensitivity andmore » spatial resolution are reported based on experiments with high-quality Si and diamond crystals. The new setup complements laboratory-based X-ray topography capabilities of the Optics group at the Advanced Photon Source.« less

Analytical performance of a versatile laboratory microscopic X-ray fluorescence system for metal uptake studies on argillaceous rocks

NASA Astrophysics Data System (ADS)

Gergely, Felicián; Osán, János; Szabó, B. Katalin; Török, Szabina

2016-02-01

Laboratory-scale microscopic X-ray fluorescence (micro-XRF) plays an increasingly important role in various fields where multielemental investigations of samples are indispensable. In case of geological samples, the reasonable detection limits (LOD) and spatial resolutions are necessary to identify the trace element content in microcrystalline level. The present study focuses on the analytical performance of a versatile laboratory-scale micro-XRF system with various options of X-ray sources and detectors to find the optimal experimental configuration in terms of sensitivities and LOD for selected elements in loaded petrographic thin sections. The method was tested for sorption studies involving thin sections prepared from cores of Boda Claystone Formation, which is a potential site for a high-level radioactive waste repository. Loaded ions in the sorption measurements were Cs(I) and Ni(II) chemically representing fission and corrosion products. Based on the collected elemental maps, the correlation between the elements representative of main rock components and the selected loaded ion was studied. For the elements of interest, Cs(I) and Ni(II) low-power iMOXS source with polycapillary and silicon drift detector was found to be the best configuration to reach the optimal LOD values. Laboratory micro-XRF was excellent to identify the responsible key minerals for the uptake of Cs(I). In case of nickel, careful corrections were needed because of the relatively high Ca content of the rock samples. The results were compared to synchrotron radiation micro-XRF.

UNDERSTANDING X-RAY STARS:. The Discovery of Binary X-ray Sources

NASA Astrophysics Data System (ADS)

Schreier, E. J.; Tananbaum, H.

2000-09-01

The discovery of binary X-ray sources with UHURU introduced many new concepts to astronomy. It provided the canonical model which explained X-ray emission from a large class of galactic X-ray sources: it confirmed the existence of collapsed objects as the source of intense X-ray emission; showed that such collapsed objects existed in binary systems, with mass accretion as the energy source for the X-ray emission; and provided compelling evidence for the existence of black holes. This model also provided the basis for explaining the power source of AGNs and QSOs. The process of discovery and interpretation also established X-ray astronomy as an essential sub-discipline of astronomy, beginning its incorporation into the mainstream of astronomy.

Thoracic spine x-ray

MedlinePlus

Vertebral radiography; X-ray - spine; Thoracic x-ray; Spine x-ray; Thoracic spine films; Back films ... The test is done in a hospital radiology department or in the health care provider's office. You will lie on the x-ray table in different positions. If the x-ray ...

X-ray binaries

NASA Technical Reports Server (NTRS)

1976-01-01

Satellite X-ray experiments and ground-based programs aimed at observation of X-ray binaries are discussed. Experiments aboard OAO-3, OSO-8, Ariel 5, Uhuru, and Skylab are included along with rocket and ground-based observations. Major topics covered are: Her X-1, Cyg X-3, Cen X-3, Cyg X-1, the transient source A0620-00, other possible X-ray binaries, and plans and prospects for future observational programs.

The Imaging X-Ray Polarimetry Explorer (IXPE): Overview

NASA Technical Reports Server (NTRS)

O'Dell, Steve; Weisskopf, M.; Soffitta, P.; Baldini, L.; Bellazzini, R.; Costa, E.; Elsner, R.; Kaspi, V.; Kolodziejczak, J.; Latronico, L.;

X-ray K-edge analysis of drain lines in Wilhelm Hall, Ames Laboratory

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

Jensen, T.; Whitmore, C.

1999-01-05

From August 12--27, 1998 X-ray K-edge measurements were made on drain lines in seven rooms in Wilhelm Hall, Ames Laboratory. The purpose of these measurements was to determine the extent of thorium (and other heavy metal) contamination inside these pipes. The K-edge method is a noninvasive inspection technique that can provide accurate quantification of heavy metal contamination interior to an object. Of the seven drain lines inspected, one was found to have no significant contamination, three showed significant thorium deposits, two showed mercury contamination, and one line was found to contain mercury, thorium and uranium. The K-edge measurements were foundmore » to be consistent with readings from hand-held survey meters, and provided much greater detail on the location and amount of heavy metal contamination.« less

Full-field transmission x-ray imaging with confocal polycapillary x-ray optics

PubMed Central

Sun, Tianxi; MacDonald, C. A.

2013-01-01

A transmission x-ray imaging setup based on a confocal combination of a polycapillary focusing x-ray optic followed by a polycapillary collimating x-ray optic was designed and demonstrated to have good resolution, better than the unmagnified pixel size and unlimited by the x-ray tube spot size. This imaging setup has potential application in x-ray imaging for small samples, for example, for histology specimens. PMID:23460760

Advanced Spectral Analysis Program (ASAP) for High-Pressure X-ray Diffraction

NASA Astrophysics Data System (ADS)

Montgomery, Jeffrey

A program for analyzing large powder diffraction data sets has been developed. This tool enables the user to fit any type of crystal structure by indexing peaks in multiple files simultaneously by manually selecting them from a 2D plot of peak positions. The program has tools for automatic peak fitting and pressure determination using various equations of state. The interface is useful for correlating information from various types of spectral data, and so tools have been added for analyzing common fluorescence markers such as ruby, strontium tetraborate, and diamond. The program operation is demonstrated by the analysis of high-pressure powder x-ray diffraction data taken on a sample of vanadium metal at the Advanced Photon Source 16-BMD beamline. Samples were compressed in three runs to a pressure of 70 GPa in an attempt to measure the phase transition from bcc to orthorhombic in hydrostatic and non-hydrostatic conditions. Using ASAP to analyze this data provides a fast and accurate tool for observation of such a subtle transition, which is characterized primarily by a narrow splitting of the bcc 110 and 112 peaks. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

X-ray generator

DOEpatents

Dawson, John M.

1976-01-01

Apparatus and method for producing coherent secondary x-rays that are controlled as to direction by illuminating a mixture of high z and low z gases with an intense burst of primary x-rays. The primary x-rays are produced with a laser activated plasma, and these x-rays strip off the electrons of the high z atoms in the lasing medium, while the low z atoms retain their electrons. The neutral atoms transfer electrons to highly excited states of the highly striped high z ions giving an inverted population which produces the desired coherent x-rays. In one embodiment, a laser, light beam provides a laser spark that produces the intense burst of coherent x-rays that illuminates the mixture of high z and low z gases, whereby the high z atoms are stripped while the low z ones are not, giving the desired mixture of highly ionized and neutral atoms. To this end, the laser spark is produced by injecting a laser light beam, or a plurality of beams, into a first gas in a cylindrical container having an adjacent second gas layer co-axial therewith, the laser producing a plasma and the intense primary x-rays in the first gas, and the second gas containing the high and low atomic number elements for receiving the primary x-rays, whereupon the secondary x-rays are produced therein by stripping desired ions in a neutral gas and transfer of electrons to highly excited states of the stripped ions from the unionized atoms. Means for magnetically confining and stabilizing the plasma are disclosed for controlling the direction of the x-rays.

Ground calibrations of the X-ray detector system of the Solar Intensity X-ray Spectrometer (SIXS) on board BepiColombo

NASA Astrophysics Data System (ADS)

Huovelin, Juhani; Lehtolainen, Arto; Genzer, Maria; Korpela, Seppo; Esko, Eero; Andersson, Hans

2014-05-01

SIXS includes X-ray and particle detector systems for the BepiColombo Mercury Planetary Orbiter (MPO). Its task is to monitor the direct solar X-rays and energetic particles in a wide field of view in the energy range of 1-20 keV (X-rays), 0.1-3 MeV (electrons) and 1-30 MeV (protons). The main purpose of these measurements is to provide quantitative information on the high energy radiation incident on Mercury's surface which causes the X-ray glow of the planet measured by the MIXS instrument. The X-ray and particle measurements of SIXS are also useful for investigations of the solar corona and the magnetosphere of Mercury. The ground calibrations of the X-ray detectors of the SIXS flight model were carried out in the X-ray laboratory of the Helsinki University during May and June 2012. The aim of the ground calibrations was to characterize the performance of the SIXS instrument's three High-Purity Silicon PIN X-ray detectors and verify that they fulfil their scientific performance requirements. The calibrations included the determination of the beginning of life energy resolution at different operational temperatures, determination of the detector's sensitivity within the field of view as a function of the off-axis and roll angles, pile-up tests for determining the speed of the read out electronics, measurements of the low energy threshold of the energy scale, a cross-calibration with the SMART-1 XSM flight spare detector, and the determination of the temperature dependence of the energy scale. An X-ray tube and the detectors' internal Ti coated 55Fe calibration sources were used as primary X-ray sources. In addition, two external fluorescence sources were used as secondary X-ray sources in the determination of the energy resolutions and in the comparison calibration with the SMART-1 XSM. The calibration results show that the detectors fulfill all of the scientific performance requirements. The ground calibration data combined with the instrument house-keeping data

X-ray lithography masking

NASA Technical Reports Server (NTRS)

Smith, Henry I. (Inventor); Lim, Michael (Inventor); Carter, James (Inventor); Schattenburg, Mark (Inventor)

1998-01-01

X-ray masking apparatus includes a frame having a supporting rim surrounding an x-ray transparent region, a thin membrane of hard inorganic x-ray transparent material attached at its periphery to the supporting rim covering the x-ray transparent region and a layer of x-ray opaque material on the thin membrane inside the x-ray transparent region arranged in a pattern to selectively transmit x-ray energy entering the x-ray transparent region through the membrane to a predetermined image plane separated from the layer by the thin membrane. A method of making the masking apparatus includes depositing back and front layers of hard inorganic x-ray transparent material on front and back surfaces of a substrate, depositing back and front layers of reinforcing material on the back and front layers, respectively, of the hard inorganic x-ray transparent material, removing the material including at least a portion of the substrate and the back layers of an inside region adjacent to the front layer of hard inorganic x-ray transparent material, removing a portion of the front layer of reinforcing material opposite the inside region to expose the surface of the front layer of hard inorganic x-ray transparent material separated from the inside region by the latter front layer, and depositing a layer of x-ray opaque material on the surface of the latter front layer adjacent to the inside region.

