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 transformation coinciding with the loss of the remaining bound water molecule. These temperature-resolved real-time powder X-ray diffraction studies provide the first comprehensive description of the sepiolite structure and the complex changes it undergoes as it dehydrates. Additional heating and cooling in situ powder X-ray diffraction experiments are underway in order to investigate the relative stabilities and rehydration behaviors of the partially-hydrated sepiolite phases. The results of these studies should provide a more robust model for predicting and modifying the properties and applications of this critical industrial material and environmentally important mineral.

xMDFF: molecular dynamics flexible fitting of low-resolution X-ray structures.

PubMed

McGreevy, Ryan; Singharoy, Abhishek; Li, Qufei; Zhang, Jingfen; Xu, Dong; Perozo, Eduardo; Schulten, Klaus

2014-09-01

X-ray crystallography remains the most dominant method for solving atomic structures. However, for relatively large systems, the availability of only medium-to-low-resolution diffraction data often limits the determination of all-atom details. A new molecular dynamics flexible fitting (MDFF)-based approach, xMDFF, for determining structures from such low-resolution crystallographic data is reported. xMDFF employs a real-space refinement scheme that flexibly fits atomic models into an iteratively updating electron-density map. It addresses significant large-scale deformations of the initial model to fit the low-resolution density, as tested with synthetic low-resolution maps of D-ribose-binding protein. xMDFF has been successfully applied to re-refine six low-resolution protein structures of varying sizes that had already been submitted to the Protein Data Bank. Finally, via systematic refinement of a series of data from 3.6 to 7 Å resolution, xMDFF refinements together with electrophysiology experiments were used to validate the first all-atom structure of the voltage-sensing protein Ci-VSP.

Simultaneous use of solution NMR and X-ray data in REFMAC5 for joint refinement/detection of structural differences.

PubMed

Rinaldelli, Mauro; Ravera, Enrico; Calderone, Vito; Parigi, Giacomo; Murshudov, Garib N; Luchinat, Claudio

2014-04-01

The program REFMAC5 from CCP4 was modified to allow the simultaneous use of X-ray crystallographic data and paramagnetic NMR data (pseudocontact shifts and self-orientation residual dipolar couplings) and/or diamagnetic residual dipolar couplings. Incorporation of these long-range NMR restraints in REFMAC5 can reveal differences between solid-state and solution conformations of molecules or, in their absence, can be used together with X-ray crystallographic data for structural refinement. Since NMR and X-ray data are complementary, when a single structure is consistent with both sets of data and still maintains reasonably `ideal' geometries, the reliability of the derived atomic model is expected to increase. The program was tested on five different proteins: the catalytic domain of matrix metalloproteinase 1, GB3, ubiquitin, free calmodulin and calmodulin complexed with a peptide. In some cases the joint refinement produced a single model consistent with both sets of observations, while in other cases it indicated, outside the experimental uncertainty, the presence of different protein conformations in solution and in the solid state.

Investigation of Synthetic Mg(1.3)V(1.7)O4 Spinel with MgO Inclusions: Case Study of a Spinel with an Apparently occupied Interstitial Site

NASA Technical Reports Server (NTRS)

Uchida, Hinako; Righter, Kevin; Lavina, Barbara; Nowell, Matthew M.; Wright, Stuart I.; Downs, Robert T.; Yang, Hexiong

2007-01-01

A magnesium vanadate spinel crystal, ideally MgV2O4, synthesized at 1 bar, 1200 C and equilibrated under FMQ + 1.3 log f(sub o2) condition, was investigated using single-crystal X-ray diffraction, electron microprobe, and electron backscatter (EBSD). The initial X-ray structure refinements gave tetrahedral and octahedral site occupancies, along with the presence of 0.053 apfu Mg at an interstitial octahedral site . Back-scattered electron (BSE) images and electron microprobe analyses revealed the existence of an Mg-rich phase in the spinel matrix, which was too small (less than or equal to 3microns) for an accurate chemical determination. The EBSD analysis combined with X-ray energy dispersive spectroscop[y (XEDS) suggested that the Mg-rich inclusions are periclase oriented coherently with the spinel matrix. The final structure refinements were optimized by subtracting the X-ray intensity contributions (approx. 9%) of periclase reflections, which eliminated the interstitial Mg. This study provides insight into possible origins of refined interstitial cations reported in the the literature for spinel, and points to the difficulty of using only X-ray diffraction data to distinguish a spinel with interstitial cations from one with coherently oriented MgO inclusions.

Preliminary joint X-ray and neutron protein crystallographic studies of ecDHFR complexed with folate and NADP{sup +}

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

Wan, Qun, E-mail: wqun@yzu.edu.cn; Kovalevsky, Andrey Y.; Wilson, Mark A.

2014-05-25

A 2.0 Å resolution neutron data set and a 1.6 Å resolution X-ray data set were collected for joint X-ray/neutron refinement of the ecDHFR–folate–NADP{sup +} complex in order to study the reaction mechanism of dihydrofolate reductase.

Polarizable atomic multipole X-ray refinement: application to peptide crystals

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

Schnieders, Michael J.; Fenn, Timothy D.; Howard Hughes Medical Institute

2009-09-01

A method to accelerate the computation of structure factors from an electron density described by anisotropic and aspherical atomic form factors via fast Fourier transformation is described for the first time. Recent advances in computational chemistry have produced force fields based on a polarizable atomic multipole description of biomolecular electrostatics. In this work, the Atomic Multipole Optimized Energetics for Biomolecular Applications (AMOEBA) force field is applied to restrained refinement of molecular models against X-ray diffraction data from peptide crystals. A new formalism is also developed to compute anisotropic and aspherical structure factors using fast Fourier transformation (FFT) of Cartesian Gaussianmore » multipoles. Relative to direct summation, the FFT approach can give a speedup of more than an order of magnitude for aspherical refinement of ultrahigh-resolution data sets. Use of a sublattice formalism makes the method highly parallelizable. Application of the Cartesian Gaussian multipole scattering model to a series of four peptide crystals using multipole coefficients from the AMOEBA force field demonstrates that AMOEBA systematically underestimates electron density at bond centers. For the trigonal and tetrahedral bonding geometries common in organic chemistry, an atomic multipole expansion through hexadecapole order is required to explain bond electron density. Alternatively, the addition of interatomic scattering (IAS) sites to the AMOEBA-based density captured bonding effects with fewer parameters. For a series of four peptide crystals, the AMOEBA–IAS model lowered R{sub free} by 20–40% relative to the original spherically symmetric scattering model.« less

Predicting X-ray diffuse scattering from translation–libration–screw structural ensembles

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

Van Benschoten, Andrew H.; Afonine, Pavel V.; Terwilliger, Thomas C.

2015-07-28

A method of simulating X-ray diffuse scattering from multi-model PDB files is presented. Despite similar agreement with Bragg data, different translation–libration–screw refinement strategies produce unique diffuse intensity patterns. Identifying the intramolecular motions of proteins and nucleic acids is a major challenge in macromolecular X-ray crystallography. Because Bragg diffraction describes the average positional distribution of crystalline atoms with imperfect precision, the resulting electron density can be compatible with multiple models of motion. Diffuse X-ray scattering can reduce this degeneracy by reporting on correlated atomic displacements. Although recent technological advances are increasing the potential to accurately measure diffuse scattering, computational modeling andmore » validation tools are still needed to quantify the agreement between experimental data and different parameterizations of crystalline disorder. A new tool, phenix.diffuse, addresses this need by employing Guinier’s equation to calculate diffuse scattering from Protein Data Bank (PDB)-formatted structural ensembles. As an example case, phenix.diffuse is applied to translation–libration–screw (TLS) refinement, which models rigid-body displacement for segments of the macromolecule. To enable the calculation of diffuse scattering from TLS-refined structures, phenix.tls-as-xyz builds multi-model PDB files that sample the underlying T, L and S tensors. In the glycerophosphodiesterase GpdQ, alternative TLS-group partitioning and different motional correlations between groups yield markedly dissimilar diffuse scattering maps with distinct implications for molecular mechanism and allostery. These methods demonstrate how, in principle, X-ray diffuse scattering could extend macromolecular structural refinement, validation and analysis.« less

A grid-enabled web service for low-resolution crystal structure refinement.

PubMed

O'Donovan, Daniel J; Stokes-Rees, Ian; Nam, Yunsun; Blacklow, Stephen C; Schröder, Gunnar F; Brunger, Axel T; Sliz, Piotr

2012-03-01

Deformable elastic network (DEN) restraints have proved to be a powerful tool for refining structures from low-resolution X-ray crystallographic data sets. Unfortunately, optimal refinement using DEN restraints requires extensive calculations and is often hindered by a lack of access to sufficient computational resources. The DEN web service presented here intends to provide structural biologists with access to resources for running computationally intensive DEN refinements in parallel on the Open Science Grid, the US cyberinfrastructure. Access to the grid is provided through a simple and intuitive web interface integrated into the SBGrid Science Portal. Using this portal, refinements combined with full parameter optimization that would take many thousands of hours on standard computational resources can now be completed in several hours. An example of the successful application of DEN restraints to the human Notch1 transcriptional complex using the grid resource, and summaries of all submitted refinements, are presented as justification.

Hirshfeld atom refinement for modelling strong hydrogen bonds.

PubMed

Woińska, Magdalena; Jayatilaka, Dylan; Spackman, Mark A; Edwards, Alison J; Dominiak, Paulina M; Woźniak, Krzysztof; Nishibori, Eiji; Sugimoto, Kunihisa; Grabowsky, Simon

2014-09-01

High-resolution low-temperature synchrotron X-ray diffraction data of the salt L-phenylalaninium hydrogen maleate are used to test the new automated iterative Hirshfeld atom refinement (HAR) procedure for the modelling of strong hydrogen bonds. The HAR models used present the first examples of Z' > 1 treatments in the framework of wavefunction-based refinement methods. L-Phenylalaninium hydrogen maleate exhibits several hydrogen bonds in its crystal structure, of which the shortest and the most challenging to model is the O-H...O intramolecular hydrogen bond present in the hydrogen maleate anion (O...O distance is about 2.41 Å). In particular, the reconstruction of the electron density in the hydrogen maleate moiety and the determination of hydrogen-atom properties [positions, bond distances and anisotropic displacement parameters (ADPs)] are the focus of the study. For comparison to the HAR results, different spherical (independent atom model, IAM) and aspherical (free multipole model, MM; transferable aspherical atom model, TAAM) X-ray refinement techniques as well as results from a low-temperature neutron-diffraction experiment are employed. Hydrogen-atom ADPs are furthermore compared to those derived from a TLS/rigid-body (SHADE) treatment of the X-ray structures. The reference neutron-diffraction experiment reveals a truly symmetric hydrogen bond in the hydrogen maleate anion. Only with HAR is it possible to freely refine hydrogen-atom positions and ADPs from the X-ray data, which leads to the best electron-density model and the closest agreement with the structural parameters derived from the neutron-diffraction experiment, e.g. the symmetric hydrogen position can be reproduced. The multipole-based refinement techniques (MM and TAAM) yield slightly asymmetric positions, whereas the IAM yields a significantly asymmetric position.

Enabling X-ray free electron laser crystallography for challenging biological systems from a limited number of crystals

DOE PAGES

Uervirojnangkoorn, Monarin; Zeldin, Oliver B.; Lyubimov, Artem Y.; ...

2015-03-17

There is considerable potential for X-ray free electron lasers (XFELs) to enable determination of macromolecular crystal structures that are difficult to solve using current synchrotron sources. Prior XFEL studies often involved the collection of thousands to millions of diffraction images, in part due to limitations of data processing methods. We implemented a data processing system based on classical post-refinement techniques, adapted to specific properties of XFEL diffraction data. When applied to XFEL data from three different proteins collected using various sample delivery systems and XFEL beam parameters, our method improved the quality of the diffraction data as well as themore » resulting refined atomic models and electron density maps. Moreover, the number of observations for a reflection necessary to assemble an accurate data set could be reduced to a few observations. In conclusion, these developments will help expand the applicability of XFEL crystallography to challenging biological systems, including cases where sample is limited.« less

Enabling X-ray free electron laser crystallography for challenging biological systems from a limited number of crystals

DOE PAGES

Uervirojnangkoorn, Monarin; Zeldin, Oliver B.; Lyubimov, Artem Y.; ...

2015-03-17

There is considerable potential for X-ray free electron lasers (XFELs) to enable determination of macromolecular crystal structures that are difficult to solve using current synchrotron sources. Prior XFEL studies often involved the collection of thousands to millions of diffraction images, in part due to limitations of data processing methods. We implemented a data processing system based on classical post-refinement techniques, adapted to specific properties of XFEL diffraction data. When applied to XFEL data from three different proteins collected using various sample delivery systems and XFEL beam parameters, our method improved the quality of the diffraction data as well as themore » resulting refined atomic models and electron density maps. Moreover, the number of observations for a reflection necessary to assemble an accurate data set could be reduced to a few observations. These developments will help expand the applicability of XFEL crystallography to challenging biological systems, including cases where sample is limited.« less

Enabling X-ray free electron laser crystallography for challenging biological systems from a limited number of crystals

PubMed Central

Uervirojnangkoorn, Monarin; Zeldin, Oliver B; Lyubimov, Artem Y; Hattne, Johan; Brewster, Aaron S; Sauter, Nicholas K; Brunger, Axel T; Weis, William I

2015-01-01

There is considerable potential for X-ray free electron lasers (XFELs) to enable determination of macromolecular crystal structures that are difficult to solve using current synchrotron sources. Prior XFEL studies often involved the collection of thousands to millions of diffraction images, in part due to limitations of data processing methods. We implemented a data processing system based on classical post-refinement techniques, adapted to specific properties of XFEL diffraction data. When applied to XFEL data from three different proteins collected using various sample delivery systems and XFEL beam parameters, our method improved the quality of the diffraction data as well as the resulting refined atomic models and electron density maps. Moreover, the number of observations for a reflection necessary to assemble an accurate data set could be reduced to a few observations. These developments will help expand the applicability of XFEL crystallography to challenging biological systems, including cases where sample is limited. DOI: http://dx.doi.org/10.7554/eLife.05421.001 PMID:25781634

COMPUTATIONAL METHODOLOGIES for REAL-SPACE STRUCTURAL REFINEMENT of LARGE MACROMOLECULAR COMPLEXES

PubMed Central

Goh, Boon Chong; Hadden, Jodi A.; Bernardi, Rafael C.; Singharoy, Abhishek; McGreevy, Ryan; Rudack, Till; Cassidy, C. Keith; Schulten, Klaus

2017-01-01

The rise of the computer as a powerful tool for model building and refinement has revolutionized the field of structure determination for large biomolecular systems. Despite the wide availability of robust experimental methods capable of resolving structural details across a range of spatiotemporal resolutions, computational hybrid methods have the unique ability to integrate the diverse data from multimodal techniques such as X-ray crystallography and electron microscopy into consistent, fully atomistic structures. Here, commonly employed strategies for computational real-space structural refinement are reviewed, and their specific applications are illustrated for several large macromolecular complexes: ribosome, virus capsids, chemosensory array, and photosynthetic chromatophore. The increasingly important role of computational methods in large-scale structural refinement, along with current and future challenges, is discussed. PMID:27145875

Recent Advances in X-ray Cone-beam Computed Laminography.

PubMed

O'Brien, Neil S; Boardman, Richard P; Sinclair, Ian; Blumensath, Thomas

2016-10-06

X-ray computed tomography is an established volume imaging technique used routinely in medical diagnosis, industrial non-destructive testing, and a wide range of scientific fields. Traditionally, computed tomography uses scanning geometries with a single axis of rotation together with reconstruction algorithms specifically designed for this setup. Recently there has however been increasing interest in more complex scanning geometries. These include so called X-ray computed laminography systems capable of imaging specimens with large lateral dimensions or large aspect ratios, neither of which are well suited to conventional CT scanning procedures. Developments throughout this field have thus been rapid, including the introduction of novel system trajectories, the application and refinement of various reconstruction methods, and the use of recently developed computational hardware and software techniques to accelerate reconstruction times. Here we examine the advances made in the last several years and consider their impact on the state of the art.

Super-resolution biomolecular crystallography with low-resolution data.

PubMed

Schröder, Gunnar F; Levitt, Michael; Brunger, Axel T

2010-04-22

X-ray diffraction plays a pivotal role in the understanding of biological systems by revealing atomic structures of proteins, nucleic acids and their complexes, with much recent interest in very large assemblies like the ribosome. As crystals of such large assemblies often diffract weakly (resolution worse than 4 A), we need methods that work at such low resolution. In macromolecular assemblies, some of the components may be known at high resolution, whereas others are unknown: current refinement methods fail as they require a high-resolution starting structure for the entire complex. Determining the structure of such complexes, which are often of key biological importance, should be possible in principle as the number of independent diffraction intensities at a resolution better than 5 A generally exceeds the number of degrees of freedom. Here we introduce a method that adds specific information from known homologous structures but allows global and local deformations of these homology models. Our approach uses the observation that local protein structure tends to be conserved as sequence and function evolve. Cross-validation with R(free) (the free R-factor) determines the optimum deformation and influence of the homology model. For test cases at 3.5-5 A resolution with known structures at high resolution, our method gives significant improvements over conventional refinement in the model as monitored by coordinate accuracy, the definition of secondary structure and the quality of electron density maps. For re-refinements of a representative set of 19 low-resolution crystal structures from the Protein Data Bank, we find similar improvements. Thus, a structure derived from low-resolution diffraction data can have quality similar to a high-resolution structure. Our method is applicable to the study of weakly diffracting crystals using X-ray micro-diffraction as well as data from new X-ray light sources. Use of homology information is not restricted to X-ray crystallography and cryo-electron microscopy: as optical imaging advances to subnanometre resolution, it can use similar tools.

Rietveld Refinement on X-Ray Diffraction Patterns of Bioapatite in Human Fetal Bones

PubMed Central

Meneghini, Carlo; Dalconi, Maria Chiara; Nuzzo, Stefania; Mobilio, Settimio; Wenk, Rudy H.

2003-01-01

Bioapatite, the main constituent of mineralized tissue in mammalian bones, is a calcium-phosphate-based mineral that is similar in structure and composition to hydroxyapatite. In this work, the crystallographic structure of bioapatite in human fetuses was investigated by synchrotron radiation x-ray diffraction (XRD) and microdiffraction (μ-XRD) techniques. Rietveld refinement analyses of XRD and μ-XRD data allow for quantitative probing of the structural modifications of bioapatite as functions of the mineralization process and gestational age. PMID:12609904

Optimization of crystallization conditions for biological macromolecules.

PubMed

McPherson, Alexander; Cudney, Bob

2014-11-01

For the successful X-ray structure determination of macromolecules, it is first necessary to identify, usually by matrix screening, conditions that yield some sort of crystals. Initial crystals are frequently microcrystals or clusters, and often have unfavorable morphologies or yield poor diffraction intensities. It is therefore generally necessary to improve upon these initial conditions in order to obtain better crystals of sufficient quality for X-ray data collection. Even when the initial samples are suitable, often marginally, refinement of conditions is recommended in order to obtain the highest quality crystals that can be grown. The quality of an X-ray structure determination is directly correlated with the size and the perfection of the crystalline samples; thus, refinement of conditions should always be a primary component of crystal growth. The improvement process is referred to as optimization, and it entails sequential, incremental changes in the chemical parameters that influence crystallization, such as pH, ionic strength and precipitant concentration, as well as physical parameters such as temperature, sample volume and overall methodology. It also includes the application of some unique procedures and approaches, and the addition of novel components such as detergents, ligands or other small molecules that may enhance nucleation or crystal development. Here, an attempt is made to provide guidance on how optimization might best be applied to crystal-growth problems, and what parameters and factors might most profitably be explored to accelerate and achieve success.

Optimization of crystallization conditions for biological macromolecules

PubMed Central

McPherson, Alexander; Cudney, Bob

2014-01-01

For the successful X-ray structure determination of macromolecules, it is first necessary to identify, usually by matrix screening, conditions that yield some sort of crystals. Initial crystals are frequently microcrystals or clusters, and often have unfavorable morphologies or yield poor diffraction intensities. It is therefore generally necessary to improve upon these initial conditions in order to obtain better crystals of sufficient quality for X-ray data collection. Even when the initial samples are suitable, often marginally, refinement of conditions is recommended in order to obtain the highest quality crystals that can be grown. The quality of an X-ray structure determination is directly correlated with the size and the perfection of the crystalline samples; thus, refinement of conditions should always be a primary component of crystal growth. The improvement process is referred to as optimization, and it entails sequential, incremental changes in the chemical parameters that influence crystallization, such as pH, ionic strength and precipitant concentration, as well as physical parameters such as temperature, sample volume and overall methodology. It also includes the application of some unique procedures and approaches, and the addition of novel components such as detergents, ligands or other small molecules that may enhance nucleation or crystal development. Here, an attempt is made to provide guidance on how optimization might best be applied to crystal-growth problems, and what parameters and factors might most profitably be explored to accelerate and achieve success. PMID:25372810

Applying an Empirical Hydropathic Forcefield in Refinement May Improve Low-Resolution Protein X-Ray Crystal Structures

PubMed Central

Koparde, Vishal N.; Scarsdale, J. Neel; Kellogg, Glen E.

2011-01-01

Background The quality of X-ray crystallographic models for biomacromolecules refined from data obtained at high-resolution is assured by the data itself. However, at low-resolution, >3.0 Å, additional information is supplied by a forcefield coupled with an associated refinement protocol. These resulting structures are often of lower quality and thus unsuitable for downstream activities like structure-based drug discovery. Methodology An X-ray crystallography refinement protocol that enhances standard methodology by incorporating energy terms from the HINT (Hydropathic INTeractions) empirical forcefield is described. This protocol was tested by refining synthetic low-resolution structural data derived from 25 diverse high-resolution structures, and referencing the resulting models to these structures. The models were also evaluated with global structural quality metrics, e.g., Ramachandran score and MolProbity clashscore. Three additional structures, for which only low-resolution data are available, were also re-refined with this methodology. Results The enhanced refinement protocol is most beneficial for reflection data at resolutions of 3.0 Å or worse. At the low-resolution limit, ≥4.0 Å, the new protocol generated models with Cα positions that have RMSDs that are 0.18 Å more similar to the reference high-resolution structure, Ramachandran scores improved by 13%, and clashscores improved by 51%, all in comparison to models generated with the standard refinement protocol. The hydropathic forcefield terms are at least as effective as Coulombic electrostatic terms in maintaining polar interaction networks, and significantly more effective in maintaining hydrophobic networks, as synthetic resolution is decremented. Even at resolutions ≥4.0 Å, these latter networks are generally native-like, as measured with a hydropathic interactions scoring tool. PMID:21246043

TOPICAL REVIEW: Digital x-ray tomosynthesis: current state of the art and clinical potential

NASA Astrophysics Data System (ADS)

Dobbins, James T., III; Godfrey, Devon J.

2003-10-01

Digital x-ray tomosynthesis is a technique for producing slice images using conventional x-ray systems. It is a refinement of conventional geometric tomography, which has been known since the 1930s. In conventional geometric tomography, the x-ray tube and image receptor move in synchrony on opposite sides of the patient to produce a plane of structures in sharp focus at the plane containing the fulcrum of the motion; all other structures above and below the fulcrum plane are blurred and thus less visible in the resulting image. Tomosynthesis improves upon conventional geometric tomography in that it allows an arbitrary number of in-focus planes to be generated retrospectively from a sequence of projection radiographs that are acquired during a single motion of the x-ray tube. By shifting and adding these projection radiographs, specific planes may be reconstructed. This topical review describes the various reconstruction algorithms used to produce tomosynthesis images, as well as approaches used to minimize the residual blur from out-of-plane structures. Historical background and mathematical details are given for the various approaches described. Approaches for optimizing the tomosynthesis image are given. Applications of tomosynthesis to various clinical tasks, including angiography, chest imaging, mammography, dental imaging and orthopaedic imaging, are also described.

Non-intrusive telemetry applications in the oilsands: from visible light and x-ray video to acoustic imaging and spectroscopy

NASA Astrophysics Data System (ADS)

Shaw, John M.

2013-06-01

While the production, transport and refining of oils from the oilsands of Alberta, and comparable resources elsewhere is performed at industrial scales, numerous technical and technological challenges and opportunities persist due to the ill defined nature of the resource. For example, bitumen and heavy oil comprise multiple bulk phases, self-organizing constituents at the microscale (liquid crystals) and the nano scale. There are no quantitative measures available at the molecular level. Non-intrusive telemetry is providing promising paths toward solutions, be they enabling technologies targeting process design, development or optimization, or more prosaic process control or process monitoring applications. Operation examples include automated large object and poor quality ore during mining, and monitoring the thickness and location of oil water interfacial zones within separation vessels. These applications involve real-time video image processing. X-ray transmission video imaging is used to enumerate organic phases present within a vessel, and to detect individual phase volumes, densities and elemental compositions. This is an enabling technology that provides phase equilibrium and phase composition data for production and refining process development, and fluid property myth debunking. A high-resolution two-dimensional acoustic mapping technique now at the proof of concept stage is expected to provide simultaneous fluid flow and fluid composition data within porous inorganic media. Again this is an enabling technology targeting visualization of diverse oil production process fundamentals at the pore scale. Far infrared spectroscopy coupled with detailed quantum mechanical calculations, may provide characteristic molecular motifs and intermolecular association data required for fluid characterization and process modeling. X-ray scattering (SAXS/WAXS/USAXS) provides characteristic supramolecular structure information that impacts fluid rheology and process fouling. The intent of this contribution is to present some of the challenges and to provide an introduction grounded in current work on non-intrusive telemetry applications - from a mine or reservoir to a refinery!

Rietveld refinement of the crystal structures of Rb2 XSi5O12 (X = Ni, Mn).

PubMed

Bell, Anthony M T; Henderson, C Michael B

2016-02-01

The synthetic leucite silicate framework mineral analogues Rb2 XSi5O12 {X = Ni [dirubidium nickel(II) penta-silicate] and Mn [dirubidium manganese(II) penta-silicate]} have been prepared by high-temperature solid-state synthesis. The results of Rietveld refinements, using X-ray powder diffraction data collected using Cu Kα X-rays, show that the title compounds crystallize in the space group Pbca and adopt the cation-ordered structure of Cs2CdSi5O12 and other leucites. The structures consist of tetra-hedral SiO4 and XO4 units sharing corners to form a partially substituted silicate framework. Extraframework Rb(+) cations sit in channels in the framework. All atoms occupy the 8c general position for this space group. In these refined structures, silicon and X atoms are ordered onto separate tetra-hedrally coordinated sites (T-sites). However, the Ni displacement parameter and the Ni-O bond lengths suggest that for the X = Ni sample, there may actually be some T-site cation disorder.

Rietveld refinement of the crystal structures of Rb2 XSi5O12 (X = Ni, Mn)

PubMed Central

Bell, Anthony M. T.; Henderson, C. Michael B.

2016-01-01

The synthetic leucite silicate framework mineral analogues Rb2 XSi5O12 {X = Ni [dirubidium nickel(II) penta­silicate] and Mn [dirubidium manganese(II) penta­silicate]} have been prepared by high-temperature solid-state synthesis. The results of Rietveld refinements, using X-ray powder diffraction data collected using Cu Kα X-rays, show that the title compounds crystallize in the space group Pbca and adopt the cation-ordered structure of Cs2CdSi5O12 and other leucites. The structures consist of tetra­hedral SiO4 and XO4 units sharing corners to form a partially substituted silicate framework. Extraframework Rb+ cations sit in channels in the framework. All atoms occupy the 8c general position for this space group. In these refined structures, silicon and X atoms are ordered onto separate tetra­hedrally coordinated sites (T-sites). However, the Ni displacement parameter and the Ni—O bond lengths suggest that for the X = Ni sample, there may actually be some T-site cation disorder. PMID:26958399

Thermal expansion in UO 2 determined by high-energy X-ray diffraction

DOE PAGES

Guthrie, M.; Benmore, C. J.; Skinner, L. B.; ...

2016-06-24

In this study, we present crystallographic analyses of high-energy X-ray diffraction data on polycrystalline UO 2 up to the melting temperature. The Rietveld refinements of our X-ray data are in agreement with previous measurements, but are systematically located around the upper bound of their uncertainty, indicating a slightly steeper trend of thermal expansion compared to established values. This observation is consistent with recent first principles calculations.

Toward Active X-ray Telescopes II

NASA Technical Reports Server (NTRS)

O'Dell, Stephen L.; Aldroft, Thomas L.; Atkins, Carolyn; Button, Timothy W.; Cotroneo, Vincenzo; Davis, William N.; Doel, Peter; Feldman, Charlotte H.; Freeman, Mark D.; Gubarev, Mikhail V.;

Application of micro X-ray diffraction to investigate the reaction products formed by the alkali silica reaction in concrete structures

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

Dähn, R.; Arakcheeva, A.; Schaub, Ph.