Static and Dynamical Structural Investigations of Metal-Oxide Nanocrystals by Powder X-ray Diffraction: Colloidal Tungsten Oxide as a Case Study

DOE PAGES

Caliandro, Rocco; Sibillano, Teresa; Belviso, B. Danilo; ...

2016-02-02

In this study, we have developed a general X-ray powder diffraction (XPD) methodology for the simultaneous structural and compositional characterization of inorganic nanomaterials. The approach is validated on colloidal tungsten oxide nanocrystals (WO 3-x NCs), as a model polymorphic nanoscale material system. Rod-shaped WO 3-x NCs with different crystal structure and stoichiometry are comparatively investigated under an inert atmosphere and after prolonged air exposure. An initial structural model for the as-synthesized NCs is preliminarily identified by means of Rietveld analysis against several reference crystal phases, followed by atomic pair distribution function (PDF) refinement of the best-matching candidates (static analysis). Subtlemore » stoichiometry deviations from the corresponding bulk standards are revealed. NCs exposed to air at room temperature are monitored by XPD measurements at scheduled time intervals. The static PDF analysis is complemented with an investigation into the evolution of the WO 3-x NC structure, performed by applying the modulation enhanced diffraction technique to the whole time series of XPD profiles (dynamical analysis). Prolonged contact with ambient air is found to cause an appreciable increase in the static disorder of the O atoms in the WO 3-x NC lattice, rather than a variation in stoichiometry. Finally, the time behavior of such structural change is identified on the basis of multivariate analysis.« less

Sinus x-ray

MedlinePlus

Paranasal sinus radiography; X-ray - sinuses ... sinus x-ray is taken in a hospital radiology department. Or the x-ray may be taken ... Brown J, Rout J. ENT, neck, and dental radiology. In: Adam A, Dixon AK, Gillard JH, Schaefer- ...

Low Energy X-Ray and Electron Physics and Technology for High-Temperature Plasma Diagnostics

DTIC Science & Technology

1987-10-01

This program in low-energy x-ray physics and technology has expanded into a major program with the principal objective of supporting research and application programs at the new large x-ray source facilities, particularly the high temperature plasma and synchrotron radiation sources. This program addresses the development of absolute x-ray diagnostics for the fusion energy and x-ray laser research and development. The new laboratory includes five specially designed

Development and tests of x-ray multifoil optical system for 1D imaging (Conference Presentation)

NASA Astrophysics Data System (ADS)

Pína, Ladislav; Hudec, René; Inneman, Adolf J.; Baca, Tomas; Blazek, M.; Platkevic, M.; Sieger, Ladislav; Doubravova, Daniela; McEntaffer, Randall L.; Schultz, Ted B.; Dániel, Vladimír.

2016-09-01

The proposed wide-field optical system has not been used yet. Described novel approach is based on the use of 1D "Lobster eye" optics in combination with Timepix X-ray detector in the energy range 3 - 40 keV. The proposed project includes theoretical study and a functional sample of the Timepix X-ray detector with multifoil wide-field X-ray "Lobster eye" optics. Using optics to focus X-rays on a detector is necessary in cases where the intensity of impinging X-ray radiation is below the sensitivity of the detector without optic. Generally this is the case of very low light phenomena, or e.g. monitoring astrophysical objects in space. Namely, such optical system could find applications in laboratory spectroscopy systems or in a rocket space experiment. Designed wide-field optical system combined with Timepix X-ray detector is described together with experimental results obtained during laboratory tests.

Recent X-ray Variability of Eta Car Approaching The X-ray Eclipse

NASA Technical Reports Server (NTRS)

Corcoran, M.; Swank, J. H.; Ishibashi, K.; Gull, T.; Humphreys, R.; Damineli, A.; Walborn, N.; Hillier, D. J.; Davidson, K.; White, S. M.

2002-01-01

We discuss recent X-ray spectral variability of the supermassive star Eta Car in the interval since the last X-ray eclipse in 1998. We concentrate on the interval just prior to the next X-ray eclipse which is expected to occur in June 2003. We compare the X-ray behavior during the 2001-2003 cycle with the previous cycle (1996-1998) and note similarities and differences in the temporal X-ray behavior. We also compare a recent X-ray observation of Eta Car obtained with the Chandra high energy transmission grating in October 2002 with an earlier observation from Nov 2002, and interpret these results in terms of the proposed colliding wind binary model for the star. In addition we discuss planned observations for the upcoming X-ray eclipse.

Large area soft x-ray collimator to facilitate x-ray optics testing

NASA Technical Reports Server (NTRS)

Espy, Samuel L.

1994-01-01

The first objective of this program is to design a nested conical foil x-ray optic which will collimate x-rays diverging from a point source. The collimator could then be employed in a small, inexpensive x-ray test stand which would be used to test various x-ray optics and detector systems. The second objective is to demonstrate the fabrication of the x-ray reflectors for this optic using lacquer-smoothing and zero-stress electroforming techniques.

MSL Chemistry and Mineralogy X-Ray Diffraction X-Ray Fluorescence (CheMin) Instrument

NASA Technical Reports Server (NTRS)

Zimmerman, Wayne; Blake, Dave; Harris, William; Morookian, John Michael; Randall, Dave; Reder, Leonard J.; Sarrazin, Phillipe

2013-01-01

This paper provides an overview of the Mars Science Laboratory (MSL) Chemistry and Mineralogy Xray Diffraction (XRD), X-ray Fluorescence (XRF) (CheMin) Instrument, an element of the landed Curiosity rover payload, which landed on Mars in August of 2012. The scientific goal of the MSL mission is to explore and quantitatively assess regions in Gale Crater as a potential habitat for life - past or present. The CheMin instrument will receive Martian rock and soil samples from the MSL Sample Acquisition/Sample Processing and Handling (SA/SPaH) system, and process it utilizing X-Ray spectroscopy methods to determine mineral composition. The Chemin instrument will analyze Martian soil and rocks to enable scientists to investigate geophysical processes occurring on Mars. The CheMin science objectives and proposed surface operations are described along with the CheMin hardware with an emphasis on the system engineering challenges associated with developing such a complex instrument.

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

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

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorptionmore » edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.« less

Locating Stardust-like Particles in Aerogel Using X-Ray Techniques

NASA Technical Reports Server (NTRS)

Jurewicz, A. J. G.; Jones, S. M.; Tsapin, A.; Mih, D. T.; Connolly, H. C., Jr.; Graham, G. A.

2003-01-01

Silica aerogel is the material that the spacecraft STARDUST is using to collect interstellar and cometary silicates. Anticipating the return of the samples to earth in January of 2006, MANY individual investigators and, especially, the investigators in NASA's SRLIDAP program are studying means of both in situ analysis of particles, as well as particle extraction. To help individual PI's with extraction of particles from aerogel in their own laboratories, we are exploring the use of standard laboratory x-ray equipment and commercial techniques for precisely locating specific particles in aerogel. We approached the evaluation of commercial x-ray techniques as follows. First, we determined the most appropriate detector for use with aerogel and particulates. Then, we compared and contrasted techniques useful for university laboratories.

Effect of surface coating with magnesium stearate via mechanical dry powder coating approach on the aerosol performance of micronized drug powders from dry powder inhalers.

PubMed

Zhou, Qi Tony; Qu, Li; Gengenbach, Thomas; Larson, Ian; Stewart, Peter J; Morton, David A V

2013-03-01

The objective of this study was to investigate the effect of particle surface coating with magnesium stearate on the aerosolization of dry powder inhaler formulations. Micronized salbutamol sulphate as a model drug was dry coated with magnesium stearate using a mechanofusion technique. The coating quality was characterized by X-ray photoelectron spectroscopy. Powder bulk and flow properties were assessed by bulk densities and shear cell measurements. The aerosol performance was studied by laser diffraction and supported by a twin-stage impinger. High degrees of coating coverage were achieved after mechanofusion, as measured by X-ray photoelectron spectroscopy. Concomitant significant increases occurred in powder bulk densities and in aerosol performance after coating. The apparent optimum performance corresponded with using 2% w/w magnesium stearate. In contrast, traditional blending resulted in no significant changes in either bulk or aerosolization behaviour compared to the untreated sample. It is believed that conventional low-shear blending provides insufficient energy levels to expose host micronized particle surfaces from agglomerates and to distribute guest coating material effectively for coating. A simple ultra-high-shear mechanical dry powder coating step was shown as highly effective in producing ultra-thin coatings on micronized powders and to substantially improve the powder aerosolization efficiency.

The Imaging X-Ray Polarimetry Explorer (IXPE)

NASA Technical Reports Server (NTRS)

Weisskopf, Martin C.; Ramsey, Brian; O’Dell, Stephen; Tennant, Allyn; Elsner, Ronald; Soffita, Paolo; Bellazzini, Ronaldo; Costa, Enrico; Kolodziejczak, Jeffery; Kaspi, Victoria;

Effect of chlorine in clay-mineral specimens prepared on silver metal-membrane mounts for X-ray powder diffraction analysis

USGS Publications Warehouse

Poppe, L.J.; Commeau, J.A.; Pense, G.M.

1989-01-01

Silver metal-membrane filters are commonly used as substrates in the preparation of oriented clay-mineral specimens for X-ray powder diffraction (XRD). They are relatively unaffected by organic solvent treatments and specimens can be prepared rapidly. The filter mounts are adaptable to automatic sample changers, have few discrete reflections at higher 20 angles, and, because of the high atomic number of silver, produce a relatively low overall background compared with other membrane filters, such as cellulose (Poppe and Hathaway, 1979). The silver metal-membrane filters, however, present some problems after heat treatment if either the filters or the samples contain significant amounts of chlorine. At elevated temperature, the chloride ions react with the silver substrate to form crystalline compounds. These compounds change the mass-absorption coefficient of the sample, reducing peak intensities and areas and, therefore, complicating the semiquantitative estimation of clay minerals. A simple procedure that eliminates most of the chloride from a sample and the silver metal-membrane substrate is presented here.