Alkali–silica reaction (ASR) is one of the most important deterioration mechanisms in concrete leading to substantial damages of structures worldwide. Synchrotron-based micro-X-ray diffraction (micro-XRD) was employed to characterize the mineral phases formed in micro-cracks of concrete aggregates as a consequence of ASR. This particular high spatial resolution technique enables to directly gain structural information on ASR products formed in a 40-year old motorway bridge damaged due to ASR. Micro-X-ray-fluorescence was applied on thin sections to locate the reaction products formed in veins within concrete aggregates. Micro-XRD pattern were collected at selected points of interest along a vein by rotating themore » sample. Rietveld refinement determined the structure of the ASR product consisting of a new layered framework similar to mountainite and rhodesite. Furthermore, it is conceivable that understanding the structure of the ASR product may help developing new technical treatments inhibiting ASR.« less

Application of micro X-ray diffraction to investigate the reaction products formed by the alkali–silica reaction in concrete structures

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

Dähn, R., E-mail: rainer.daehn@psi.ch; Arakcheeva, A.; Schaub, Ph.

Alkali–silica reaction (ASR) is one of the most important deterioration mechanisms in concrete leading to substantial damages of structures worldwide. Synchrotron-based micro-X-ray diffraction (micro-XRD) was employed to characterize the mineral phases formed in micro-cracks of concrete aggregates as a consequence of ASR. This high spatial resolution technique enables to directly gain structural information on ASR products formed in a 40-year old motorway bridge damaged due to ASR. Micro-X-ray-fluorescence was applied on thin sections to locate the reaction products formed in veins within concrete aggregates. Micro-XRD pattern were collected at selected points of interest along a vein by rotating the sample.more » Rietveld refinement determined the structure of the ASR product consisting of a new layered framework similar to mountainite and rhodesite. It is conceivable that understanding the structure of the ASR product may help developing new technical treatments inhibiting ASR.« less

History of HERMES III diode to z-pinch breakthrough and beyond :

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

Sanford, Thomas Williamlou.

HERMES III and Z are two flagship accelerators of Sandias pulsed-power program developed to generate intense -ray fields for the study of nuclear radiation effects, and to explore high energy-density physics (including the production of intense x-ray fields for Inertia Confinement Fusion [ICF]), respectively. A diode at the exit of HERMES III converts its 20-MeV electron beam into -rays. In contrast, at the center of Z, a z-pinch is used to convert its 20-MA current into an intense burst of x-rays. Here the history of how the HERMES III diode emerged from theoretical considerations to actual hardware is discussed. Next,more » the reverse process of how the experimental discovery of wire-array stabilization in a z-pinch, led to a better theory of wirearray implosions and its application to one of the ICF concepts on Z--the DH (Dynamic Hohlraum) is reviewed. Lastly, the report concludes with how the unexpected axial radiation asymmetry measured in the DH is understood. The first discussion illustrates the evolution of physics from theory-to-observationto- refinement. The second two illustrate the reverse process of observationto- theory-to refinement. The histories are discussed through the vehicle of my research at Sandia, illustrating the unique environment Sandia provides for personal growth and development into a scientific leader.« less

Modelling dynamics in protein crystal structures by ensemble refinement

PubMed Central

Burnley, B Tom; Afonine, Pavel V; Adams, Paul D; Gros, Piet

2012-01-01

Single-structure models derived from X-ray data do not adequately account for the inherent, functionally important dynamics of protein molecules. We generated ensembles of structures by time-averaged refinement, where local molecular vibrations were sampled by molecular-dynamics (MD) simulation whilst global disorder was partitioned into an underlying overall translation–libration–screw (TLS) model. Modeling of 20 protein datasets at 1.1–3.1 Å resolution reduced cross-validated Rfree values by 0.3–4.9%, indicating that ensemble models fit the X-ray data better than single structures. The ensembles revealed that, while most proteins display a well-ordered core, some proteins exhibit a ‘molten core’ likely supporting functionally important dynamics in ligand binding, enzyme activity and protomer assembly. Order–disorder changes in HIV protease indicate a mechanism of entropy compensation for ordering the catalytic residues upon ligand binding by disordering specific core residues. Thus, ensemble refinement extracts dynamical details from the X-ray data that allow a more comprehensive understanding of structure–dynamics–function relationships. DOI: http://dx.doi.org/10.7554/eLife.00311.001 PMID:23251785

Single crystal X-ray diffraction study of the HgBa2CuO4+δ superconducting compound

NASA Astrophysics Data System (ADS)

Bordet, P.; Duc, F.; Lefloch, S.; Capponi, J. J.; Alexandre, E.; Rosa-Nunes, M.; Antipov, E. V.; Putilin, S.

1996-02-01

A high precision X-ray diffraction analysis up to sin θ/λ = 1.15 of a HgBa2CuO4+δ single crystal having a Tc of ~ 90 K is presented. The cell parameters are a = 3.8815(4), c = 9.485 (7) Å. The refinements indicate the existence of a split barium site due to the presence of excess oxygen in the mercury layer. The position of this excess oxygen might be slightly displaced from the (1/2 1/2 0) position. A 6% mercury deficiency is observed. Models, including mercury defects, substitution by copper cations, or carbonate groups, are compared. However, we obtain no definite evidence for either of the three models. A possible disorder of the Hg position, due to the formation of chemical bonds with neighbouring extra oxygen anions, could correlate to the refinements of mixed species at the Hg site. A low temperature single crystal x-ray diffraction study, and comparison of refinements for the same single crystal with different extra oxygen contents, are in progress to help clarify this problem.

Experimental determination of spin-dependent electron density by joint refinement of X-ray and polarized neutron diffraction data.

PubMed

Deutsch, Maxime; Claiser, Nicolas; Pillet, Sébastien; Chumakov, Yurii; Becker, Pierre; Gillet, Jean Michel; Gillon, Béatrice; Lecomte, Claude; Souhassou, Mohamed

2012-11-01

New crystallographic tools were developed to access a more precise description of the spin-dependent electron density of magnetic crystals. The method combines experimental information coming from high-resolution X-ray diffraction (XRD) and polarized neutron diffraction (PND) in a unified model. A new algorithm that allows for a simultaneous refinement of the charge- and spin-density parameters against XRD and PND data is described. The resulting software MOLLYNX is based on the well known Hansen-Coppens multipolar model, and makes it possible to differentiate the electron spins. This algorithm is validated and demonstrated with a molecular crystal formed by a bimetallic chain, MnCu(pba)(H(2)O)(3)·2H(2)O, for which XRD and PND data are available. The joint refinement provides a more detailed description of the spin density than the refinement from PND data alone.

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

Predicting X-ray diffuse scattering from translation–libration–screw structural ensembles

PubMed Central

Van Benschoten, Andrew H.; Afonine, Pavel V.; Terwilliger, Thomas C.; Wall, Michael E.; Jackson, Colin J.; Sauter, Nicholas K.; Adams, Paul D.; Urzhumtsev, Alexandre; Fraser, James S.

2015-01-01

Identifying the intramolecular motions of proteins and nucleic acids is a major challenge in macromolecular X-ray crystallography. Because Bragg diffraction describes the average positional distribution of crystalline atoms with imperfect precision, the resulting electron density can be compatible with multiple models of motion. Diffuse X-ray scattering can reduce this degeneracy by reporting on correlated atomic displacements. Although recent technological advances are increasing the potential to accurately measure diffuse scattering, computational modeling and validation tools are still needed to quantify the agreement between experimental data and different parameterizations of crystalline disorder. A new tool, phenix.diffuse, addresses this need by employing Guinier’s equation to calculate diffuse scattering from Protein Data Bank (PDB)-formatted structural ensembles. As an example case, phenix.diffuse is applied to translation–libration–screw (TLS) refinement, which models rigid-body displacement for segments of the macromolecule. To enable the calculation of diffuse scattering from TLS-refined structures, phenix.tls_as_xyz builds multi-model PDB files that sample the underlying T, L and S tensors. In the glycerophos­phodiesterase GpdQ, alternative TLS-group partitioning and different motional correlations between groups yield markedly dissimilar diffuse scattering maps with distinct implications for molecular mechanism and allostery. These methods demonstrate how, in principle, X-ray diffuse scattering could extend macromolecular structural refinement, validation and analysis. PMID:26249347

Predicting X-ray diffuse scattering from translation–libration–screw structural ensembles

DOE PAGES

Van Benschoten, Andrew H.; Afonine, Pavel V.; Terwilliger, Thomas C.; ...

2015-07-28

Identifying the intramolecular motions of proteins and nucleic acids is a major challenge in macromolecular X-ray crystallography. Because Bragg diffraction describes the average positional distribution of crystalline atoms with imperfect precision, the resulting electron density can be compatible with multiple models of motion. Diffuse X-ray scattering can reduce this degeneracy by reporting on correlated atomic displacements. Although recent technological advances are increasing the potential to accurately measure diffuse scattering, computational modeling and validation tools are still needed to quantify the agreement between experimental data and different parameterizations of crystalline disorder. A new tool, phenix.diffuse, addresses this need by employing Guinier'smore » equation to calculate diffuse scattering from Protein Data Bank (PDB)-formatted structural ensembles. As an example case, phenix.diffuse is applied to translation–libration–screw (TLS) refinement, which models rigid-body displacement for segments of the macromolecule. To enable the calculation of diffuse scattering from TLS-refined structures, phenix.tls_as_xyz builds multi-model PDB files that sample the underlying T, L and S tensors. In the glycerophosphodiesterase GpdQ, alternative TLS-group partitioning and different motional correlations between groups yield markedly dissimilar diffuse scattering maps with distinct implications for molecular mechanism and allostery. In addition, these methods demonstrate how, in principle, X-ray diffuse scattering could extend macromolecular structural refinement, validation and analysis.« less

Atomic pair distribution function at the Brazilian Synchrotron Light Laboratory: application to the Pb 1–x La xZr 0.40Ti 0.60O 3 ferroelectric system

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

Saleta, M. E.; Eleotério, M.; Mesquita, A.

2017-07-29

This work reports the setting up of the X-ray diffraction and spectroscopy beamline at the Brazilian Synchrotron Light Laboratory for performing total scattering experiments to be analyzed by atomic pair distribution function (PDF) studies. The results of a PDF refinement for Al 2O 3 standard are presented and compared with data acquired at a beamline of the Advanced Photon Source, where it is common to perform this type of experiment. A preliminary characterization of the Pb 1–xLa xZr 0.40Ti 0.60O 3 ferroelectric system, withx= 0.11, 0.12 and 0.15, is also shown.

Establishing nonlinearity thresholds with ultraintense X-ray pulses

NASA Astrophysics Data System (ADS)

Szlachetko, Jakub; Hoszowska, Joanna; Dousse, Jean-Claude; Nachtegaal, Maarten; Błachucki, Wojciech; Kayser, Yves; Sà, Jacinto; Messerschmidt, Marc; Boutet, Sebastien; Williams, Garth J.; David, Christian; Smolentsev, Grigory; van Bokhoven, Jeroen A.; Patterson, Bruce D.; Penfold, Thomas J.; Knopp, Gregor; Pajek, Marek; Abela, Rafael; Milne, Christopher J.

2016-09-01

X-ray techniques have evolved over decades to become highly refined tools for a broad range of investigations. Importantly, these approaches rely on X-ray measurements that depend linearly on the number of incident X-ray photons. The advent of X-ray free electron lasers (XFELs) is opening the ability to reach extremely high photon numbers within ultrashort X-ray pulse durations and is leading to a paradigm shift in our ability to explore nonlinear X-ray signals. However, the enormous increase in X-ray peak power is a double-edged sword with new and exciting methods being developed but at the same time well-established techniques proving unreliable. Consequently, accurate knowledge about the threshold for nonlinear X-ray signals is essential. Herein we report an X-ray spectroscopic study that reveals important details on the thresholds for nonlinear X-ray interactions. By varying both the incident X-ray intensity and photon energy, we establish the regimes at which the simplest nonlinear process, two-photon X-ray absorption (TPA), can be observed. From these measurements we can extract the probability of this process as a function of photon energy and confirm both the nature and sub-femtosecond lifetime of the virtual intermediate electronic state.

Aplanatic telescopes based on Schwarzschild optical configuration: from grazing incidence Wolter-like x-ray optics to Cherenkov two-mirror normal incidence telescopes

NASA Astrophysics Data System (ADS)

Sironi, Giorgia

2017-09-01

At the beginning of XX century Karl Schwarzschild defined a method to design large-field aplanatic telescopes based on the use of two aspheric mirrors. The approach was then refined by Couder (1926) who, in order to correct for the astigmatic aberration, introduced a curvature of the focal plane. By the way, the realization of normal-incidence telescopes implementing the Schwarzschild aplanatic configuration has been historically limited by the lack of technological solutions to manufacture and test aspheric mirrors. On the other hand, the Schwarzschild solution was recovered for the realization of coma-free X-ray grazing incidence optics. Wolter-like grazing incidence systems are indeed free of spherical aberration, but still suffer from coma and higher order aberrations degrading the imaging capability for off-axis sources. The application of the Schwarzschild's solution to X-ray optics allowed Wolter to define an optical system that exactly obeys the Abbe sine condition, eliminating coma completely. Therefore these systems are named Wolter-Schwarzschild telescopes and have been used to implement wide-field X-ray telescopes like the ROSAT WFC and the SOHO X-ray telescope. Starting from this approach, a new class of X-ray optical system was proposed by Burrows, Burg and Giacconi assuming polynomials numerically optimized to get a flat field of view response and applied by Conconi to the wide field x-ray telescope (WFXT) design. The Schwarzschild-Couder solution has been recently re-discovered for the application to normal-incidence Cherenkov telescopes, thanks to the suggestion by Vassiliev and collaborators. The Italian Institute for Astrophysics (INAF) realized the first Cherenkov telescope based on the polynomial variation of the Schwarzschild configuration (the so-called ASTRI telescope). Its optical qualification was successfully completed in 2016, demonstrating the suitability of the Schwarzschild-like configuration for the Cherenkov astronomy requirements. Moreover, other Cherenkov telescopes based on Schwarzschild-Couder solutions are currently being completed at Fred Lawrence Whipple Observatory in southern Arizona, USA and at the Observatoire de Paris-Meudon. In this paper we will review the Karl Schwarzschild solution and its application to grazing incidence and Cherenkov telescopes, discussing on future applications in the field of high-energy astronomy.

Rapid alignment of nanotomography data using joint iterative reconstruction and reprojection.

PubMed

Gürsoy, Doğa; Hong, Young P; He, Kuan; Hujsak, Karl; Yoo, Seunghwan; Chen, Si; Li, Yue; Ge, Mingyuan; Miller, Lisa M; Chu, Yong S; De Andrade, Vincent; He, Kai; Cossairt, Oliver; Katsaggelos, Aggelos K; Jacobsen, Chris

2017-09-18

As x-ray and electron tomography is pushed further into the nanoscale, the limitations of rotation stages become more apparent, leading to challenges in the alignment of the acquired projection images. Here we present an approach for rapid post-acquisition alignment of these projections to obtain high quality three-dimensional images. Our approach is based on a joint estimation of alignment errors, and the object, using an iterative refinement procedure. With simulated data where we know the alignment error of each projection image, our approach shows a residual alignment error that is a factor of a thousand smaller, and it reaches the same error level in the reconstructed image in less than half the number of iterations. We then show its application to experimental data in x-ray and electron nanotomography.

An Improved X-ray Diffraction Method For Cellulose Crystallinity Measurement

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

Ju, Xiaohui; Bowden, Mark E.; Brown, Elvie E.

2015-06-01

We show in this work a modified X-ray diffraction method to determine cellulose crystallinity index (CrI). Nanocrystalline cellulose (NCC) dervided from bleached wood pulp was used as a model substrate. Rietveld refinement was applied with consideration of March-Dollase preferred orientation at the (001) plane. In contrast to most previous methods, three distinct amorphous peaks identified from new model samples which are used to calculate CrI. A 2 theta range from 10° to 75° was found to be more suitable to determine CrI and crystallite structural parameters such as d-spacing and crystallite size. This method enables a more reliable measurement ofmore » CrI of cellulose and may be applicable to other types of cellulose polymorphs.« less

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

Gürsoy, Doğa; Hong, Young P.; He, Kuan

As x-ray and electron tomography is pushed further into the nanoscale, the limitations of rotation stages become more apparent, leading to challenges in the alignment of the acquired projection images. Here we present an approach for rapid post-acquisition alignment of these projections to obtain high quality three-dimensional images. Our approach is based on a joint estimation of alignment errors, and the object, using an iterative refinement procedure. With simulated data where we know the alignment error of each projection image, our approach shows a residual alignment error that is a factor of a thousand smaller, and it reaches the samemore » error level in the reconstructed image in less than half the number of iterations. We then show its application to experimental data in x-ray and electron nanotomography.« less

Accurate determination of segmented X-ray detector geometry

PubMed Central

Yefanov, Oleksandr; Mariani, Valerio; Gati, Cornelius; White, Thomas A.; Chapman, Henry N.; Barty, Anton

2015-01-01

Recent advances in X-ray detector technology have resulted in the introduction of segmented detectors composed of many small detector modules tiled together to cover a large detection area. Due to mechanical tolerances and the desire to be able to change the module layout to suit the needs of different experiments, the pixels on each module might not align perfectly on a regular grid. Several detectors are designed to permit detector sub-regions (or modules) to be moved relative to each other for different experiments. Accurate determination of the location of detector elements relative to the beam-sample interaction point is critical for many types of experiment, including X-ray crystallography, coherent diffractive imaging (CDI), small angle X-ray scattering (SAXS) and spectroscopy. For detectors with moveable modules, the relative positions of pixels are no longer fixed, necessitating the development of a simple procedure to calibrate detector geometry after reconfiguration. We describe a simple and robust method for determining the geometry of segmented X-ray detectors using measurements obtained by serial crystallography. By comparing the location of observed Bragg peaks to the spot locations predicted from the crystal indexing procedure, the position, rotation and distance of each module relative to the interaction region can be refined. We show that the refined detector geometry greatly improves the results of experiments. PMID:26561117

X-ray and neutron total scattering analysis of Hy·(Bi0.2Ca0.55Sr0.25)(Ag0.25Na0.75)Nb3O10·xH2O perovskite nanosheet booklets with stacking disorder

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

Metz, Peter; Koch, Robert; Cladek, Bernadette

Ion-exchanged Aurivillius materials form perovskite nanosheet booklets wherein well-defined bi-periodic sheets, with ~11.5 Å thickness, exhibit extensive stacking disorder. The perovskite layer contents were defined initially using combined synchrotron X-ray and neutron Rietveld refinement of the parent Aurivillius structure. The structure of the subsequently ion-exchanged material, which is disordered in its stacking sequence, is analyzed using both pair distribution function (PDF) analysis and recursive method simulations of the scattered intensity. Combined X-ray and neutron PDF refinement of supercell stacking models demonstrates sensitivity of the PDF to both perpendicular and transverse stacking vector components. Further, hierarchical ensembles of stacking models weightedmore » by a standard normal distribution are demonstrated to improve PDF fit over 1–25 Å. Recursive method simulations of the X-ray scattering profile demonstrate agreement between the real space stacking analysis and more conventional reciprocal space methods. The local structure of the perovskite sheet is demonstrated to relax only slightly from the Aurivillius structure after ion exchange.« less

Taguchi's technique: an effective method for improving X-ray medical radiographic screen performance.

PubMed

Vlachogiannis, J G

2003-01-01

Taguchi's technique is a helpful tool to achieve experimental optimization of a large number of decision variables with a small number of off-line experiments. The technique appears to be an ideal tool for improving the performance of X-ray medical radiographic screens under a noise source. Currently there are very many guides available for improving the efficiency of X-ray medical radiographic screens. These guides can be refined using a second-stage parameter optimization. based on Taguchi's technique, selecting the optimum levels of controllable X-ray radiographic screen factors. A real example of the proposed technique is presented giving certain performance criteria. The present research proposes the reinforcement of X-ray radiography by Taguchi's technique as a novel hardware mechanism.

Estimation of Uncertainties in the Global Distance Test (GDT_TS) for CASP Models.

PubMed

Li, Wenlin; Schaeffer, R Dustin; Otwinowski, Zbyszek; Grishin, Nick V

2016-01-01

The Critical Assessment of techniques for protein Structure Prediction (or CASP) is a community-wide blind test experiment to reveal the best accomplishments of structure modeling. Assessors have been using the Global Distance Test (GDT_TS) measure to quantify prediction performance since CASP3 in 1998. However, identifying significant score differences between close models is difficult because of the lack of uncertainty estimations for this measure. Here, we utilized the atomic fluctuations caused by structure flexibility to estimate the uncertainty of GDT_TS scores. Structures determined by nuclear magnetic resonance are deposited as ensembles of alternative conformers that reflect the structural flexibility, whereas standard X-ray refinement produces the static structure averaged over time and space for the dynamic ensembles. To recapitulate the structural heterogeneous ensemble in the crystal lattice, we performed time-averaged refinement for X-ray datasets to generate structural ensembles for our GDT_TS uncertainty analysis. Using those generated ensembles, our study demonstrates that the time-averaged refinements produced structure ensembles with better agreement with the experimental datasets than the averaged X-ray structures with B-factors. The uncertainty of the GDT_TS scores, quantified by their standard deviations (SDs), increases for scores lower than 50 and 70, with maximum SDs of 0.3 and 1.23 for X-ray and NMR structures, respectively. We also applied our procedure to the high accuracy version of GDT-based score and produced similar results with slightly higher SDs. To facilitate score comparisons by the community, we developed a user-friendly web server that produces structure ensembles for NMR and X-ray structures and is accessible at http://prodata.swmed.edu/SEnCS. Our work helps to identify the significance of GDT_TS score differences, as well as to provide structure ensembles for estimating SDs of any scores.

The X-Ray Lightcurve of Eta Carinae: Refinement of the Orbit and Evidence for Phase Dependent Mass Loss

NASA Technical Reports Server (NTRS)

Corcoran, M. F.; Ishibashi, K.; Swank, J. H.; Petre, R.; White, Nicholas E. (Technical Monitor)

2000-01-01

We solve the RXTE X-ray lightcurve of the extremely luminous and massive star eta Carinae with a colliding wind emission model to refine the ground-based orbital elements. The sharp decline to X-ray minimum at the end of 1997 fixes the date of the last periastron passage at 1997.95 +/- 0.05, not 1998.13 as derived from ground-based radial velocities. This helps resolve a discrepancy between the ground-based radial velocities and spatially-resolved velocity measures obtained by STIS. The X-ray data are consistent with a mass function f(M) approx. = 1.5, lower than the value f(M) approx. = 7.5 previously reported, so that the masses of eta Carinae and the companion are M(sub eta) greater than or = 80 solar mass and M(sub c) approx. 30 solar mass respectively. In addition the X-ray data suggest that the mass loss rate from eta Carinae is generally less than 3 x 10(exp -4) solar mass/yr, about a factor of 5 lower than that derived from some observations in other wavebands. We could not match the duration of the X-ray minimum with any standard colliding wind model in which the wind is spherically symmetric and the mass loss rate is constant. However we show that we can match the variations around X-ray minimum if we include an increase of a factor of approx. 20 in the mass loss rate from eta Carinae for approximately 80 days following periastron. If real, this excess in M would be the first evidence of enhanced mass flow off the primary when the two stars are close (presumably driven by tidal interactions). Our interpretation of the X-ray data suggest that the ASCA and RXTE X-ray spectra near the X-ray minimum are significantly contaminated by unresolved hard emission (E greater than or = 2 keV) from sonic other nearby source, probably associated with scattering of tile colliding wind emission by circumstellar dust. Based on the X-ray fluxes the distance to n Carinae is 2300 pc with formal uncertainties of only approx. 10%.

Rietveld refinement and electrical properties of Ni-Zn spinel ferrites

NASA Astrophysics Data System (ADS)

Hooda, Ashima; Sanghi, Sujata; Agarwal, Ashish; Khasa, Satish; Hooda, Bhawana

2017-05-01

NiFe2O4, ZnFe2O4, Ni0.5Zn0.5Fe2O4 spinel samples have been synthesized by conventional solid state reaction technique. Powder X-ray diffraction and Rietveld refinement revealed that the samples were single Spinel phase with space group fd3m. The average crystalline size (D), lattice constant (a), X-ray density (ρx), measured density (ρm) and Porosity (P) of prepared samples were determined from XRD data. The dc electrical resistivity (p) was measured as a function of temperature. The variations of ρ were explained on the basis of Verwey and de Bohr mechanism. The value of DC resistivity found to increase with increase Zn concentration.

X-ray characterization of solid small molecule organic materials

DOEpatents

Billinge, Simon; Shankland, Kenneth; Shankland, Norman; Florence, Alastair

2014-06-10

The present invention provides, inter alia, methods of characterizing a small molecule organic material, e.g., a drug or a drug product. This method includes subjecting the solid small molecule organic material to x-ray total scattering analysis at a short wavelength, collecting data generated thereby, and mathematically transforming the data to provide a refined set of data.

In situ data collection and structure refinement from microcapillary protein crystallization

PubMed Central

Yadav, Maneesh K.; Gerdts, Cory J.; Sanishvili, Ruslan; Smith, Ward W.; Roach, L. Spencer; Ismagilov, Rustem F.; Kuhn, Peter; Stevens, Raymond C.

2007-01-01

In situ X-ray data collection has the potential to eliminate the challenging task of mounting and cryocooling often fragile protein crystals, reducing a major bottleneck in the structure determination process. An apparatus used to grow protein crystals in capillaries and to compare the background X-ray scattering of the components, including thin-walled glass capillaries against Teflon, and various fluorocarbon oils against each other, is described. Using thaumatin as a test case at 1.8 Å resolution, this study demonstrates that high-resolution electron density maps and refined models can be obtained from in situ diffraction of crystals grown in microcapillaries. PMID:17468785

Establishing nonlinearity thresholds with ultraintense X-ray pulses

DOE PAGES

Szlachetko, Jakub; Hoszowska, Joanna; Dousse, Jean-Claude; ...

2016-09-13

X-ray techniques have evolved over decades to become highly refined tools for a broad range of investigations. Importantly, these approaches rely on X-ray measurements that depend linearly on the number of incident X-ray photons. The advent of X-ray free electron lasers (XFELs) is opening the ability to reach extremely high photon numbers within ultrashort X-ray pulse durations and is leading to a paradigm shift in our ability to explore nonlinear X-ray signals. However, the enormous increase in X-ray peak power is a double-edged sword with new and exciting methods being developed but at the same time well-established techniques proving unreliable.more » Consequently, accurate knowledge about the threshold for nonlinear X-ray signals is essential. Here in this paper we report an X-ray spectroscopic study that reveals important details on the thresholds for nonlinear X-ray interactions. By varying both the incident X-ray intensity and photon energy, we establish the regimes at which the simplest nonlinear process, two-photon X-ray absorption (TPA), can be observed. From these measurements we can extract the probability of this process as a function of photon energy and confirm both the nature and sub-femtosecond lifetime of the virtual intermediate electronic state.« less

PDB_REDO: automated re-refinement of X-ray structure models in the PDB.

PubMed

Joosten, Robbie P; Salzemann, Jean; Bloch, Vincent; Stockinger, Heinz; Berglund, Ann-Charlott; Blanchet, Christophe; Bongcam-Rudloff, Erik; Combet, Christophe; Da Costa, Ana L; Deleage, Gilbert; Diarena, Matteo; Fabbretti, Roberto; Fettahi, Géraldine; Flegel, Volker; Gisel, Andreas; Kasam, Vinod; Kervinen, Timo; Korpelainen, Eija; Mattila, Kimmo; Pagni, Marco; Reichstadt, Matthieu; Breton, Vincent; Tickle, Ian J; Vriend, Gert

2009-06-01

Structural biology, homology modelling and rational drug design require accurate three-dimensional macromolecular coordinates. However, the coordinates in the Protein Data Bank (PDB) have not all been obtained using the latest experimental and computational methods. In this study a method is presented for automated re-refinement of existing structure models in the PDB. A large-scale benchmark with 16 807 PDB entries showed that they can be improved in terms of fit to the deposited experimental X-ray data as well as in terms of geometric quality. The re-refinement protocol uses TLS models to describe concerted atom movement. The resulting structure models are made available through the PDB_REDO databank (http://www.cmbi.ru.nl/pdb_redo/). Grid computing techniques were used to overcome the computational requirements of this endeavour.

A thermal/nonthermal approach to solar flares

NASA Technical Reports Server (NTRS)

Benka, Stephen G.

1991-01-01

An approach for modeling solar flare high-energy emissions is developed in which both thermal and nonthermal particles coexist and contribute to the radiation. The thermal/nonthermal distribution function is interpreted physically by postulating the existence of DC sheets in the flare region. The currents then provide both primary plasma heating through Joule dissipation, and runaway electron acceleration. The physics of runaway acceleration is discussed. Several methods are presented for obtaining approximations to the thermal/nonthermal distribution function, both within the current sheets and outside of them. Theoretical hard x ray spectra are calculated, allowing for thermal bremsstrahlung from the heated plasma electrons impinging on the chromosphere. A simple model for hard x ray images of two-ribbon flares is presented. Theoretical microwave gyrosynchrotron spectra are calculated and analyzed, uncovering important new effects caused by the interplay of thermal and nonthermal particles. The theoretical spectra are compared with observed high resolution spectra of solar flares, and excellent agreement is found, in both hard x rays and microwaves. The future detailed application of this approach to solar flares is discussed, as are possible refinements to this theory.