Single-pulse coherent diffraction imaging using soft x-ray laser.

PubMed

Kang, Hyon Chol; Kim, Hyung Taek; Kim, Sang Soo; Kim, Chan; Yu, Tae Jun; Lee, Seong Ku; Kim, Chul Min; Kim, I Jong; Sung, Jae Hee; Janulewicz, Karol A; Lee, Jongmin; Noh, Do Young

2012-05-15

We report a coherent diffraction imaging (CDI) using a single 8 ps soft x-ray laser pulse at a wavelength of 13.9 nm. The soft x-ray pulse was generated by a laboratory-scale intense pumping laser providing coherent x-ray pulses up to the level of 10(11) photons/pulse. A spatial resolution below 194 nm was achieved with a single pulse, and it was shown that a resolution below 55 nm is feasible with improved detector capability. The single-pulse CDI might provide a way to investigate dynamics of nanoscale molecules or particles.

Calorimetry investigations of milled α-tricalcium phosphate (α-TCP) powders to determine the formation enthalpies of α-TCP and X-ray amorphous tricalcium phosphate.

PubMed

Hurle, Katrin; Neubauer, Juergen; Bohner, Marc; Doebelin, Nicola; Goetz-Neunhoeffer, Friedlinde

2015-09-01

One α-tricalcium phosphate (α-TCP) powder was either calcined at 500°C to obtain fully crystalline α-TCP or milled for different durations to obtain α-TCP powders containing various amounts of X-ray amorphous tricalcium phosphate (ATCP). These powders containing between 0 and 71wt.% ATCP and up to 2.0±0.1wt.% β-TCP as minor phase were then hydrated in 0.1M Na2HPO4 aqueous solution and the resulting heat flows were measured by isothermal calorimetry. Additionally, the evolution of the phase composition during hydration was determined by in situ XRD combined with the G-factor method, an external standard method which facilitates the indirect quantification of amorphous phases. Maximum ATCP hydration was reached after about 1h, while that of crystalline α-TCP hydration occurred between 4 and 11h, depending on the ATCP content. An enthalpy of formation of -4065±6kJ/mol (T=23°C) was calculated for ATCP (Ca3(PO4)2), while for crystalline α-TCP (α-Ca3(PO4)2) a value of -4113±6kJ/mol (T=23°C) was determined. Copyright © 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Panoramic Dental X-Ray

MedlinePlus

... Physician Resources Professions Site Index A-Z Panoramic Dental X-ray Panoramic dental x-ray uses a very small dose of ... x-ray , is a two-dimensional (2-D) dental x-ray examination that captures the entire mouth ...

Single-Shot X-Ray Phase-Contrast Computed Tomography with Nonmicrofocal Laboratory Sources

NASA Astrophysics Data System (ADS)

Diemoz, P. C.; Hagen, C. K.; Endrizzi, M.; Minuti, M.; Bellazzini, R.; Urbani, L.; De Coppi, P.; Olivo, A.

2017-04-01

We present a method that enables performing x-ray phase-contrast imaging (XPCI) computed tomography with a laboratory setup using a single image per projection angle, eliminating the need to move optical elements during acquisition. Theoretical derivation of the method is presented, and its validity conditions are provided. The object is assumed to be quasihomogeneous, i.e., to feature a ratio between the refractive index and the linear attenuation coefficient that is approximately constant across the field of view. The method is experimentally demonstrated on a plastics phantom and on biological samples using a continuous rotation acquisition scheme achieving scan times of a few minutes. Moreover, we show that such acquisition times can be further reduced with the use of a high-efficiency photon-counting detector. Thanks to its ability to substantially simplify the image-acquisition procedure and greatly reduce collection times, we believe this method represents a very important step towards the application of XPCI to real-world problems.

X-ray imaging of fibers

NASA Astrophysics Data System (ADS)

Moosman, B.; Song, Y.; Weathers, L.; Wessel, F.

1996-11-01

A pulsed x-ray backlighter was developed to image exploding wires and cryogenic fibers. The x-ray pulse width is between 10-20 ns, with an output of 100-150 mJ, mostly in the Al k-shell (1.486 keV). The backlighter is located 50 cm from the 20-50 micron diameter target (typically, a copper wire). A 15 micron Al filter eliminates UV emission from the backlighter and target. It is placed 3 cm from the target with SB-5 film directly behind it. From the optical density of the film, target absorption and density can be calculated. The spatial resolution of this system is better than 40 microns. The wire is exploded using a 10 kA, 1 microsecond pulser. Analysis with simultaneous Moire imaging will also be presented. Supported by Los Alamos National Laboratories

Quantitative determination of airborne respirable non-fibrous alpha-silicon carbide by x-ray powder diffractometry.

PubMed

Bye, E; Føreland, S; Lundgren, L; Kruse, K; Rønning, R

2009-06-01

The purpose of the present investigation was to establish a method for the determination of airborne respirable non-fibrous silicon carbide (SiC). The main application is within the industrial production of SiC. Due to the complex airborne aerosol mixture of crystalline compounds in the SiC industry, X-ray powder diffractometry was selected as the most appropriate method. Without any international standard material for the respirable fraction of non-fibrous SiC, pure and suitable products from three SiC plants in Norway were selected. These products have a median particle diameter in the range 4.4-5.1 mum. The method is based on thin sample technique, with the dust deposited on a polycarbonate filter. Absorption correction is done by standard procedures with the use of a silver filter, situated below the polycarbonate filter. The diffraction line used for quantitative determination was selected carefully. This was done to avoid interferences from quartz, cristobalite, and graphite, which all are airborne components present in the atmosphere during the industrial process. The instrumental limit of detection for the method is 12 microg. This method has been used to determine airborne non-fibrous SiC in a comprehensive ongoing project in the Norwegian SiC industry for further epidemiological studies. The method is fully applicable for compliance work.

Effect of Tube-Based X-Ray Microtomography Imaging on the Amino Acid and Amine Content of the Murchison CM2 Chondrite

NASA Technical Reports Server (NTRS)

Glavin, D. P.; Friedrich, J. M.; Aponte, J. C.; Dworkin, J. P.; Ebel, D. S.; Elsila, J. E.; Hill, M.; McLain, H. L.; Towbin, W. H.

2017-01-01

X-ray and synchrotron X-ray micro-computed tomography (micro-CT) are increasingly being used for three dimensional reconnaissance imaging of chondrites and returned extraterrestrial material prior to detailed chemical and mineralogical analyses. Although micro-CT imaging is generally considered to be a non-destructive technique since silicate and metallic minerals in chondrites are not affected by X-ray exposures at the intensities and wavelengths typically used, there are concerns that the use of micro-CT could be detrimental to the organics in carbonaceous chondrites. We recently conducted a synchrotron micro-CT experiment on a powdered sample of the Murchison CM2 carbonaceous chondrite exposed to a monochromatic high energy (approximately 48 kiloelectronvolts) total X-ray radiation dose of approximately 1 kilogray (kGy) using the Advanced Photon Source beamline 13-BMD (13-Bending Magnet-D Beamline) at Argonne National Laboratory and found that there were no detectable changes in the amino acid abundances or enantiomeric compositions in the chondrite after exposure relative to a Murchison control sample that was not exposed. However, lower energy bremsstrahlung X-rays could interact more with amino acids and other lower molecular weight amines in meteorites. To test for this possibility, three separate micro-CT imaging experiments of the Murchison meteorite using the GE Phoenix v/tome/x s 240 kilovolt microfocus high resolution tungsten target X-ray tube instrument at the American Museum of Natural History (AMNH) were conducted and the amino acid abundances and enantiomeric compositions were determined. We also investigated the abundances of the C1-C5 amines in Murchison which were not analyzed in the first study.

The Generation-X X-ray Observatory Vision Mission and Technology Study

NASA Technical Reports Server (NTRS)

Figueroa-Feliciano, Enectali

2004-01-01

The new frontier in astrophysics is the study of the birth and evolution of the first stars, galaxies and black holes in the early Universe. X-ray astronomy opens a window into these objects by studying the emission from black holes, supernova explosions and the gamma-ray burst afterglows of massive stars. However, such objects are beyond the grasp of current or near-future observatories. X-ray imaging and spectroscopy of such distant objects will require an X-ray telescope with large collecting area and high angular resolution. Our team has conceived the Generation-X Vision Mission based on an X-ray observatory with 100 sq m collecting area at 1 keV (1000 times larger than Chandra) and 0.1 arcsecond angular resolution (several times better than Chandra and 50 times better than the Constellation-X resolution goal). Such an observatory would be capable of detecting the earliest black holes and galaxies in the Universe, and will also study extremes of density, gravity, magnetic fields, and kinetic energy which cannot be created in laboratories. NASA has selected the Generation-X mission for study under its Vision Mission Program. We describe the studies being performed to develop the mission concept and define candidate technologies and performance requirements for Generation-X. The baseline Generation-X mission involves four 8m diameter X-ray telescopes operating at Sun-Earth L2. We trade against an alternate concept of a single 26m diameter telescope with focal plane instruments on a separate spacecraft. A telescope of this size will require either robotic or human-assisted in-flight assembly. The required effective area implies that extremely lightweight grazing incidence X-ray optics must be developed. To achieve the required aerial density of at least 100 times lower than in Chandra, we will study 0.1mm thick mirrors which have active on-orbit figure control. We discuss the suite of required detectors, including a large FOV high angular resolution imager, a

Airborne particulate matter (PM) filter analysis and modeling by total reflection X-ray fluorescence (TXRF) and X-ray standing wave (XSW).