Nano-Crystalline Thermally Evaporated Bi2Se3 Thin Films Synthesized from Mechanically Milled Powder

NASA Astrophysics Data System (ADS)

Amara, A.; Abdennouri, N.; Drici, A.; Abdelkader, D.; Bououdina, M.; Chaffar Akkari, F.; Khemiri, N.; Kanzari, M.; Bernède, J. C.

2017-08-01

Bi2Se3 powder has been successfully synthesized via mechanical ball milling of bismuth and selenium as starting materials. X-ray diffraction characterization revealed the formation of the rhombohedral and orthorhombic phases of Bi2Se3 material belonging to systems with space groups R\\bar{3}m and Pbnm, respectively. The advantageous last finding is confirmed by the Rietveld refinement of the x-ray diffraction data. Furthermore, the analysis of the x-ray data of thermally deposited thin films revealed that both orthorhombic and rhombohedral phases are coexisting in the layer. The morphology of the ball milled powder was studied by scanning electron microscopy. The phase formation of the material is confirmed by Raman spectroscopy. M-H (Magnetization versus Magnetic field) curve indicates that Bi2Se3 powder has a ferromagnetic behavior. Additionally, absorbance and transmittance measurements were carried out on the obtained thermally evaporated thin films and yielded a band gap of 1.33 eV supporting the potential application of the heterogeneous rhombohedral/orthorhombic Bi2Se3 material in photovoltaics.

Unambiguous determination of H-atom positions: comparing results from neutron and high-resolution X-ray crystallography.

PubMed

Gardberg, Anna S; Del Castillo, Alexis Rae; Weiss, Kevin L; Meilleur, Flora; Blakeley, Matthew P; Myles, Dean A A

2010-05-01

The locations of H atoms in biological structures can be difficult to determine using X-ray diffraction methods. Neutron diffraction offers a relatively greater scattering magnitude from H and D atoms. Here, 1.65 A resolution neutron diffraction studies of fully perdeuterated and selectively CH(3)-protonated perdeuterated crystals of Pyrococcus furiosus rubredoxin (D-rubredoxin and HD-rubredoxin, respectively) at room temperature (RT) are described, as well as 1.1 A resolution X-ray diffraction studies of the same protein at both RT and 100 K. The two techniques are quantitatively compared in terms of their power to directly provide atomic positions for D atoms and analyze the role played by atomic thermal motion by computing the sigma level at the D-atom coordinate in simulated-annealing composite D-OMIT maps. It is shown that 1.65 A resolution RT neutron data for perdeuterated rubredoxin are approximately 8 times more likely overall to provide high-confidence positions for D atoms than 1.1 A resolution X-ray data at 100 K or RT. At or above the 1.0sigma level, the joint X-ray/neutron (XN) structures define 342/378 (90%) and 291/365 (80%) of the D-atom positions for D-rubredoxin and HD-rubredoxin, respectively. The X-ray-only 1.1 A resolution 100 K structures determine only 19/388 (5%) and 8/388 (2%) of the D-atom positions above the 1.0sigma level for D-rubredoxin and HD-rubredoxin, respectively. Furthermore, the improved model obtained from joint XN refinement yielded improved electron-density maps, permitting the location of more D atoms than electron-density maps from models refined against X-ray data only.

Construction and assembly of the wire planes for the MicroBooNE Time Projection Chamber

DOE PAGES

Acciarri, R.; Adams, C.; Asaadi, J.; ...

2017-03-09

As x-ray and electron tomography is pushed further into the nanoscale, the limitations of rotation stages become more apparent, leading to challenges in the alignment of the acquired projection images. Here we present an approach for rapid post-acquisition alignment of these projections to obtain high quality three-dimensional images. Our approach is based on a joint estimation of alignment errors, and the object, using an iterative refinement procedure. With simulated data where we know the alignment error of each projection image, our approach shows a residual alignment error that is a factor of a thousand smaller, and it reaches the samemore » error level in the reconstructed image in less than half the number of iterations. We then show its application to experimental data in x-ray and electron nanotomography.« less

Rapid alignment of nanotomography data using joint iterative reconstruction and reprojection

DOE PAGES

Gürsoy, Doğa; Hong, Young P.; He, Kuan; ...

2017-09-18

As x-ray and electron tomography is pushed further into the nanoscale, the limitations of rotation stages become more apparent, leading to challenges in the alignment of the acquired projection images. Here we present an approach for rapid post-acquisition alignment of these projections to obtain high quality three-dimensional images. Our approach is based on a joint estimation of alignment errors, and the object, using an iterative refinement procedure. With simulated data where we know the alignment error of each projection image, our approach shows a residual alignment error that is a factor of a thousand smaller, and it reaches the samemore » error level in the reconstructed image in less than half the number of iterations. We then show its application to experimental data in x-ray and electron nanotomography.« less

Construction and assembly of the wire planes for the MicroBooNE Time Projection Chamber

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

Acciarri, R.; Adams, C.; Asaadi, J.

As x-ray and electron tomography is pushed further into the nanoscale, the limitations of rotation stages become more apparent, leading to challenges in the alignment of the acquired projection images. Here we present an approach for rapid post-acquisition alignment of these projections to obtain high quality three-dimensional images. Our approach is based on a joint estimation of alignment errors, and the object, using an iterative refinement procedure. With simulated data where we know the alignment error of each projection image, our approach shows a residual alignment error that is a factor of a thousand smaller, and it reaches the samemore » error level in the reconstructed image in less than half the number of iterations. We then show its application to experimental data in x-ray and electron nanotomography.« less

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.

DiSCaMB: a software library for aspherical atom model X-ray scattering factor calculations with CPUs and GPUs.

PubMed

Chodkiewicz, Michał L; Migacz, Szymon; Rudnicki, Witold; Makal, Anna; Kalinowski, Jarosław A; Moriarty, Nigel W; Grosse-Kunstleve, Ralf W; Afonine, Pavel V; Adams, Paul D; Dominiak, Paulina Maria

2018-02-01

It has been recently established that the accuracy of structural parameters from X-ray refinement of crystal structures can be improved by using a bank of aspherical pseudoatoms instead of the classical spherical model of atomic form factors. This comes, however, at the cost of increased complexity of the underlying calculations. In order to facilitate the adoption of this more advanced electron density model by the broader community of crystallographers, a new software implementation called DiSCaMB , 'densities in structural chemistry and molecular biology', has been developed. It addresses the challenge of providing for high performance on modern computing architectures. With parallelization options for both multi-core processors and graphics processing units (using CUDA), the library features calculation of X-ray scattering factors and their derivatives with respect to structural parameters, gives access to intermediate steps of the scattering factor calculations (thus allowing for experimentation with modifications of the underlying electron density model), and provides tools for basic structural crystallographic operations. Permissively (MIT) licensed, DiSCaMB is an open-source C++ library that can be embedded in both academic and commercial tools for X-ray structure refinement.

Accurate determination of segmented X-ray detector geometry

DOE PAGES

Yefanov, Oleksandr; Mariani, Valerio; Gati, Cornelius; ...

2015-10-22

Recent advances in X-ray detector technology have resulted in the introduction of segmented detectors composed of many small detector modules tiled together to cover a large detection area. Due to mechanical tolerances and the desire to be able to change the module layout to suit the needs of different experiments, the pixels on each module might not align perfectly on a regular grid. Several detectors are designed to permit detector sub-regions (or modules) to be moved relative to each other for different experiments. Accurate determination of the location of detector elements relative to the beam-sample interaction point is critical formore » many types of experiment, including X-ray crystallography, coherent diffractive imaging (CDI), small angle X-ray scattering (SAXS) and spectroscopy. For detectors with moveable modules, the relative positions of pixels are no longer fixed, necessitating the development of a simple procedure to calibrate detector geometry after reconfiguration. We describe a simple and robust method for determining the geometry of segmented X-ray detectors using measurements obtained by serial crystallography. By comparing the location of observed Bragg peaks to the spot locations predicted from the crystal indexing procedure, the position, rotation and distance of each module relative to the interaction region can be refined. Furthermore, we show that the refined detector geometry greatly improves the results of experiments.« less

When combined X-ray and polarized neutron diffraction data challenge high-level calculations: spin-resolved electron density of an organic radical.

PubMed

Voufack, Ariste Bolivard; Claiser, Nicolas; Lecomte, Claude; Pillet, Sébastien; Pontillon, Yves; Gillon, Béatrice; Yan, Zeyin; Gillet, Jean Michel; Marazzi, Marco; Genoni, Alessandro; Souhassou, Mohamed

2017-08-01

Joint refinement of X-ray and polarized neutron diffraction data has been carried out in order to determine charge and spin density distributions simultaneously in the nitronyl nitroxide (NN) free radical Nit(SMe)Ph. For comparison purposes, density functional theory (DFT) and complete active-space self-consistent field (CASSCF) theoretical calculations were also performed. Experimentally derived charge and spin densities show significant differences between the two NO groups of the NN function that are not observed from DFT theoretical calculations. On the contrary, CASSCF calculations exhibit the same fine details as observed in spin-resolved joint refinement and a clear asymmetry between the two NO groups.

Ion-pairing in aqueous CaCl 2 and RbBr solutions. Simultaneous structural refinement of XAFS and XRD data

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

Pham, Thai V.; Fulton, John L.

2013-01-22

We present a new methodology involving the simultaneous refinement of both x-ray absorption and x-ray diffraction spectra (X-ray Absorption/Diffraction Structural Refinement,XADSR), to study hydration and ion pair structure of CaCl 2 and RbBr salts in concentrated aqueous solutions. The XADSR analysis includes the XAFS spectra analysis of both the cation and anion as a probe of their short-range structure with an XRD spectral analysis as a probe of the global structural. Together they deliver a comprehensive picture of the cation and anion hydration, the contact ion pair (CIP) structure and the solvent-separated ion pair (SSIP) structure. XADSR analysis of 6.0more » m aqueous CaCl 2 reveals that there are an insignificant number of Ca 2+-Cl- CIP’s, but there are approximately 3.4 SSIP’s separated by about 4.99 Å. In contrast XADSR analysis of aqueous RbBr yields about 0.7 pair CIP at a bond length 3.51 Å. The present work demonstrates a new approach for a direct co-refinement of XRD and XAFS spectra in a simple and reliable fashion, opening new opportunities for analysis in various disordered and crystalline systems. This work was supported by the U.S. Department of Energy (DOE), Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences and Biosciences. Pacific Northwest National Laboratory (PNNL) is operated for the U.S. Department of Energy by Battelle.« less

Synchrotron-based XAS on structure investigation of La0.99-xSrx(Na, K, Ba)0.01MnO3 nanoparticles: Evidence of magnetic properties

NASA Astrophysics Data System (ADS)

Daengsakul, Sujittra; Saengplot, Saowalak; Kidkhunthod, Pinit; Pimsawat, Adulphan; Maensiri, Santi

2018-04-01

This work presents the structural study of La0.99-xSrx(Na, K, Ba)0.01MnO3 or LSAM nanoparticles synthesized using thermal-hydro decomposition method where A denotes Na, K, Sr and Ba, respectively. The effect of ionic radii size of A dopants or rA from the substitution of A for La and Sr on the MnO6 octrahedral structure, where the average size of the cations occupying in A-site or 〈rA〉 is fixed at ∼ 1.24 Å, is focused. The LSAM nanoparticles are carefully studied using X-ray diffraction (XRD) including Rietveld refinement and X-ray Absorption Spectroscopy (XAS) including X-ray Absorption Near edge Structure (XANES) and X-ray Absorption Fine Structure (EXAFS). The Rietveld refinement shows all nano-powder samples have rhombohedral structure. By XANES technique we found that the effect of A substitutions at A-site causes a slight change of mean oxidation state of Mn between 3.54 and 3.60. Furthermore, the structural distortion of MnO6 octrahedral in samples is analysed and obtained from EXAFS. The observed trend of ferromagnetism for all LSAM samples can be clearly explained by evidences of A-site doping, structural distortion around Mn atoms and mixing Mn3+/Mn4+ valence states.

Yes, one can obtain better quality structures from routine X-ray data collection.

PubMed

Sanjuan-Szklarz, W Fabiola; Hoser, Anna A; Gutmann, Matthias; Madsen, Anders Østergaard; Woźniak, Krzysztof

2016-01-01

Single-crystal X-ray diffraction structural results for benzidine dihydrochloride, hydrated and protonated N,N,N,N-peri(dimethylamino)naphthalene chloride, triptycene, dichlorodimethyltriptycene and decamethylferrocene have been analysed. A critical discussion of the dependence of structural and thermal parameters on resolution for these compounds is presented. Results of refinements against X-ray data, cut off to different resolutions from the high-resolution data files, are compared to structural models derived from neutron diffraction experiments. The Independent Atom Model (IAM) and the Transferable Aspherical Atom Model (TAAM) are tested. The average differences between the X-ray and neutron structural parameters (with the exception of valence angles defined by H atoms) decrease with the increasing 2θmax angle. The scale of differences between X-ray and neutron geometrical parameters can be significantly reduced when data are collected to the higher, than commonly used, 2θmax diffraction angles (for Mo Kα 2θmax > 65°). The final structural and thermal parameters obtained for the studied compounds using TAAM refinement are in better agreement with the neutron values than the IAM results for all resolutions and all compounds. By using TAAM, it is still possible to obtain accurate results even from low-resolution X-ray data. This is particularly important as TAAM is easy to apply and can routinely be used to improve the quality of structural investigations [Dominiak (2015 ▸). LSDB from UBDB. University of Buffalo, USA]. We can recommend that, in order to obtain more adequate (more accurate and precise) structural and displacement parameters during the IAM model refinement, data should be collected up to the larger diffraction angles, at least, for Mo Kα radiation to 2θmax = 65° (sin θmax/λ < 0.75 Å(-1)). The TAAM approach is a very good option to obtain more adequate results even using data collected to the lower 2θmax angles. Also the results of translation-libration-screw (TLS) analysis and vibrational entropy values are more reliable for 2θmax > 65°.

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

Thimmaiah, Srinivasa; Tener, Zachary; Lamichhane, Tej N.