PubMed

Borgese, L; Salmistraro, M; Gianoncelli, A; Zacco, A; Lucchini, R; Zimmerman, N; Pisani, L; Siviero, G; Depero, L E; Bontempi, E

2012-01-30

This work is presented as an improvement of a recently introduced method for airborne particulate matter (PM) filter analysis [1]. X-ray standing wave (XSW) and total reflection X-ray fluorescence (TXRF) were performed with a new dedicated laboratory instrumentation. The main advantage of performing both XSW and TXRF, is the possibility to distinguish the nature of the sample: if it is a small droplet dry residue, a thin film like or a bulk sample. Another advantage is related to the possibility to select the angle of total reflection to make TXRF measurements. Finally, the possibility to switch the X-ray source allows to measure with more accuracy lighter and heavier elements (with a change in X-ray anode, for example from Mo to Cu). The aim of the present study is to lay the theoretical foundation of the new proposed method for airborne PM filters quantitative analysis improving the accuracy and efficiency of quantification by means of an external standard. The theoretical model presented and discussed demonstrated that airborne PM filters can be considered as thin layers. A set of reference samples is prepared in laboratory and used to obtain a calibration curve. Our results demonstrate that the proposed method for quantitative analysis of air PM filters is affordable and reliable without the necessity to digest filters to obtain quantitative chemical analysis, and that the use of XSW improve the accuracy of TXRF analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

Illicit drug detection using energy dispersive x-ray diffraction

NASA Astrophysics Data System (ADS)

Cook, E. J.; Griffiths, J. A.; Koutalonis, M.; Gent, C.; Pani, S.; Horrocks, J. A.; George, L.; Hardwick, S.; Speller, R.

2009-05-01

Illicit drugs are imported into countries in myriad ways, including via the postal system and courier services. An automated system is required to detect drugs in parcels for which X-ray diffraction is a suitable technique as it is non-destructive, material specific and uses X-rays of sufficiently high energy to penetrate parcels containing a range of attenuating materials. A database has been constructed containing the measured powder diffraction profiles of several thousand materials likely to be found in parcels. These include drugs, cutting agents, packaging and other innocuous materials. A software model has been developed using these data to predict the diffraction profiles which would be obtained by X-ray diffraction systems with a range of suggested detector (high purity germanium, CZT and scintillation), source and collimation options. The aim of the model was to identify the most promising system geometries, which was done with the aid of multivariate analysis (MVA). The most promising systems were constructed and tested. The diffraction profiles of a range of materials have been measured and used to both validate the model and to identify the presence of drugs in sample packages.

A novel von Hamos spectrometer for efficient X-ray emission spectroscopy in the laboratory

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

Anklamm, Lars, E-mail: anklamm@physik.tu-berlin.de; Schlesiger, Christopher; Malzer, Wolfgang

2014-05-15

We present a novel, highly efficient von Hamos spectrometer for X-ray emission spectroscopy (XES) in the laboratory using highly annealed pyrolitic graphite crystals as the dispersive element. The spectrometer covers an energy range from 2.5 keV to 15 keV giving access to chemical speciation and information about the electronic configuration of 3d transition metals by means of the Kβ multiplet. XES spectra of Ti compounds are presented to demonstrate the speciation capabilities of the instrument. A spectral resolving power of E/ΔE = 2000 at 8 keV was achieved. Typical acquisition times range from 10 min for bulk material to hours formore » thin samples below 1 μm.« less

Anisotropic crystal deformation measurements determined using powder X-ray diffraction and a new in situ compression stage.

PubMed

Haware, Rahul V; Kim, Paul; Ruffino, Lauren; Nimi, Brian; Fadrowsky, Catherine; Doyle, Michael; Boerrigter, Stephan X M; Cuitino, Alberto; Morris, Ken

2011-10-14

This report addresses the development of experimental and computational estimations of the anisotropic elastic moduli (EM) of single crystals to aid in the a priori (i.e., starting with the crystal structure) prediction of the trend as a function of the direction of applied stress. Experimentally EM values in the normal direction to the X-, Y- and Z-planes of block shaped aspirin and acetaminophen crystals were determined using data generated by the newly designed compression stage housed in our powder X-ray diffractometer. Computational estimations of EM were made using the applicable modules in Material Studio 5.5. The measured EM values normal to the (100), (020) and (002) planes of aspirin, and (20-1), (020) and (001) planes of acetaminophen crystals by both methods succeeded in detected the anisotropic behavior. However, disparity in the relative values between measured EM values by different techniques was observed. This may be attributed to deformation sources other than lattice compression including inelastic processes such as local failure and plasticity as well as deformation at the crystal-probe interfaces due to crystal surface roughness (asperities). The trend of the ratio of the values from the respective methods showed reasonable agreement and promise for the technique. The present approach demonstrated the suitability of the compression stage to determine and predict anisotropic EM of subjected small molecular organic crystals. Copyright © 2011 Elsevier B.V. All rights reserved.

First Results from a Microfocus X-Ray System for Macromolecular Crystallography

NASA Technical Reports Server (NTRS)

Gubarev, Mikhail; Ciszak, Ewa; Ponomarev, Igor; Gibson, Walter; Joy, Marshall

1999-01-01

The design and performance of a 40 Watt laboratory crystallography system optimized for the structure determination of small protein crystals are described. This system combines a microfocus x-ray generator (40 microns FWHM spot size at a power level of 40 Watts) and a short focal length (F = 2.6 mm) polycapillary collimating optic, and produces a small diameter quasi-parallel x-ray beam. Measurements of x-ray flux, divergence and spectral purity of the resulting x-ray beam are presented. The x-ray flux in a 250 microns diameter aperture produced by the microfocus system is 14.7 times higher .than that from a 3.15 kW rotating anode generator equipped with graphite monochromator. Crystallography data taken with the microfocus system are presented, and indicate that the divergence and spectral purity of the x-ray are sufficient to refine the diffraction data using a standard crystallographic software. Significant additional improvements in flux and beam divergence are possible, and plans for achieving these coals are discussed.

Microfocus/Polycapillary-Optic Crystallographic X-Ray System

NASA Technical Reports Server (NTRS)

Joy, Marshall; Gubarev, Mikhail; Ciszak, Ewa

2005-01-01

A system that generates an intense, nearly collimated, nearly monochromatic, small-diameter x-ray beam has been developed for use in macromolecular crystallography. A conventional x-ray system for macromolecular crystallography includes a rotating-anode x-ray source, which is massive (.500 kg), large (approximately 2 by 2 by 1 m), and power-hungry (between 2 and 18 kW). In contrast, the present system generates a beam of the required brightness from a microfocus source, which is small and light enough to be mounted on a laboratory bench, and operates at a power level of only tens of watts. The figure schematically depicts the system as configured for observing x-ray diffraction from a macromolecular crystal. In addition to the microfocus x-ray source, the system includes a polycapillary optic . a monolithic block (typically a bundle of fused glass tubes) that contains thousands of straight or gently curved capillary channels, along which x-rays propagate with multiple reflections. This particular polycapillary optic is configured to act as a collimator; the x-ray beam that emerges from its output face consists of quasi-parallel subbeams with a small angular divergence and a diameter comparable to the size of a crystal to be studied. The gap between the microfocus x-ray source and the input face of the polycapillary optic is chosen consistently with the focal length of the polycapillary optic and the need to maximize the solid angle subtended by the optic in order to maximize the collimated x-ray flux. The spectrum from the source contains a significant component of Cu K (photon energy is 8.08 keV) radiation. The beam is monochromatized (for Cu K ) by a nickel filter 10 m thick. In a test, this system was operated at a power of 40 W (current of 897 A at an accelerating potential of 45 kV), with an anode x-ray spot size of 41+/-2 microns. Also tested, in order to provide a standard for comparison, was a commercial rotating-anode x-ray crystallographic system with a

X-ray beam finder

DOEpatents

Gilbert, H.W.

1983-06-16

An X-ray beam finder for locating a focal spot of an X-ray tube includes a mass of X-ray opaque material having first and second axially-aligned, parallel-opposed faces connected by a plurality of substantially identical parallel holes perpendicular to the faces and a film holder for holding X-ray sensitive film tightly against one face while the other face is placed in contact with the window of an X-ray head.

X-ray and gamma ray astronomy detectors

NASA Technical Reports Server (NTRS)

Decher, Rudolf; Ramsey, Brian D.; Austin, Robert

1994-01-01

X-ray and gamma ray astronomy was made possible by the advent of space flight. Discovery and early observations of celestial x-rays and gamma rays, dating back almost 40 years, were first done with high altitude rockets, followed by Earth-orbiting satellites> once it became possible to carry detectors above the Earth's atmosphere, a new view of the universe in the high-energy part of the electromagnetic spectrum evolved. Many of the detector concepts used for x-ray and gamma ray astronomy were derived from radiation measuring instruments used in atomic physics, nuclear physics, and other fields. However, these instruments, when used in x-ray and gamma ray astronomy, have to meet unique and demanding requirements related to their operation in space and the need to detect and measure extremely weak radiation fluxes from celestial x-ray and gamma ray sources. Their design for x-ray and gamma ray astronomy has, therefore, become a rather specialized and rapidly advancing field in which improved sensitivity, higher energy and spatial resolution, wider spectral coverage, and enhanced imaging capabilities are all sought. This text is intended as an introduction to x-ray and gamma ray astronomy instruments. It provides an overview of detector design and technology and is aimed at scientists, engineers, and technical personnel and managers associated with this field. The discussion is limited to basic principles and design concepts and provides examples of applications in past, present, and future space flight missions.

X-Ray Diffraction Study of Elemental Erbium to 65 GPa

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

Pravica, M.G.; Lipinska-Kalita, K.; Quine, Z.

2006-02-02

We have investigated phase transitions in elemental erbium in a diamond anvil cell up to 65 GPa using x-ray powder diffraction methods. We present preliminary evidence of a series of phase transitions that appear to follow the expected hcp {yields} Sm-type {yields} dhcp {yields} distorted fcc sequence. In particular, we believe that we have evidence for the predicted dhcp {yields} distorted fcc transition between 43 GPa and 65 GPa.

X-ray imaging crystal spectrometer for extended X-ray sources

DOEpatents

Bitter, Manfred L.; Fraenkel, Ben; Gorman, James L.; Hill, Kenneth W.; Roquemore, A. Lane; Stodiek, Wolfgang; von Goeler, Schweickhard E.

2001-01-01

Spherically or toroidally curved, double focusing crystals are used in a spectrometer for X-ray diagnostics of an extended X-ray source such as a hot plasma produced in a tokomak fusion experiment to provide spatially and temporally resolved data on plasma parameters using the imaging properties for Bragg angles near 45. For a Bragg angle of 45.degree., the spherical crystal focuses a bundle of near parallel X-rays (the cross section of which is determined by the cross section of the crystal) from the plasma to a point on a detector, with parallel rays inclined to the main plain of diffraction focused to different points on the detector. Thus, it is possible to radially image the plasma X-ray emission in different wavelengths simultaneously with a single crystal.

Miniature X-Ray Solar Spectrometer: A Science-Oriented, University 3U CubeSat

NASA Technical Reports Server (NTRS)

Mason, James P.; Woods, Thomas N.; Caspi, Amir; Chamberlin, Phillip C.; Moore, Christopher; Jones, Andrew; Kohnert, Rick; Li, Xinlin; Palo, Scott; Solomon, Stanley C.

2016-01-01

The miniature x-ray solar spectrometer is a three-unit CubeSat developed at the Laboratory for Atmospheric and Space Physics at the University of Colorado, Boulder. Over 40 students contributed to the project with professional mentorship and technical contributions from professors in the Aerospace Engineering Sciences Department at University of Colorado, Boulder and from Laboratory for Atmospheric and Space Physics scientists and engineers. The scientific objective of the miniature x-ray solar spectrometer is to study processes in the dynamic sun, from quiet sun to solar flares, and to further understand how these changes in the sun influence the Earth's atmosphere by providing unique spectral measurements of solar soft x-rays. The enabling technology providing the advanced solar soft x-ray spectral measurements is the Amptek X123, a commercial off-the-shelf silicon drift detector. The Amptek X123 has a low mass (approx. 324 g after modification), modest power consumption (approx. 2.50 W), and small volume (6.86 x 9.91 x 2.54 cm), making it ideal for a CubeSat. This paper provides an overview of the miniature x-ray solar spectrometer mission: the science objectives, project history, subsystems, and lessons learned, which can be useful for the small-satellite community.

Planetary X-ray studies: past, present and future

NASA Astrophysics Data System (ADS)

Branduardi-Raymont, Graziella

2016-07-01

Our solar system is a fascinating physics laboratory and X-ray observations are now firmly established as a powerful diagnostic tool of the multiple processes taking place in it. The science that X-rays reveal encompasses solar, space plasma and planetary physics, and the response of bodies in the solar system to the impact of the Sun's activity. This talk will review what we know from past observations and what we expect to learn in the short, medium and long term. Observations with Chandra and XMM-Newton have demonstrated that the origin of Jupiter's bright soft X-ray aurorae lies in the Charge eXchange (CX) process, likely to involve the interaction with atmospheric neutrals of local magnetospheric ions, as well as those carried in the solar wind. At higher energies electron bremsstrahlung is thought to be the X-ray emitting mechanism, while the whole planetary disk acts as a mirror for the solar X-ray flux via Thomson and fluorescent scattering. This 'X-ray mirror' phenomenon is all that is observed from Saturn's disk, which otherwise lacks X-ray auroral features. The Earth's X-ray aurora is bright and variable and mostly due to electron bremsstrahlung and line emission from atmospheric species. Un-magnetised planets, Venus and Mars, do not show X-ray aurorae but display the interesting combination of mirroring the solar X-ray flux and producing X-rays by Solar Wind Charge eXchange (SWCX) in their exospheres. These processes respond to different solar stimulation (photons and solar wind plasma respectively) hence their relative contributions are seen to vary according to the Sun's output. Present and future of planetary X-ray studies are very bright. We are preparing for the arrival of the Juno mission at Jupiter this summer and for coordinated observations with Chandra and XMM-Newton on the approach and later during Juno's orbital phase. These will allow direct correlation of the local plasma conditions with the X-ray emissions and the establishment of the

X-ray lithography source

DOEpatents

Piestrup, M.A.; Boyers, D.G.; Pincus, C.

1991-12-31

A high-intensity, inexpensive X-ray source for X-ray lithography for the production of integrated circuits is disclosed. Foil stacks are bombarded with a high-energy electron beam of 25 to 250 MeV to produce a flux of soft X-rays of 500 eV to 3 keV. Methods of increasing the total X-ray power and making the cross section of the X-ray beam uniform are described. Methods of obtaining the desired X-ray-beam field size, optimum frequency spectrum and eliminating the neutron flux are all described. A method of obtaining a plurality of station operation is also described which makes the process more efficient and economical. The satisfying of these issues makes transition radiation an excellent moderate-priced X-ray source for lithography. 26 figures.

X-ray lithography source

DOEpatents

Piestrup, Melvin A.; Boyers, David G.; Pincus, Cary

1991-01-01

A high-intensity, inexpensive X-ray source for X-ray lithography for the production of integrated circuits. Foil stacks are bombarded with a high-energy electron beam of 25 to 250 MeV to produce a flux of soft X-rays of 500 eV to 3 keV. Methods of increasing the total X-ray power and making the cross section of the X-ray beam uniform are described. Methods of obtaining the desired X-ray-beam field size, optimum frequency spectrum and elminating the neutron flux are all described. A method of obtaining a plurality of station operation is also described which makes the process more efficient and economical. The satisfying of these issues makes transition radiation an exellent moderate-priced X-ray source for lithography.

Bone cartilage imaging with x-ray interferometry using a practical x-ray tube

NASA Astrophysics Data System (ADS)

Kido, Kazuhiro; Makifuchi, Chiho; Kiyohara, Junko; Itou, Tsukasa; Honda, Chika; Momose, Atsushi

2010-04-01

The purpose of this study was to design an X-ray Talbot-Lau interferometer for the imaging of bone cartilage using a practical X-ray tube and to develop that imaging system for clinical use. Wave-optics simulation was performed to design the interferometer with a practical X-ray tube, a source grating, two X-ray gratings, and an X-ray detector. An imaging system was created based on the results of the simulation. The specifications were as follows: the focal spot size was 0.3 mm of an X-ray tube with a tungsten anode (Toshiba, Tokyo, Japan). The tube voltage was set at 40 kVp with an additive aluminum filter, and the mean energy was 31 keV. The pixel size of the X-ray detector, a Condor 486 (Fairchild Imaging, California, USA), was 15 μm. The second grating was a Ronchi-type grating whose pitch was 5.3 μm. Imaging performance of the system was examined with X-ray doses of 0.5, 3 and 9 mGy so that the bone cartilage of a chicken wing was clearly depicted with X-ray doses of 3 and 9 mGy. This was consistent with the simulation's predictions. The results suggest that X-ray Talbot-Lau interferometry would be a promising tool in detecting soft tissues in the human body such as bone cartilage for the X-ray image diagnosis of rheumatoid arthritis. Further optimization of the system will follow to reduce the X-ray dose for clinical use.

Bandpass x-ray diode and x-ray multiplier detector

DOEpatents

Wang, C.L.

1982-09-27

An absorption-edge of an x-ray absorption filter and a quantum jump of a photocathode determine the bandpass characteristics of an x-ray diode detector. An anode, which collects the photoelectrons emitted by the photocathode, has enhanced amplification provided by photoelectron-multiplying means which include dynodes or a microchannel-plate electron-multiplier. Suppression of undesired high frequency response for a bandpass x-ray diode is provided by subtracting a signal representative of energies above the passband from a signal representative of the overall response of the bandpass diode.

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.

X-ray diffraction study of the caged magnetic compound DyFe 2 Zn 20 at low temperatures

NASA Astrophysics Data System (ADS)

Ohashi, M.; Ohashi, K.; Sawabu, M.; Miyagawa, M.; Maeta, K.; Isikawa, Y.

2018-05-01

We have carried out high-angle X-ray powder diffraction measurements of the caged magnetic compound DyFe2Zn20 at low temperature between 14 and 300 K. Even though a strong magnetic anisotropy exists in the magnetization and magnetic susceptibility due to strong exchange interaction between Fe and Dy, almost all X-ray powder diffraction peaks correspond to Bragg reflections of the cubic structural models not only at room temperature paramagnetic state but also at low temperature magnetic ordering state. The Debye temperature is obtained to be 227 K from the results of the volumetric thermal expansion coefficient, which is approximately coincident with that of CeRu2Zn20 (245 K) and that of pure Zn metal (235 K).

Improving image quality in laboratory x-ray phase-contrast imaging

NASA Astrophysics Data System (ADS)

De Marco, F.; Marschner, M.; Birnbacher, L.; Viermetz, M.; Noël, P.; Herzen, J.; Pfeiffer, F.

2017-03-01

Grating-based X-ray phase-contrast (gbPC) is known to provide significant benefits for biomedical imaging. To investigate these benefits, a high-sensitivity gbPC micro-CT setup for small (≍ 5 cm) biological samples has been constructed. Unfortunately, high differential-phase sensitivity leads to an increased magnitude of data processing artifacts, limiting the quality of tomographic reconstructions. Most importantly, processing of phase-stepping data with incorrect stepping positions can introduce artifacts resembling Moiré fringes to the projections. Additionally, the focal spot size of the X-ray source limits resolution of tomograms. Here we present a set of algorithms to minimize artifacts, increase resolution and improve visual impression of projections and tomograms from the examined setup. We assessed two algorithms for artifact reduction: Firstly, a correction algorithm exploiting correlations of the artifacts and differential-phase data was developed and tested. Artifacts were reliably removed without compromising image data. Secondly, we implemented a new algorithm for flatfield selection, which was shown to exclude flat-fields with strong artifacts. Both procedures successfully improved image quality of projections and tomograms. Deconvolution of all projections of a CT scan can minimize blurring introduced by the finite size of the X-ray source focal spot. Application of the Richardson-Lucy deconvolution algorithm to gbPC-CT projections resulted in an improved resolution of phase-contrast tomograms. Additionally, we found that nearest-neighbor interpolation of projections can improve the visual impression of very small features in phase-contrast tomograms. In conclusion, we achieved an increase in image resolution and quality for the investigated setup, which may lead to an improved detection of very small sample features, thereby maximizing the setup's utility.

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

X-Ray

MedlinePlus

... of gray. For some types of X-ray tests, a contrast medium — such as iodine or barium — is introduced into your body to provide greater detail on the images. Why it's done X-ray technology is used to examine many parts of the ...