Here, the γ-region of the Mn–Al phase diagram between 45 and 70 at.% Al was re-investigated by a combination of powder and single crystal X-ray diffraction as well as EDS analysis to establish the distribution of Mn and Al atoms. Single crystals of γ-Mn 5–x Al 8+x were grown using Sn-flux at 650 °C. The crystal structure, atomic coordinates and site occupancy parameters of γ-Mn 5–x Al 8+x phases were refined from single crystal X-ray data. The γ-Mn 5-x Al 8+x phase adopts the rhombohedral Cr 5Al 8-type structure rather than a cubic γ-brass structure. The refined compositions from twomore » crystals extracted from the Al-rich and Mn-rich sides are, respectively, Mn 4.76Al 8.24(2) (I) and Mn 6.32Al 6.68(2) (II). The structure was refined in the acentric R3m space group (No.160, Z=6), in order to compare with other reported rhombohedral γ-brasses. In addition, according to X-ray powder diffraction analysis, at the Al-rich side the γ-phase coexists with LT–Mn 4Al 11 and, at the Mn-rich side, with a hitherto unknown phase. The refined lattice parameters from powder patterns fall in the range a=12.6814(7)–12.6012(5) Å and c=7.9444(2)–7.9311(2) Å from Al-rich to Mn-rich loadings, and the corresponding rhombohedral angles distorted from a pseudo-cubic cell were found to be 89.1(1)°–88.9(1)°. Magnetic susceptibility and magnetization studies of Mn 4.92Al 8.08(2) are consistent with moment bearing Mn and suggest a spin glass state below 27 K. Tight-binding electronic structure calculations (LMTO-ASA with LSDA) showed that the calculated Fermi level for γ-“Mn 5Al 8” falls within a pseudogap of the density of states, a result which is in accordance with a Hume-Rothery stabilization mechanism γ-brass type phases.« less

Multidataset Refinement Resonant Diffraction, and Magnetic Structures

PubMed Central

Attfield, J. Paul

2004-01-01

The scope of Rietveld and other powder diffraction refinements continues to expand, driven by improvements in instrumentation, methodology and software. This will be illustrated by examples from our research in recent years. Multidataset refinement is now commonplace; the datasets may be from different detectors, e.g., in a time-of-flight experiment, or from separate experiments, such as at several x-ray energies giving resonant information. The complementary use of x rays and neutrons is exemplified by a recent combined refinement of the monoclinic superstructure of magnetite, Fe3O4, below the 122 K Verwey transition, which reveals evidence for Fe2+/Fe3+ charge ordering. Powder neutron diffraction data continue to be used for the solution and Rietveld refinement of magnetic structures. Time-of-flight instruments on cold neutron sources can produce data that have a high intensity and good resolution at high d-spacings. Such profiles have been used to study incommensurate magnetic structures such as FeAsO4 and β–CrPO4. A multiphase, multidataset refinement of the phase-separated perovskite (Pr0.35Y0.07Th0.04Ca0.04Sr0.5)MnO3 has been used to fit three components with different crystal and magnetic structures at low temperatures. PMID:27366599

Correction of Hydrostatic Cluster Masses through Power Ratios and Weak Lensing

NASA Astrophysics Data System (ADS)

Mahdavi, Andisheh

2009-09-01

The evolution of rich, X-ray emitting clusters of galaxies has given us precise measurements of the cosmological parameters, with dramatic constraints on the dark energy equation of state. Built into these measurements are wholesale corrections for the infamous "X-ray mass underestimate"---the fact that X-ray masses are systematically low due to the incomplete thermalization of the intracluster plasma. We seek to refine the mass correction for cosmological use through morphological power ratios. Power ratios deliver more accurate correction factors because they take into account variations in substructure from cluster to cluster. We will test their ability to correct X-ray masses by comparing hydrostatic and weak lensing mass profiles for a sample of 44 rich clusters of galaxies.

Hirshfeld atom refinement.

PubMed

Capelli, Silvia C; Bürgi, Hans-Beat; Dittrich, Birger; Grabowsky, Simon; Jayatilaka, Dylan

2014-09-01

Hirshfeld atom refinement (HAR) is a method which determines structural parameters from single-crystal X-ray diffraction data by using an aspherical atom partitioning of tailor-made ab initio quantum mechanical molecular electron densities without any further approximation. Here the original HAR method is extended by implementing an iterative procedure of successive cycles of electron density calculations, Hirshfeld atom scattering factor calculations and structural least-squares refinements, repeated until convergence. The importance of this iterative procedure is illustrated via the example of crystalline ammonia. The new HAR method is then applied to X-ray diffraction data of the dipeptide Gly-l-Ala measured at 12, 50, 100, 150, 220 and 295 K, using Hartree-Fock and BLYP density functional theory electron densities and three different basis sets. All positions and anisotropic displacement parameters (ADPs) are freely refined without constraints or restraints - even those for hydrogen atoms. The results are systematically compared with those from neutron diffraction experiments at the temperatures 12, 50, 150 and 295 K. Although non-hydrogen-atom ADPs differ by up to three combined standard uncertainties (csu's), all other structural parameters agree within less than 2 csu's. Using our best calculations (BLYP/cc-pVTZ, recommended for organic molecules), the accuracy of determining bond lengths involving hydrogen atoms from HAR is better than 0.009 Å for temperatures of 150 K or below; for hydrogen-atom ADPs it is better than 0.006 Å(2) as judged from the mean absolute X-ray minus neutron differences. These results are among the best ever obtained. Remarkably, the precision of determining bond lengths and ADPs for the hydrogen atoms from the HAR procedure is comparable with that from the neutron measurements - an outcome which is obtained with a routinely achievable resolution of the X-ray data of 0.65 Å.

Hirshfeld atom refinement

PubMed Central

Capelli, Silvia C.; Bürgi, Hans-Beat; Dittrich, Birger; Grabowsky, Simon; Jayatilaka, Dylan

2014-01-01

Hirshfeld atom refinement (HAR) is a method which determines structural parameters from single-crystal X-ray diffraction data by using an aspherical atom partitioning of tailor-made ab initio quantum mechanical molecular electron densities without any further approximation. Here the original HAR method is extended by implementing an iterative procedure of successive cycles of electron density calculations, Hirshfeld atom scattering factor calculations and structural least-squares refinements, repeated until convergence. The importance of this iterative procedure is illustrated via the example of crystalline ammonia. The new HAR method is then applied to X-ray diffraction data of the dipeptide Gly–l-Ala measured at 12, 50, 100, 150, 220 and 295 K, using Hartree–Fock and BLYP density functional theory electron densities and three different basis sets. All positions and anisotropic displacement parameters (ADPs) are freely refined without constraints or restraints – even those for hydrogen atoms. The results are systematically compared with those from neutron diffraction experiments at the temperatures 12, 50, 150 and 295 K. Although non-hydrogen-atom ADPs differ by up to three combined standard uncertainties (csu’s), all other structural parameters agree within less than 2 csu’s. Using our best calculations (BLYP/cc-pVTZ, recommended for organic molecules), the accuracy of determining bond lengths involving hydrogen atoms from HAR is better than 0.009 Å for temperatures of 150 K or below; for hydrogen-atom ADPs it is better than 0.006 Å2 as judged from the mean absolute X-ray minus neutron differences. These results are among the best ever obtained. Remarkably, the precision of determining bond lengths and ADPs for the hydrogen atoms from the HAR procedure is comparable with that from the neutron measurements – an outcome which is obtained with a routinely achievable resolution of the X-ray data of 0.65 Å. PMID:25295177

Bragg projection ptychography on niobium phase domains

NASA Astrophysics Data System (ADS)

Burdet, Nicolas; Shi, Xiaowen; Clark, Jesse N.; Huang, Xiaojing; Harder, Ross; Robinson, Ian

2017-07-01

Bragg projection ptychography (BPP) is a coherent x-ray diffraction imaging technique which combines the strengths of scanning microscopy with the phase contrast of x-ray ptychography. Here we apply it for high resolution imaging of the phase-shifted crystalline domains associated with epitaxial growth. The advantages of BPP are that the spatial extent of the sample is arbitrary, it is nondestructive, and it gives potentially diffraction limited spatial resolution. Here we demonstrate the application of BPP for revealing the domain structure caused by epitaxial misfit in a nanostructured metallic thin film. Experimental coherent diffraction data were collected from a niobium thin film, epitaxially grown on a sapphire substrate as the beam was scanned across the sample. The data were analyzed by BPP using a carefully selected combination of refinement procedures. The resulting image shows a close packed array of epitaxial domains, shifted with respect to each other due to misfit between the film and its substrate.

Spot size characterization of focused non-Gaussian X-ray laser beams.

PubMed

Chalupský, J; Krzywinski, J; Juha, L; Hájková, V; Cihelka, J; Burian, T; Vysín, L; Gaudin, J; Gleeson, A; Jurek, M; Khorsand, A R; Klinger, D; Wabnitz, H; Sobierajski, R; Störmer, M; Tiedtke, K; Toleikis, S

2010-12-20

We present a new technique for the characterization of non-Gaussian laser beams which cannot be described by an analytical formula. As a generalization of the beam spot area we apply and refine the definition of so called effective area (A(eff)) [1] in order to avoid using the full-width at half maximum (FWHM) parameter which is inappropriate for non-Gaussian beams. Furthermore, we demonstrate a practical utilization of our technique for a femtosecond soft X-ray free-electron laser. The ablative imprints in poly(methyl methacrylate) - PMMA and amorphous carbon (a-C) are used to characterize the spatial beam profile and to determine the effective area. Two procedures of the effective area determination are presented in this work. An F-scan method, newly developed in this paper, appears to be a good candidate for the spatial beam diagnostics applicable to lasers of various kinds.

Application of star identification using pattern matching to space ground systems at GSFC

NASA Technical Reports Server (NTRS)

Fink, D.; Shoup, D.

1994-01-01

This paper reports the application of pattern recognition techniques for star identification based on those proposed by Van Bezooijen to space ground systems for near-real-time attitude determination. A prototype was developed using these algorithms, which was used to assess the suitability of these techniques for support of the X-Ray Timing Explorer (XTE), Submillimeter Wave Astronomy Satellite (SWAS), and the Solar and Heliospheric Observatory (SOHO) missions. Experience with the prototype was used to refine specifications for the operational system. Different geometry tests appropriate to the mission requirements of XTE, SWAS, and SOHO were adopted. The applications of these techniques to upcoming mission support of XTE, SWAS, and SOHO are discussed.

Rietveld refined structural and room temperature vibrational properties of BaTiO3 doped La0.67Ba0.33MnO3 composites

NASA Astrophysics Data System (ADS)

Dar, M. A.; Sheikh, M. W.; Malla, M. S.; Varshney, Dinesh

2016-05-01

The composites of (1-x) La0.67Ba0.33MnO3 (LBMO) + xBaTiO3 (BTO) (x = 0, 0.25 and 1.0) were synthesized by conventional solid-state reaction method. Rietveld refinement was employed to characterize the structural information of the prepared ceramics. The result of the Rietveld refinement of X-ray powder diffraction of La0.67Ba0.33MnO3 and BaTiO3 shows that these compounds crystallize in rhombohedral (R3c) and tetragonal (P4mm), respectively. The structural parameters and the reliability factors for the LBMO-BTO composite ceramics were successfully determined by the Rietveld refinement. At room temperature, Raman active phonon modes predicted by the group theory were observed only in BaTiO3 and composite sample. Pure LBMO does not show any Raman active Phonon mode at room temperature.

A Deep Pulse Search in 11 Low Mass X-Ray Binaries

NASA Astrophysics Data System (ADS)

Patruno, A.; Wette, K.; Messenger, C.

2018-06-01

We present a systematic coherent X-ray pulsation search in 11 low mass X-ray binaries (LMXBs). We select a relatively broad variety of LMXBs, including persistent and transient sources, spanning orbital periods between 0.3 and 17 hr. We use about 3.6 Ms of data collected by the Rossi X-Ray Timing Explorer and XMM-Newton and apply a semi-coherent search strategy to look for weak and persistent pulses in a wide spin frequency range. We find no evidence for X-ray pulsations in these systems and consequently set upper limits on the pulsed sinusoidal semi-amplitude below 1.6% for ten outbursting/persistent LMXBs and 6% for a quiescent system; the upper limits are further refined, by searching a narrower parameter space around the outliers, down to 0.14%–0.78% and 2.9%, respectively. These results suggest that weak pulsations might not form in (most) non pulsating LMXBs.

Microstructural analysis of biodegradable Mg-0.9Ca-1.2Zr alloy

NASA Astrophysics Data System (ADS)

Istrate, B.; Munteanu, C.; Geanta, V.; Baltatu, S.; Focsaneanu, S.; Earar, K.

2016-08-01

Magnesium alloys have applications in aerospace and medical applications as biodegradable orthopedic implants. Alloying with biocompatible elements, such as calcium or zirconium contribute to refining the the microstructure and improves corrosion resistance with the formation of an eutectic compound - Mg2Ca at boundary alpha-Mg grains. The purpose of this paper is to present the microstructure throw optical and scanning electron methods and phase and constituents identification with X-ray analysis. The results showed the presence of alpha-Mg grains with formation of a mechanical compound - Mg2Ca and appearance of alpha- Zr phase relatively uniformly distributed in nests.

Assessing the Chemical Accuracy of Protein Structures via Peptide Acidity

PubMed Central

Anderson, Janet S.; Hernández, Griselda; LeMaster, David M.

2012-01-01

Although the protein native state is a Boltzmann conformational ensemble, practical applications often require a representative model from the most populated region of that distribution. The acidity of the backbone amides, as reflected in hydrogen exchange rates, is exquisitely sensitive to the surrounding charge and dielectric volume distribution. For each of four proteins, three independently determined X-ray structures of differing crystallographic resolution were used to predict exchange for the static solvent-exposed amide hydrogens. The average correlation coefficients range from 0.74 for ubiquitin to 0.93 for Pyrococcus furiosus rubredoxin, reflecting the larger range of experimental exchange rates exhibited by the latter protein. The exchange prediction errors modestly correlate with the crystallographic resolution. MODELLER 9v6-derived homology models at ~60% sequence identity (36% identity for chymotrypsin inhibitor CI2) yielded correlation coefficients that are ~0.1 smaller than for the cognate X-ray structures. The most recently deposited NOE-based ubiquitin structure and the original NMR structure of CI2 fail to provide statistically significant predictions of hydrogen exchange. However, the more recent RECOORD refinement study of CI2 yielded predictions comparable to the X-ray and homology model-based analyses. PMID:23182463

[Semiotics of lesions of the cerebral venous collectors on application of noninvasive techniques of x-ray diagnosis].

PubMed

Semenov, S; Abalmasov, V

2001-01-01

The study included application of a complex of the noninvasive diagnostic techniques such as MR tomography, MR venography, duplex scanning of the internal jugular veins, and transcranial Doppler sonography. The authors provide a detailed description of the semiotics of the MR signs of cerebral venous collector lesion in patients with thrombosis, extravasal compression, aneurysms, and developmental anomalies. Present the quantitative ultrasound parameters of hemodynamics in the efferent vessels of the brain accessible to inspections describe the effect of spontaneous echo-opacification in the internal jugular veins, which is assumed to be a predictor of thrombosis. Intravenous injection of magnevist resulted in an appreciable refinement of visualization of small dural sinuses at MR venography thereby allowing for the diagnosis of their thrombosis. It is suggested that the use of the entire complex of the x-ray modalities under consideration may lead to a more complete and noninvasive evaluation of the nature of cerebral venous insufficiency and of the degree of hemodynamic significance. Moreover, this will make it possible to outline approaches to therapeutic or surgical correction of the disease.