Hard x-ray phase contrastmicroscopy - techniques and applications

NASA Astrophysics Data System (ADS)

Holzner, Christian

In 1918, Einstein provided the first description of the nature of the refractive index for X-rays, showing that phase contrast effects are significant. A century later, most x-ray microscopy and nearly all medical imaging remains based on absorption contrast, even though phase contrast offers orders of magnitude improvements in contrast and reduced radiation exposure at multi-keV x-ray energies. The work presented is concerned with developing practical and quantitative methods of phase contrast for x-ray microscopy. A theoretical framework for imaging in phase contrast is put forward; this is used to obtain quantitative images in a scanning microscope using a segmented detector, and to correct for artifacts in a commercial phase contrast x-ray nano-tomography system. The principle of reciprocity between scanning and full-field microscopes is then used to arrive at a novel solution: Zernike contrast in a scanning microscope. These approaches are compared on a theoretical and experimental basis in direct connection with applications using multi-keV x-ray microscopes at the Advanced Photon Source at Argonne National Laboratory. Phase contrast provides the best means to image mass and ultrastructure of light elements that mainly constitute biological matter, while stimulated x-ray fluorescence provides high sensitivity for studies of the distribution of heavier trace elements, such as metals. These approaches are combined in a complementary way to yield quantitative maps of elemental concentration from 2D images, with elements placed in their ultrastructural context. The combination of x-ray fluorescence and phase contrast poses an ideal match for routine, high resolution tomographic imaging of biological samples in the future. The presented techniques and demonstration experiments will help pave the way for this development.

X-ray luminescence computed tomography using a focused x-ray beam.

PubMed

Zhang, Wei; Lun, Michael C; Nguyen, Alex Anh-Tu; Li, Changqing

2017-11-01

Due to the low x-ray photon utilization efficiency and low measurement sensitivity of the electron multiplying charge coupled device camera setup, the collimator-based narrow beam x-ray luminescence computed tomography (XLCT) usually requires a long measurement time. We, for the first time, report a focused x-ray beam-based XLCT imaging system with measurements by a single optical fiber bundle and a photomultiplier tube (PMT). An x-ray tube with a polycapillary lens was used to generate a focused x-ray beam whose x-ray photon density is 1200 times larger than a collimated x-ray beam. An optical fiber bundle was employed to collect and deliver the emitted photons on the phantom surface to the PMT. The total measurement time was reduced to 12.5 min. For numerical simulations of both single and six fiber bundle cases, we were able to reconstruct six targets successfully. For the phantom experiment, two targets with an edge-to-edge distance of 0.4 mm and a center-to-center distance of 0.8 mm were successfully reconstructed by the measurement setup with a single fiber bundle and a PMT. (2017) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE).

Preparation of relatively clean carbon backings used in charged particle induced x-ray studies for x-rays below 4 KeV

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

Kocur, P.; Duggan, J.L.; McDaniel, F.D.

1983-04-01

In a recent series of studies of M-shell ionization induced by protons, alpha particles, and fluorine ions, an unmanageable background of low energy contaminant x rays was observed. These K-shell x rays were primarily from Ca, K, Cl, S, P, Si and Na. The energy range of these contaminants is from 3.691 to 1.041 keV. The M-shell x rays being studied were for various elements from U ( about 3.5 keV) down to Eu (1.5 keV). In order to evaluate and reduce the problem, the contaminants for carbon foils from a number of different manufacturers and a wide variety ofmore » foil float-off procedures have been studied. Carbon foils have been produced in our laboratory using carbon rods from several different manufacturers. In this paper, techniques will be described that are most appropriate to reduce the above contaminants to a reasonable level. These techniques should be useful in trace element analysis (PIXE) studies and fundamental ionization measurements for low x-ray energies.« less

X-ray mirror development and testing for the ATHENA mission

NASA Astrophysics Data System (ADS)

Della Monica Ferreira, Desiree; Jakobsen, Anders C.; Massahi, Sonny; Christensen, Finn E.; Shortt, Brian; Garnæs, Jørgen; Torras-Rosell, Antoni; Krumrey, Michael; Cibik, Levent; Marggraf, Stefanie

2016-07-01

This study reports development and testing of coatings on silicon pore optics (SPO) substrates including pre and post coating characterisation of the x-ray mirrors using Atomic Force Microscopy (AFM) and X-ray reflectometry (XRR) performed at the 8 keV X-ray facility at DTU Space and with synchrotron radiation in the laboratory of PTB at BESSY II. We report our findings on surface roughness and coating reflectivity of Ir/B4C coatings considering the grazing incidence angles and energies of ATHENA and long term stability of Ir/B4C, Pt/B4C, W/Si and W/B4C coatings.

X-ray Observations of Cosmic Ray Acceleration

NASA Technical Reports Server (NTRS)

Petre, Robert

2012-01-01

Since the discovery of cosmic rays, detection of their sources has remained elusive. A major breakthrough has come through the identification of synchrotron X-rays from the shocks of supernova remnants through imaging and spectroscopic observations by the most recent generation of X-ray observatories. This radiation is most likely produced by electrons accelerated to relativistic energy, and thus has offered the first, albeit indirect, observational evidence that diffusive shock acceleration in supernova remnants produces cosmic rays to TeV energies, possibly as high as the "knee" in the cosmic ray spectrum. X-ray observations have provided information about the maximum energy to which these shOCks accelerate electrons, as well as indirect evidence of proton acceleration. Shock morphologies measured in X-rays have indicated that a substantial fraction of the shock energy can be diverted into particle acceleration. This presentation will summarize what we have learned about cosmic ray acceleration from X-ray observations of supernova remnants over the past two decades.

The Focusing Optics Solar X-ray Imager (FOXSI)

NASA Astrophysics Data System (ADS)

Christe, Steven; Glesener, L.; Krucker, S.; Ramsey, B.; Ishikawa, S.; Takahashi, T.; Tajima, H.

2010-05-01

The Focusing Optics x-ray Solar Imager (FOXSI) is a sounding rocket payload funded under the NASA Low Cost Access to Space program to test hard x-ray focusing optics and position-sensitive solid state detectors for solar observations. Today's leading solar hard x-ray instrument, the Reuven Ramaty High Energy Solar Spectroscopic Imager (RHESSI) provides excellent spatial (2 arcseconds) and spectral (1 keV) resolution. Yet, due to its use of indirect imaging, the derived images have a low dynamic range (<30) and sensitivity. These limitations make it difficult to study faint x-ray sources in the solar corona which are crucial for understanding the solar flare acceleration process. Grazing-incidence x-ray focusing optics combined with position-sensitive solid state detectors can overcome both of these limitations enabling the next breakthrough in understanding particle acceleration in solar flares. The FOXSI project is led by the Space Science Laboratory at the University of California. The NASA Marshall Space Flight Center, with experience from the HERO balloon project, is responsible for the grazing-incidence optics, while the Astro H team (JAXA/ISAS) will provide double-sided silicon strip detectors. FOXSI will be a pathfinder for the next generation of solar hard x-ray spectroscopic imagers. Such observatories will be able to image the non-thermal electrons within the solar flare acceleration region, trace their paths through the corona, and provide essential quantitative measurements such as energy spectra, density, and energy content in accelerated electrons.

The Focusing Optics X-ray Solar Imager (FOXSI)

NASA Astrophysics Data System (ADS)

Krucker, Sam; Christe, Steven; Glesener, Lindsay; McBride, Steve; Turin, Paul; Glaser, David; Saint-Hilaire, Pascal; Delory, Gregory; Lin, R. P.; Gubarev, Mikhail; Ramsey, Brian; Terada, Yukikatsu; Ishikawa, Shin-Nosuke; Kokubun, Motohide; Saito, Shinya; Takahashi, Tadayuki; Watanabe, Shin; Nakazawa, Kazuhiro; Tajima, Hiroyasu; Masuda, Satoshi; Minoshima, Takashi; Shomojo, Masumi

2009-08-01

The Focusing Optics x-ray Solar Imager (FOXSI) is a sounding rocket payload funded under the NASA Low Cost Access to Space program to test hard x-ray focusing optics and position-sensitive solid state detectors for solar observations. Today's leading solar hard x-ray instrument, the Reuven Ramaty High Energy Solar Spectroscopic Imager (RHESSI) provides excellent spatial (2 arcseconds) and spectral (1 keV) resolution. Yet, due to its use of indirect imaging, the derived images have a low dynamic range (<30) and sensitivity. These limitations make it difficult to study faint x-ray sources in the solar corona which are crucial for understanding the solar flare acceleration process. Grazing-incidence x-ray focusing optics combined with position-sensitive solid state detectors can overcome both of these limitations enabling the next breakthrough in understanding particle acceleration in solar flares. The FOXSI project is led by the Space Science Laboratory at the University of California. The NASA Marshall Space Flight Center, with experience from the HERO balloon project, is responsible for the grazing-incidence optics, while the Astro H team (JAXA/ISAS) will provide double-sided silicon strip detectors. FOXSI will be a pathfinder for the next generation of solar hard x-ray spectroscopic imagers. Such observatories will be able to image the non-thermal electrons within the solar flare acceleration region, trace their paths through the corona, and provide essential quantitative measurements such as energy spectra, density, and energy content in accelerated electrons.

The Focusing Optics Solar X-ray Imager (FOXSI)

NASA Astrophysics Data System (ADS)

Christe, S.; Glesener, L.; Krucker, S.; Ramsey, B.; Ishikawa, S.; Takahashi, T.

2009-12-01

The Focusing Optics x-ray Solar Imager is a sounding rocket payload funded under the NASA Low Cost Access to Space program to test hard x-ray focusing optics and position-sensitive solid state detectors for solar observations. Today's leading solar hard x-ray instrument, the Reuven Ramaty High Energy Solar Spectroscopic Imager provides excellent spatial (2 arcseconds) and spectral (1~keV) resolution. Yet, due to its use of indirect imaging, the derived images have a low dynamic range (<30) and sensitivity. These limitations make it difficult to study faint x-ray sources in the solar corona which are crucial for understanding the solar flare acceleration process. Grazing-incidence x-ray focusing optics combined with position-sensitive solid state detectors can overcome both of these limitations enabling the next breakthrough in understanding particle acceleration in solar flares. The foxsi project is led by the Space Science Laboratory at the University of California. The NASA Marshall Space Flight Center, with experience from the HERO balloon project, is responsible for the grazing-incidence optics, while the Astro H team (JAXA/ISAS) will provide double-sided silicon strip detectors. FOXSI will be a pathfinder for the next generation of solar hard x-ray spectroscopic imagers. Such observatories will be able to image the non-thermal electrons within the solar flare acceleration region, trace their paths through the corona, and provide essential quantitative measurements such as energy spectra, density, and energy content in accelerated electrons.

Portable X-Ray, K-Edge Heavy Metal Detector

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

Fricke, V.

The X-Ray, K-Edge Heavy Metal Detection System was designed and built by Ames Laboratory and the Center for Nondestructive Evaluation at Iowa State University. The system uses a C-frame inspection head with an X-ray tube mounted on one side of the frame and an imaging unit and a high purity germanium detector on the other side. the inspection head is portable and can be easily positioned around ventilation ducts and pipes up to 36 inches in diameter. Wide angle and narrow beam X-ray shots are used to identify the type of holdup material and the amount of the contaminant. Precisemore » assay data can be obtained within minutes of the interrogation. A profile of the containerized holdup material and a permanent record of the measurement are immediately available.« less

Spectroscopic observations of X-ray selected late type stars

NASA Technical Reports Server (NTRS)

Takalo, L. O.

1988-01-01

A spectroscopic survey of nine X-ray selected late type stars was conducted. These stars are serendipitously discovered EINSTEIN X-ray sources, selected from two large x-ray surveys: the Columbia Astrophysical Laboratory survey (five stars) and the CFA Medium Sensitivity survey (four stars). Four of the Columbia survey stars were found to be short period binaries. The fifth was found to be an active single G dwarf. None of the Medium Sensitivity survey stars were found to be either binaries or active stars. Activity was measured by comparing the H-alpha and the CaII infrared triplet (8498, 8542) lines in these stars to the lines in inactive stars of similar spectral type. A correlation was found between the excess H-alpha lime emission and V sin(i) and between the excess H-alpha line emission and X-ray luminosity. No correlation was found between the infrared line emission and any other measured quantity.

X ray reflection masks: Manufacturing, characterization and first tests

NASA Astrophysics Data System (ADS)

Rahn, Stephen

1992-09-01

SXPL (Soft X-ray Projection Lithography) multilayer mirrors are characterized, laterally structured and then used as reflection masks in a projecting lithography procedure. Mo/Si-multilayer mirrors with a 2d in the region of 14 nm were characterized by Cu-k(alpha) grazing incidence as well as soft X-ray normal incidence reflectivity measurements. The multilayer mirrors were patterned by reactive ion etching with CF4 using a photoresist as etch mask, thus producing X-ray reflection masks. The masks were tested at the synchrotron radiation laboratory of the electron accelerator ELSA. A double crystal X-ray monochromator was modified so as to allow about 0.5 sq cm of the reflection mask to be illuminated by white synchrotron radiation. The reflected patterns were projected (with an energy of 100 eV) onto a resist and structure sizes down to 8 micrometers were nicely reproduced. Smaller structures were distorted by Fresnel-diffraction. The theoretically calculated diffraction images agree very well with the observed images.

Powder X-ray diffraction method for the quantification of cocrystals in the crystallization mixture.

PubMed

Padrela, Luis; de Azevedo, Edmundo Gomes; Velaga, Sitaram P

2012-08-01

The solid state purity of cocrystals critically affects their performance. Thus, it is important to accurately quantify the purity of cocrystals in the final crystallization product. The aim of this study was to develop a powder X-ray diffraction (PXRD) quantification method for investigating the purity of cocrystals. The method developed was employed to study the formation of indomethacin-saccharin (IND-SAC) cocrystals by mechanochemical methods. Pure IND-SAC cocrystals were geometrically mixed with 1:1 w/w mixture of indomethacin/saccharin in various proportions. An accurately measured amount (550 mg) of the mixture was used for the PXRD measurements. The most intense, non-overlapping, characteristic diffraction peak of IND-SAC was used to construct the calibration curve in the range 0-100% (w/w). This calibration model was validated and used to monitor the formation of IND-SAC cocrystals by liquid-assisted grinding (LAG). The IND-SAC cocrystal calibration curve showed excellent linearity (R(2) = 0.9996) over the entire concentration range, displaying limit of detection (LOD) and limit of quantification (LOQ) values of 1.23% (w/w) and 3.74% (w/w), respectively. Validation results showed excellent correlations between actual and predicted concentrations of IND-SAC cocrystals (R(2) = 0.9981). The accuracy and reliability of the PXRD quantification method depend on the methods of sample preparation and handling. The crystallinity of the IND-SAC cocrystals was higher when larger amounts of methanol were used in the LAG method. The PXRD quantification method is suitable and reliable for verifying the purity of cocrystals in the final crystallization product.

Method for spatially modulating X-ray pulses using MEMS-based X-ray optics

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

Lopez, Daniel; Shenoy, Gopal; Wang, Jin

A method and apparatus are provided for spatially modulating X-rays or X-ray pulses using microelectromechanical systems (MEMS) based X-ray optics. A torsionally-oscillating MEMS micromirror and a method of leveraging the grazing-angle reflection property are provided to modulate X-ray pulses with a high-degree of controllability.

X-ray monitoring optical elements

DOEpatents

Stoupin, Stanislav; Shvydko, Yury; Katsoudas, John; Blank, Vladimir D.; Terentyev, Sergey A.

2016-12-27

An X-ray article and method for analyzing hard X-rays which have interacted with a test system. The X-ray article is operative to diffract or otherwise process X-rays from an input X-ray beam which have interacted with the test system and at the same time provide an electrical circuit adapted to collect photoelectrons emitted from an X-ray optical element of the X-ray article to analyze features of the test system.

Laboratory experiments on soft x-ray emissions from the solar wind

NASA Astrophysics Data System (ADS)

Kanda, T.; Ohashi, H.; Maeno, S.; Ishida, T.; Tanuma, H.; Akamatsu, H.; Abe, Y.; Yokota, W.; Henmi, K.; Ishisaki, Y.; Ezoe, Y.; Ohashi, T.; Shinozaki, K.; Mitsuda, K.

2011-06-01

We have observed emission spectra in collisions of hydrogen-like oxygen and nitrogen ions with a helium target gas in the soft x-ray region using a window-less Si(Li) detector at collision energies of about 100 keV. The dominant soft x-ray emission is the 1s2-1s2p transition of helium-like ions produced by a single-electron capture reaction. We indicate that the cascades from the upper states give a large population of the 2p state, even though direct capture into the 2p state is much smaller than the 3ell and 4ell states. The intensity ratios of the 1s-2p and 1s-3p transitions are discussed, along with a comparison with the theoretical calculation.

Optical and X-ray studies of Compact X-ray Binaries in NGC 5904

NASA Astrophysics Data System (ADS)

Bhalotia, Vanshree; Beck-Winchatz, Bernhard

2018-06-01

Due to their high stellar densities, globular cluster systems trigger various dynamical interactions, such as the formation of compact X-ray binaries. Stellar collisional frequencies have been correlated to the number of X-ray sources detected in various clusters and we hope to measure this correlation for NGC 5904. Optical fluxes of sources from archival HST images of NGC 5904 have been measured using a DOLPHOT PSF photometry in the UV, optical and near-infrared. We developed a data analysis pipeline to process the fluxes of tens of thousands of objects using awk, python and DOLPHOT. We plot color magnitude diagrams in different photometric bands in order to identify outliers that could be X-ray binaries, since they do not evolve the same way as singular stars. Aligning previously measured astrometric data for X-ray sources in NGC 5904 from Chandra with archival astrometric data from HST will filter out the outlier objects that are not X-ray producing, and provide a sample of compact binary systems that are responsible for X-ray emission in NGC 5904. Furthermore, previously measured X-ray fluxes of NGC 5904 from Chandra have also been used to measure the X-ray to optical flux ratio and identify the types of compact X-ray binaries responsible for the X-ray emissions in NGC 5904. We gratefully acknowledge the support from the Illinois Space Grant Consortium.

Structure and collective dynamics of hydrated anti-freeze protein type III from 180 K to 298 K by X-ray diffraction and inelastic X-ray scattering

NASA Astrophysics Data System (ADS)

Yoshida, Koji; Baron, Alfred Q. R.; Uchiyama, Hiroshi; Tsutsui, Satoshi; Yamaguchi, Toshio

2016-04-01

We investigated hydrated antifreeze protein type III (AFP III) powder with a hydration level h (=mass of water/mass of protein) of 0.4 in the temperature range between 180 K and 298 K using X-ray diffraction and inelastic X-ray scattering (IXS). The X-ray diffraction data showed smooth, largely monotonic changes between 180 K and 298 K without freezing water. Meanwhile, the collective dynamics observed by IXS showed a strong change in the sound velocity at 180 K, after being largely temperature independent at higher temperatures (298-220 K). We interpret this change in terms of the dynamic transition previously discussed using other probes including THz IR absorption spectroscopy and incoherent elastic and quasi-elastic neutron scattering. This finding suggests that the dynamic transition of hydrated proteins is observable on the subpicosecond time scale as well as nano- and pico-second scales, both in collective dynamics from IXS and single particle dynamics from neutron scattering. Moreover, it is most likely that the dynamic transition of hydrated AFP III is not directly correlated with its hydration structure.

Structure and collective dynamics of hydrated anti-freeze protein type III from 180 K to 298 K by X-ray diffraction and inelastic X-ray scattering.