Probing the accuracy and precision of Hirshfeld atom refinement with HARt interfaced with Olex2.

PubMed

Fugel, Malte; Jayatilaka, Dylan; Hupf, Emanuel; Overgaard, Jacob; Hathwar, Venkatesha R; Macchi, Piero; Turner, Michael J; Howard, Judith A K; Dolomanov, Oleg V; Puschmann, Horst; Iversen, Bo B; Bürgi, Hans-Beat; Grabowsky, Simon

2018-01-01

Hirshfeld atom refinement (HAR) is a novel X-ray structure refinement technique that employs aspherical atomic scattering factors obtained from stockholder partitioning of a theoretically determined tailor-made static electron density. HAR overcomes many of the known limitations of independent atom modelling (IAM), such as too short element-hydrogen distances, r ( X -H), or too large atomic displacement parameters (ADPs). This study probes the accuracy and precision of anisotropic hydrogen and non-hydrogen ADPs and of r ( X -H) values obtained from HAR. These quantities are compared and found to agree with those obtained from (i) accurate neutron diffraction data measured at the same temperatures as the X-ray data and (ii) multipole modelling (MM), an established alternative method for interpreting X-ray diffraction data with the help of aspherical atomic scattering factors. Results are presented for three chemically different systems: the aromatic hydro-carbon rubrene (orthorhombic 5,6,11,12-tetra-phenyl-tetracene), a co-crystal of zwitterionic betaine, imidazolium cations and picrate anions (BIPa), and the salt potassium hydrogen oxalate (KHOx). The non-hydrogen HAR-ADPs are as accurate and precise as the MM-ADPs. Both show excellent agreement with the neutron-based values and are superior to IAM-ADPs. The anisotropic hydrogen HAR-ADPs show a somewhat larger deviation from neutron-based values than the hydrogen SHADE-ADPs used in MM. Element-hydrogen bond lengths from HAR are in excellent agreement with those obtained from neutron diffraction experiments, although they are somewhat less precise. The residual density contour maps after HAR show fewer features than those after MM. Calculating the static electron density with the def2-TZVP basis set instead of the simpler def2-SVP one does not improve the refinement results significantly. All HARs were performed within the recently introduced HARt option implemented in the Olex2 program. They are easily launched inside its graphical user interface following a conventional IAM.

Modeling Contamination Migration on the Chandra X-ray Observatory II

NASA Technical Reports Server (NTRS)

O'Dell, Steve; Swartz, Doug; Tice, Neil; Plucinsky, Paul; Grant, Catherine; Marshall, Herman; Vikhlinin, Alexey

2013-01-01

During its first 14 years of operation, the cold (about -60degC) optical blocking filter of the Advanced CCD Imaging Spectrometer (ACIS), aboard the Chandra X-ray Observatory, has accumulated a growing layer of molecular contamination that attenuates low-energy x rays. Over the past few years, the accumulation rate, spatial distribution, and composition may have changed, perhaps partially related to changes in the operating temperature of the ACIS housing. This evolution of the accumulation of the molecular contamination has motivated further analysis of contamination migration on the Chandra X-ray Observatory, particularly within and near the ACIS cavity. To this end, the current study employs a higher-fidelity geometric model of the ACIS cavity, detailed thermal modeling based upon monitored temperature data, and an accordingly refined model of the molecular transport.

Structure and photoluminescence properties of Ba2-xSi4O10:2xSm3+

NASA Astrophysics Data System (ADS)

Ramteke, D. D.; Swart, H. C.

2018-04-01

We investigated the structure and photoluminescence properties of novel Ba2-xSi4O10:2xSm3+ phosphor prepared by the solid state reaction method. In the prepared phosphor the high temperature monoclinic phase was dominant over the low temperature orthorhombic phase. The shifting of the X-ray diffraction peaks with the Sm3+ ion addition was explained on the basis of the refinement results. The photoluminescence study showed that on excitation with 402 nm the phosphor emitted at 560 nm, 600 nm and 645 nm which corresponds to the 4G5/2→4H5/2, 4G5/2→4H7/2 and 4G5/2→4H9/2 transitions, respectively. Concentration quenching effect was also observed in the prepared phosphor. CIE chromaticity coordinates showed that the phosphor can be further developed for display applications.

Formal Technical Reports and Publications Completed Under Fuels and Lubricants RDTE Programs 1960 thru 1987

DTIC Science & Technology

1988-01-01

Synthetic Motor Oils Basic Research on Mist Flamma- AFLRL-97 A046345 Sep 77 D.W. Naegeli bility--Phase I, Experimental W.D. Weatherford, Jr. Facility...Fuels on Combustor Properties D.W. Naegeli Application of Energy Dispersive AFLRL-102 A062792 Feb 78 M.K. Greenberg X-Ray Fluorescence Spectroscopy...the Literature J.P. Cuellar, Jr. Military Fuels Refined From AFLRL-131 A101069 Mar 81 J.N. Bowden Paraho-Il Shale Oil E.C. Owens D.W. Naegeli L.L

Sharp chemical interface in epitaxial Fe{sub 3}O{sub 4} thin films

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

Gálvez, S.; Rubio-Zuazo, J., E-mail: rubio@esrf.fr; Salas-Colera, E.

Chemically sharp interface was obtained on single phase single oriented Fe{sub 3}O{sub 4} (001) thin film (7 nm) grown on NiO (001) substrate using oxygen assisted molecular beam epitaxy. Refinement of the atomic structure, stoichiometry, and oxygen vacancies were determined by soft and hard x-ray photoelectron spectroscopy, low energy electron diffraction and synchrotron based X-ray reflectivity, and X-ray diffraction. Our results demonstrate an epitaxial growth of the magnetite layer, perfect iron stoichiometry, absence of oxygen vacancies, and the existence of an intermixing free interface. Consistent magnetic and electrical characterizations are also shown.

Modeling Contamination Migration on the Chandra X-ray Observatory - II

NASA Technical Reports Server (NTRS)

O'Dell, Stephen L.; Swartz, Douglas A.; Tice, Neil W.; Plucinsky, Paul P.; Grant, Catherine E.; Marshall, Herman L.; Vikhlinin, Alexey A.; Tennant, Allyn F.

2013-01-01

During its first 14 years of operation, the cold (about -60C) optical blocking filter of the Advanced CCD Imaging Spectrometer (ACIS), aboard the Chandra X-ray Observatory, has accumulated a growing layer of molecular contamination that attenuates low-energy x rays. Over the past few years, the accumulation rate, spatial distribution, and composition have changed. This evolution has motivated further analysis of contamination migration within and near the ACIS cavity. To this end, the current study employs a higher-fidelity geometric model of the ACIS cavity, detailed thermal modeling based upon temperature data, and a refined model of the molecular transport.

Accurate macromolecular crystallographic refinement: incorporation of the linear scaling, semiempirical quantum-mechanics program DivCon into the PHENIX refinement package.

PubMed

Borbulevych, Oleg Y; Plumley, Joshua A; Martin, Roger I; Merz, Kenneth M; Westerhoff, Lance M

2014-05-01

Macromolecular crystallographic refinement relies on sometimes dubious stereochemical restraints and rudimentary energy functionals to ensure the correct geometry of the model of the macromolecule and any covalently bound ligand(s). The ligand stereochemical restraint file (CIF) requires a priori understanding of the ligand geometry within the active site, and creation of the CIF is often an error-prone process owing to the great variety of potential ligand chemistry and structure. Stereochemical restraints have been replaced with more robust functionals through the integration of the linear-scaling, semiempirical quantum-mechanics (SE-QM) program DivCon with the PHENIX X-ray refinement engine. The PHENIX/DivCon package has been thoroughly validated on a population of 50 protein-ligand Protein Data Bank (PDB) structures with a range of resolutions and chemistry. The PDB structures used for the validation were originally refined utilizing various refinement packages and were published within the past five years. PHENIX/DivCon does not utilize CIF(s), link restraints and other parameters for refinement and hence it does not make as many a priori assumptions about the model. Across the entire population, the method results in reasonable ligand geometries and low ligand strains, even when the original refinement exhibited difficulties, indicating that PHENIX/DivCon is applicable to both single-structure and high-throughput crystallography.

Simultaneous X-ray and neutron diffraction Rietveld refinements of nanophase iron substituted hydroxyapatite

NASA Astrophysics Data System (ADS)

Kyriacou, Andreas

The effect of Fe substitution on the crystal structure of hydroxyapatite (HAp) is studied by applying simultaneous Rietveld refinements of powder x-ray and neutron diffraction patterns. Fe is one of the trace elements replacing Ca in HAp, which is the major mineral phase in bones and teeth. The morphology and magnetic properties of the Fe-HAp system are also studied by transmission electron microscopy and magnetization measurements. Samples of Ca(5-x)Fex(PO4)3OH with 0 ≤ x ≤ 0.3 were prepared. Single phase HAp was identified in x-ray diffraction patterns (XRD) of samples with x < 0.1 inferring that the solubility limits are less than 0.1. Hematite (alpha-Fe2O3) is identified as a secondary phase for higher Fe content. The refined parameters show that Fe is incorporated in the HAp structure by replacing Ca in the two crystallographic sites with a preference at the Ca2 site. This preference explains the small effect of the Fe substitution on the lattice constants of HAp. The overall decrease of the lattice constants is explained by the ionic size difference of Ca and Fe. The increasing trend of the a-lattice constant with x in the Fe substituted samples is attributed to a lattice relaxation caused by the substitution of the 4- and 6-fold Fe at the 7- and 9-fold Ca1 and Ca2 sites. This Ca local geometry reduction is indicated by a slight increase of the Ca1-O3 and Ca2-O1 bond lengths. Above the solubility limit x = 0.05, the Fe is partitioned in and out of the HAp structure with increasing nominal Fe content x. The excess Fe is oxidized to hematite. The TEM analysis and magnetic measurements support the results of the simultaneous Rietveld refinements. The TEM images show no significant effect on the morphology and size of the HAp particles upon Fe incorporation. The particles are either spheres or short rods of dimensions 20--60 nm. Hematite particles are imaged in the samples with x exceeding the solubility limit. These particles are spheres, about 15 nm in diameter and are more resistant to electron beam damage. Magnetic measurements reveal a transition of the diamagnetic pure HAp to paramagnetic Fe substituted HAp.

Refinement of the crystal structures of biomimetic weddellites produced by microscopic fungus Aspergillus niger

NASA Astrophysics Data System (ADS)

Rusakov, A. V.; Frank-Kamenetskaya, O. V.; Gurzhiy, V. V.; Zelenskaya, M. S.; Izatulina, A. R.; Sazanova, K. V.

2014-05-01

The single-crystal structures of four biomimetic weddellites CaC2O4 · (2 + x)H2O with different contents of zeolitic water ( x = 0.10-0.24 formula units) produced by the microscopic fungus Aspergillus niger were refined from X-ray diffraction data ( R = 0.029-0.038). The effect of zeolitic water content on the structural stability of weddellite was analyzed. The parameter a was shown to increase with increasing x due to the increase in the distance between water molecules along this direction. The water content and structural parameters of the synthesized weddellites are similar to those of weddellites from biofilms and kidney stones.

X-ray and gamma-ray line production by nonthermal ions

NASA Technical Reports Server (NTRS)

Bussard, R. W.; Omidvar, K.; Ramaty, R.

1977-01-01

X-ray production was calculated at approximately 6.8 keV by the 2p to 1s transition in fast hydrogen- and helium-like iron ions, following both electron capture to excited levels and collisional excitation. A refinement of the OBK approximation was used to obtain an improved charge exchange cross section. This, and the corresponding ionization cross section were used to determine equilibrium charge fractions for iron ions as functions of their energy. The effective X-ray line production cross section was found to be sharply peaked in energy at about 8 to 12 MeV/amu. Because fast ions of similar energies can also excite nuclear levels, the ratio of selected strong gamma ray line emissivities to the X-ray line emissivity was also calculated. Limits set by this method on the intensity of gamma ray line emission from the galactic center and the radio galaxy Centaurus A are generally lower than those reported in the literature.

Anchoring the Distance Scale via X-Ray/Infrared Data for Cepheid Clusters: SU Cas

NASA Astrophysics Data System (ADS)

Majaess, D.; Turner, D. G.; Gallo, L.; Gieren, W.; Bonatto, C.; Lane, D. J.; Balam, D.; Berdnikov, L.

2012-07-01

New X-ray (XMM-Newton) and JHKs (Observatoire du Mont-Mégantic) observations for members of the star cluster Alessi 95, which Turner et al. discovered hosts the classical Cepheid SU Cas, were used in tandem with UCAC3 (proper motion) and Two Micron All Sky Survey observations to determine precise cluster parameters: E(J - H) = 0.08 ± 0.02 and d = 405 ± 15 pc. The ensuing consensus among cluster, pulsation, and trigonometric distances (d=414+/- 5(\\sigma _{\\bar{x}}) +/- 10 (\\sigma) pc) places SU Cas in a select group of nearby fundamental Cepheid calibrators (δ Cep, ζ Gem). High-resolution X-ray observations may be employed to expand that sample as the data proved pertinent for identifying numerous stars associated with SU Cas. Acquiring X-ray observations of additional fields may foster efforts to refine Cepheid calibrations used to constrain H 0.

Simultaneous broadband observations and high-resolution X-ray spectroscopy of the transitional millisecond pulsar PSR J1023+0038

NASA Astrophysics Data System (ADS)

Coti Zelati, F.; Campana, S.; Braito, V.; Baglio, M. C.; D'Avanzo, P.; Rea, N.; Torres, D. F.

2018-03-01

We report on the first simultaneous XMM-Newton, NuSTAR, and Swift observations of the transitional millisecond pulsar PSR J1023+0038 in the X-ray active state. Our multi-wavelength campaign allowed us to investigate with unprecedented detail possible spectral variability over a broad energy range in the X-rays, as well as correlations and lags among emissions in different bands. The soft and hard X-ray emissions are significantly correlated, with no lags between the two bands. On the other hand, the X-ray emission does not correlate with the UV emission. We refine our model for the observed mode switching in terms of rapid transitions between a weak propeller regime and a rotation-powered radio pulsar state, and report on a detailed high-resolution X-ray spectroscopy using all XMM-Newton Reflection Grating Spectrometer data acquired since 2013. We discuss our results in the context of the recent discoveries on the system and of the state of the art simulations on transitional millisecond pulsars, and show how the properties of the narrow emission lines in the soft X-ray spectrum are consistent with an origin within the accretion disc.