PubMed

Yoshida, Koji; Baron, Alfred Q R; Uchiyama, Hiroshi; Tsutsui, Satoshi; Yamaguchi, Toshio

2016-04-07

We investigated hydrated antifreeze protein type III (AFP III) powder with a hydration level h (=mass of water/mass of protein) of 0.4 in the temperature range between 180 K and 298 K using X-ray diffraction and inelastic X-ray scattering (IXS). The X-ray diffraction data showed smooth, largely monotonic changes between 180 K and 298 K without freezing water. Meanwhile, the collective dynamics observed by IXS showed a strong change in the sound velocity at 180 K, after being largely temperature independent at higher temperatures (298-220 K). We interpret this change in terms of the dynamic transition previously discussed using other probes including THz IR absorption spectroscopy and incoherent elastic and quasi-elastic neutron scattering. This finding suggests that the dynamic transition of hydrated proteins is observable on the subpicosecond time scale as well as nano- and pico-second scales, both in collective dynamics from IXS and single particle dynamics from neutron scattering. Moreover, it is most likely that the dynamic transition of hydrated AFP III is not directly correlated with its hydration structure.

Detection of nanoscale embedded layers using laboratory specular X-ray diffraction

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

Beekman, Matt, E-mail: matt.beekman@oit.edu; Rodriguez, Gabriel; Atkins, Ryan

Unusual specular X-ray diffraction patterns have been observed from certain thin film intergrowths of metal monochalcogenide (MX) and transition metal dichalcogenide (TX{sub 2}) structures. These patterns exhibit selective “splitting” or broadening of selected (00l) diffraction peaks, while other (00l) reflections remain relatively unaffected [Atkins et al., Chem. Mater. 24, 4594 (2012)]. Using a simplified optical model in the kinematic approximation, we illustrate that these peculiar and somewhat counterintuitive diffraction features can be understood in terms of additional layers of one of the intergrowth components, MX or TX{sub 2}, interleaved between otherwise “ideal” regions of MX-TX{sub 2} intergrowth. The interpretation ismore » in agreement with scanning transmission electron microscope imaging, which reveals the presence of such stacking “defects” in films prepared from non-ideal precursors. In principle, the effect can be employed as a simple, non-destructive laboratory probe to detect and characterize ultrathin layers of one material, e.g., 2-dimensional crystals, embedded between two slabs of a second material, effectively using the two slabs as a highly sensitive interferometer of their separation distance.« less

Neutron and X-ray diffraction of plasma-sprayed zirconia-yttria thermal barrier coatings

NASA Technical Reports Server (NTRS)

Shankar, N. R.; Herman, H.; Singhal, S. P.; Berndt, C. C.

1984-01-01

ZrO2-7.8mol. pct. YO1.5, a fused powder, and ZrO2-8.7mol. pct. YO1.5, a prereacted powder, were plasma-sprayed onto steel substrates. Neutron diffraction and X-ray diffraction of the as-received powder, the powder plasma sprayed into water, as-sprayed coatings, and coatings heat-treated for 10 and 100 h were carried out to study phase transformations and ordering of the oxygen ions on the oxygen sublattice. The as-received fused powder has a much lower monoclinic percentage than does the pre-reacted powder, this resulting in a much lower monoclinic percentage in the coating. Heat treatment increases the percentages of the cubic and monoclinic phases, while decreasing the tetragonal content. An ordered tetragonal phase is detected by the presence of extra neutron diffraction peaks. These phase transformations and ordering will result in volume changes. The implications of these transformations on the performance of partially stabilized zirconia thermal barrier coatings is discussed.

X-ray coherent scattering tomography of textured material (Conference Presentation)

NASA Astrophysics Data System (ADS)

Zhu, Zheyuan; Pang, Shuo

2017-05-01

Small-angle X-ray scattering (SAXS) measures the signature of angular-dependent coherently scattered X-rays, which contains richer information in material composition and structure compared to conventional absorption-based computed tomography. SAXS image reconstruction method of a 2 or 3 dimensional object based on computed tomography, termed as coherent scattering computed tomography (CSCT), enables the detection of spatially-resolved, material-specific isotropic scattering signature inside an extended object, and provides improved contrast for medical diagnosis, security screening, and material characterization applications. However, traditional CSCT methods assumes materials are fine powders or amorphous, and possess isotropic scattering profiles, which is not generally true for all materials. Anisotropic scatters cannot be captured using conventional CSCT method and result in reconstruction errors. To obtain correct information from the sample, we designed new imaging strategy which incorporates extra degree of detector motion into X-ray scattering tomography for the detection of anisotropic scattered photons from a series of two-dimensional intensity measurements. Using a table-top, narrow-band X-ray source and a panel detector, we demonstrate the anisotropic scattering profile captured from an extended object and the reconstruction of a three-dimensional object. For materials possessing a well-organized crystalline structure with certain symmetry, the scatter texture is more predictable. We will also discuss the compressive schemes and implementation of data acquisition to improve the collection efficiency and accelerate the imaging process.

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.

Aplanatic Three-Mirror Objective for High-Magnification Soft X-Ray Microscopy

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

Toyoda, M.; Jinno, T.; Yanagihara, M.

2011-09-09

An innovative solution for high-magnification microscopy, based on attaching afocal optics for focal length reduction, is proposed. The solution, consisting of three spherical mirrors, allows one to enhance a magnification of a laboratory based soft x-ray microscope over 1000x, where movies with diffraction-limited resolution can be observed with an x-ray CCD. The design example, having a numerical aperture of 0.25, was successfully demonstrated both a high magnification and a large field of view.

Compact X-ray sources: X-rays from self-reflection

NASA Astrophysics Data System (ADS)

Mangles, Stuart P. D.

2012-05-01

Laser-based particle acceleration offers a way to reduce the size of hard-X-ray sources. Scientists have now developed a simple scheme that produces a bright flash of hard X-rays by using a single laser pulse both to generate and to scatter an electron beam.

Understanding the X-ray spectrum of anomalous X-ray pulsars and soft gamma-ray repeaters

NASA Astrophysics Data System (ADS)

Guo, Yan-Jun; Dai, Shi; Li, Zhao-Sheng; Liu, Yuan; Tong, Hao; Xu, Ren-Xin

2015-04-01

Hard X-rays above 10 keV are detected from several anomalous X-ray pulsars (AXPs) and soft gamma-ray repeaters (SGRs), and different models have been proposed to explain the physical origin within the frame of either a magnetar model or a fallback disk system. Using data from Suzaku and INTEGRAL, we study the soft and hard X-ray spectra of four AXPs/SGRs: 1RXS J170849-400910, 1E 1547.0-5408, SGR 1806-20 and SGR 0501+4516. It is found that the spectra could be well reproduced by the bulk-motion Comptonization (BMC) process as was first suggested by Trümper et al., showing that the accretion scenario could be compatible with X-ray emission from AXPs/SGRs. Simulated results from the Hard X-ray Modulation Telescope using the BMC model show that the spectra would have discrepancies from the power-law, especially the cutoff at ˜200 keV. Thus future observations will allow researchers to distinguish different models of the hard X-ray emission and will help us understand the nature of AXPs/SGRs. Supported by the National Natural Science Foundation of China.

X-Ray modeling of η Carinae & WR 140 from SPH simulations

NASA Astrophysics Data System (ADS)

Russell, Christopher M. P.; Corcoran, Michael F.; Okazaki, Atsuo T.; Madura, Thomas I.; Owocki, Stanley P.

2011-07-01

The colliding wind binary (CWB) systems η Carinae and WR140 provide unique laboratories for X-ray astrophysics. Their wind-wind collisions produce hard X-rays that have been monitored extensively by several X-ray telescopes, including RXTE. To interpret these RXTE X-ray light curves, we apply 3D hydrodynamic simulations of the wind-wind collision using smoothed particle hydrodynamics (SPH). We find adiabatic simulations that account for the absorption of X-rays from an assumed point source of X-ray emission at the apex of the wind-collision shock cone can closely match the RXTE light curves of both η Car and WR140. This point-source model can also explain the early recovery of η Car's X-ray light curve from the 2009.0 minimum by a factor of 2-4 reduction in the mass loss rate of η Car. Our more recent models account for the extended emission and absorption along the full wind-wind interaction shock front. For WR140, the computed X-ray light curves again match the RXTE observations quite well. But for η Car, a hot, post-periastron bubble leads to an emission level that does not match the extended X-ray minimum observed by RXTE. Initial results from incorporating radiative cooling and radiative forces via an anti-gravity approach into the SPH code are also discussed.

Characterization of uranium bearing material using x-ray fluorescence and direct gamma-rays measurement techniques

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

Mujaini, M., E-mail: madihah@uniten.edu.my; Chankow, N.; Yusoff, M. Z.

2016-01-22

Uranium ore can be easily detected due to various gamma-ray energies emitted from uranium daughters particularly from {sup 238}U daughters such as {sup 214}Bi, {sup 214}Pb and {sup 226}Ra. After uranium is extracted from uranium ore, only low energy gamma-rays emitted from {sup 235}U may be detected if the detector is placed in close contact to the specimen. In this research, identification and characterization of uranium bearing materials is experimentally investigated using direct measurement of gamma-rays from {sup 235}U in combination with the x-ray fluorescence (XRF) technique. Measurement of gamma-rays can be conducted by using high purity germanium (HPGe) detectormore » or cadmium telluride (CdTe) detector while a {sup 57}Coradioisotope-excited XRF spectrometer using CdTe detector is used for elemental analysis. The proposed technique was tested with various uranium bearing specimens containing natural, depleted and enriched uranium in both metallic and powder forms.« less

Atomic Data Needs for X-ray Astronomy

NASA Technical Reports Server (NTRS)

Bautista, Manuel A. (Editor); Kallman, Timothy R. (Editor); Pradhan, Anil K. (Editor)

2000-01-01

This publication contains written versions of most of the invited talks presented at the workshop on "Atomic Data Needs for X-ray Astronomy," which was held at NASA's Goddard Space Flight Center on December 16-17, 1999. The workshop was divided into five major areas: Observational Spectroscopy, Theoretical Calculations of Atomic Data, Laboratory Measurements of Atomic Parameters, Spectra Modeling, and Atomic Databases. These proceedings are expected to be of interest to producers and users of atomic data. Moreover, the contributions presented here have been written in a way that can be used by a general audience of scientists and graduate students in X-ray astronomy, modelling, and in computational and experimental atomic physics.

X-band RF gun and linac for medical Compton scattering X-ray source