Conformational Sampling of a Biomolecular Rugged Energy Landscape.

PubMed

Rydzewski, Jakub; Jakubowski, Rafal; Nicosia, Giuseppe; Nowak, Wieslaw

2018-01-01

The protein structure refinement using conformational sampling is important in hitherto protein studies. In this paper, we examined the protein structure refinement by means of potential energy minimization using immune computing as a method of sampling conformations. The method was tested on the x-ray structure and 30 decoys of the mutant of [Leu]Enkephalin, a paradigmatic example of the biomolecular multiple-minima problem. In order to score the refined conformations, we used a standard potential energy function with the OPLSAA force field. The effectiveness of the search was assessed using a variety of methods. The robustness of sampling was checked by the energy yield function which measures quantitatively the number of the peptide decoys residing in an energetic funnel. Furthermore, the potential energy-dependent Pareto fronts were calculated to elucidate dissimilarities between peptide conformations and the native state as observed by x-ray crystallography. Our results showed that the probed potential energy landscape of [Leu]Enkephalin is self-similar on different metric scales and that the local potential energy minima of the peptide decoys are metastable, thus they can be refined to conformations whose potential energy is decreased by approximately 250 kJ/mol.

Amorphous boron gasket in diamond anvil cell research

NASA Astrophysics Data System (ADS)

Lin, Jung-Fu; Shu, Jinfu; Mao, Ho-kwang; Hemley, Russell J.; Shen, Guoyin

2003-11-01

Recent advances in high-pressure diamond anvil cell experiments include high-energy synchrotron x-ray techniques as well as new cell designs and gasketing procedures. The success of high-pressure experiments usually depends on a well-prepared sample, in which the gasket plays an important role. Various gasket materials such as diamond, beryllium, rhenium, and stainless steel have been used. Here we introduce amorphous boron as another gasket material in high-pressure diamond anvil cell experiments. We have applied the boron gasket for laser-heating x-ray diffraction, radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, and inelastic x-ray scattering. The high shear strength of the amorphous boron maximizes the thickness of the sample chamber and increases the pressure homogeneity, improving the quality of high-pressure data. Use of amorphous boron avoids unwanted x-ray diffraction peaks and reduces the absorption of incident and x rays exiting the gasket material. The high quality of the diffraction patterns makes it possible to refine the cell parameters with powder x-ray diffraction data under high pressure and high temperature. The reactivity of boron prevents its use at high temperatures, however. When heated, boron may also react with the specimen to produce unwanted phases. The relatively porous boron starting material at ambient conditions also poses some challenges for sample preparation.

Use of barium-strontium carbonatite for flux welding and surfacing of mining machines

NASA Astrophysics Data System (ADS)

Kryukov, R. E.; Kozyrev, N. A.; Usoltsev, A. A.

2017-09-01

The results of application of barium-strontium carbonatite for modifying and refining iron-carbon alloys, used for welding and surfacing in ore mining and smelting industry, are generalized. The technology of manufacturing a flux additive containing 70 % of barium-strontium carbonatite and 30 % of liquid glass is proposed. Several compositions of welding fluxes based on silicomanganese slag were tested. The flux additive was introduced in an amount of 1, 3, 5 %. Technological features of welding with the application of the examined fluxes are determined. X-ray spectral analysis of the chemical composition of examined fluxes, slag crusts and weld metal was carried out, as well as metallographic investigations of welded joints. The principal possibility of applying barium-strontium carbonatite as a refining and gas-protective additive for welding fluxes is shown. The use of barium-strontium carbonatite reduces the contamination of the weld seam with nonmetallic inclusions: non-deforming silicates, spot oxides and brittle silicates, and increases the desulfurizing capacity of welding fluxes.

X-ray diffraction and infrared spectroscopy studies of Ba(Fe1/2Nb1/2)O3-(Na1/2Bi1/2)TiO3 ceramics

NASA Astrophysics Data System (ADS)

Chandra, K. P.; Yadav, Anjana; Prasad, K.

2018-05-01

Ceramics (1-x)Ba(Fe1/2Nb1/2)O3-x(Na1/2Bi1/2)TiO3; 0≤x≤1.0 were prepared by conventional ceramic synthesis technique. Rietveld refinements of X-ray diffraction data of these ceramics were carried out using FullProf software and determined their crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that Ba(Fe1/2Nb1/2)O3 has cubic structure with space group Pm 3 ¯ m and Na1/2Bi1/2)TiO3 has rhombohedral structure with space group R3c. Addition of (Na1/2Bi1/2)TiO3 to Ba(Fe1/2Nb1/2)O3 resulted in the change of unit cell structure from cubic to tetragonal (P4/mmm) for x = 0.75 and the X-Ray diffraction peaks slightly shift towards higher Bragg's angle, suggesting slight decrease in unit cell volume. SEM studies were carried out in order to access the quality of the prepared ceramics which showed a change in grain shapes with the increase of (Na1/2Bi1/2)TiO3 content. FTIR spectra confirmed the formation of perovskite type solid solutions.

Two-dimensional time-resolved X-ray diffraction study of liquid/solid fraction and solid particle size in Fe-C binary system with an electrostatic levitator furnace

NASA Astrophysics Data System (ADS)

Yonemura, M.; Okada, J.; Watanabe, Y.; Ishikawa, T.; Nanao, S.; Shobu, T.; Toyokawa, H.

2013-03-01

Liquid state provides functions such as matter transport or a reaction field and plays an important role in manufacturing processes such as refining, forging or welding. However, experimental procedures are significantly difficult for an observation of solidification process of iron and iron-based alloys in order to identify rapid transformations subjected to fast temperature evolution. Therefore, in order to study the solidification in iron and iron-based alloys, we considered a combination of high energy X-ray diffraction measurements and an electrostatic levitation method (ESL). In order to analyze the liquid/solid fraction, the solidification of melted spherical specimens was measured at a time resolution of 0.1 seconds during rapid cooling using the two-dimensional time-resolved X-ray diffraction. Furthermore, the observation of particle sizes and phase identification was performed on a trial basis using X-ray small angle scattering with X-ray diffraction.

Ultra-high-resolution X-ray structure of proteins.

PubMed

Lecomte, C; Guillot, B; Muzet, N; Pichon-Pesme, V; Jelsch, C

2004-04-01

The constant advances in synchrotron radiation sources and crystallogenesis methods and the impulse of structural genomics projects have brought biocrystallography to a context favorable to subatomic resolution protein and nucleic acid structures. Thus, as soon as such precision can be frequently obtained, the amount of information available in the precise electron density should also be easily and naturally exploited, similarly to the field of small molecule charge density studies. Indeed, the use of a nonspherical model for the atomic electron density in the refinement of subatomic resolution protein structures allows the experimental description of their electrostatic properties. Some methods we have developed and implemented in our multipolar refinement program MoPro for this purpose are presented. Examples of successful applications to several subatomic resolution protein structures, including the 0.66 angstrom resolution human aldose reductase, are described.

X-ray and optical observations of four polars

NASA Astrophysics Data System (ADS)

Worpel, H.; Schwope, A. D.; Granzer, T.; Reinsch, K.; Schwarz, R.; Traulsen, I.

2016-08-01

Aims: We investigate the temporal and spectral behaviour of four polar cataclysmic variables from the infrared to X-ray regimes, refine our knowledge of the physical parameters of these systems at different accretion rates, and search for a possible excess of soft X-ray photons. Methods: We obtained and analysed four XMM-Newton X-ray observations of three of the sources, two of them discovered with the SDSS and one in the RASS. The X-ray data were complemented by optical photometric and spectroscopic observations and, for two sources, archival Swift observations. Results: SDSSJ032855.00+052254.2 was X-ray bright in two XMM-Newton and two Swift observations, and shows transitions from high and low accretion states on a timescale of a few months. The source shows no significant soft excess. We measured the magnetic field strength at the main accreting pole to be 39 MG and the inclination to be 45° ≤ I ≤ 77°, and we refined the long-term ephemeris. SDSSJ133309.20+143706.9 was X-ray faint. We measured a faint phase X-ray flux and plasma temperature for this source, which seems to spend almost all of its time accreting at a low level. Its inclination is less than about 76°. 1RXSJ173006.4+033813 was X-ray bright in the XMM-Newton observation. Its spectrum contained a modest soft blackbody component, not luminous enough to be considered a significant soft excess. We inferred a magnetic field strength at the main accreting pole of 20 to 25 MG, and that the inclination is less than 77° and probably less than 63°. V808 Aur, also known as CSS081231:J071126+440405, was X-ray faint in the Swift observation, but there is nonetheless strong evidence for bright and faint phases in X-rays and perhaps in UV. Residual X-ray flux from the faint phase is difficult to explain by thermal emission from the white dwarf surface, or by accretion onto the second pole. We present a revised distance estimate of 250 pc. Conclusions: The three systems we were able to study in detail appear to be normal polars with luminosities and magnetic field strengths typical for this class of accreting binary. None of the four systems studied shows the strong soft excess thought commonplace in polars prior to the XMM-Newton era. Based on observations obtained with XMM-Newton, an ESA science mission with instruments and contributions directly funded by ESA Member States and NASA.Based on observations collected at the Centro Astronómico Hispano Alemán (CAHA) at Calar Alto, operated jointly by the Max Planck Institut für Astronomie and the Instituto de Astrofísica de Andalucía (CSIC).

Investigation of the structure of human dental tissue at multiple length scales using high energy synchrotron X-ray SAXS/WAXS

NASA Astrophysics Data System (ADS)

Sui, Tan; Landini, Gabriel; Korsunsky, Alexander M.

2011-10-01

High energy (>50keV) synchrotron X-ray scattering experiments were carried out on beamline I12 JEEP at the Diamond Light Source (DLS, Oxford, UK). Although a complete human tooth could be studied, in the present study attention was focused on coupons from the region of the Dentin-Enamel Junction (DEJ). Simultaneous high energy SAXS/WAXS measurements were carried out. Quantitative analysis of the results allows multiple length scale characterization of the nano-crystalline structure of dental tissues. SAXS patterns analysis provide insight into the mean thickness and orientation of hydroxyapatite particles, while WAXS (XRD) patterns allow the determination of the crystallographic unit cell parameters of the hydroxyapatite phase. It was found that the average particle thickness determined from SAXS interpretation varies as a function of position in the vicinity of the DEJ. Most mineral particles are randomly orientated within dentin, although preferred orientation emerges and becomes stronger on approach to the enamel. Within the enamel, texture is stronger than anywhere in the dentin, and the determination of lattice parameters can be accomplished by Pawley refinement of the multiple peak diffraction pattern. The results demonstrate the feasibility of using high energy synchrotron X-ray beams for the characterization of human dental tissues. This opens up the opportunity of studying thick samples (e.g., complete teeth) in complex sample environments (e.g., under saline solution). This opens new avenues for the application of high energy synchrotron X-ray scattering to dental research.

Finite element analyses of thin film active grazing incidence x-ray optics

NASA Astrophysics Data System (ADS)

Davis, William N.; Reid, Paul B.; Schwartz, Daniel A.

2010-09-01

The Chandra X-ray Observatory, with its sub-arc second resolution, has revolutionized X-ray astronomy by revealing an extremely complex X-ray sky and demonstrating the power of the X-ray window in exploring fundamental astrophysical problems. Larger area telescopes of still higher angular resolution promise further advances. We are engaged in the development of a mission concept, Generation-X, a 0.1 arc second resolution x-ray telescope with tens of square meters of collecting area, 500 times that of Chandra. To achieve these two requirements of imaging and area, we are developing a grazing incidence telescope comprised of many mirror segments. Each segment is an adjustable mirror that is a section of a paraboloid or hyperboloid, aligned and figure corrected in situ on-orbit. To that end, finite element analyses of thin glass mirrors are performed to determine influence functions for each actuator on the mirrors, in order to develop algorithms for correction of mirror deformations. The effects of several mirror mounting schemes are also studied. The finite element analysis results, combined with measurements made on prototype mirrors, will be used to further refine the correction algorithms.

Surface applicator of a miniature X-ray tube for superficial electronic brachytherapy of skin cancer.

PubMed

Kim, Hyun Nam; Lee, Ju Hyuk; Park, Han Beom; Kim, Hyun Jin; Cho, Sung Oh

2018-01-01

We designed and fabricated a surface applicator of a novel carbon nanotube (CNT)-based miniature X-ray tube for the use in superficial electronic brachytherapy of skin cancer. To investigate the effectiveness of the surface applicator, the performance of the applicator was numerically and experimentally analyzed. The surface applicator consists of a graphite flattening filter and an X-ray shield. A Monte Carlo radiation transport code, MCNP6, was used to optimize the geometries of both the flattening filter and the shield so that X-rays are generated uniformly over the desired region. The performance of the graphite filter was compared with that of conventional aluminum (Al) filters of different geometries using the numerical simulations. After fabricating a surface applicator, the X-ray spatial distribution was measured to evaluate the performance of the applicator. The graphite filter shows better spatial dose uniformity and less dose distortion than Al filters. Moreover, graphite allows easy fabrication of the flattening filter due to its low X-ray attenuation property, which is particularly important for low-energy electronic brachytherapy. The applicator also shows that no further X-ray shielding is required for the application because unwanted X-rays are completely protected. As a result, highly uniform X-ray dose distribution was achieved from the miniature X-ray tube mounted with the surface applicators. The measured values of both flatness and symmetry were less than 5% and the measured penumbra values were less than 1 mm. All these values satisfy the currently accepted tolerance criteria for radiation therapy. The surface applicator exhibits sufficient performance capability for their application in electronic brachytherapy of skin cancers. © 2017 American Association of Physicists in Medicine.

The Quality and Validation of Structures from Structural Genomics

PubMed Central

Domagalski, Marcin J.; Zheng, Heping; Zimmerman, Matthew D.; Dauter, Zbigniew; Wlodawer, Alexander; Minor, Wladek

2014-01-01

Quality control of three-dimensional structures of macromolecules is a critical step to ensure the integrity of structural biology data, especially those produced by structural genomics centers. Whereas the Protein Data Bank (PDB) has proven to be a remarkable success overall, the inconsistent quality of structures reveals a lack of universal standards for structure/deposit validation. Here, we review the state-of-the-art methods used in macromolecular structure validation, focusing on validation of structures determined by X-ray crystallography. We describe some general protocols used in the rebuilding and re-refinement of problematic structural models. We also briefly discuss some frontier areas of structure validation, including refinement of protein–ligand complexes, automation of structure redetermination, and the use of NMR structures and computational models to solve X-ray crystal structures by molecular replacement. PMID:24203341

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

Kiyota, Eduardo; Centro de Biologia Molecular e Engenharia Genética, Universidade Estadual de Campinas, Campinas-SP; Sousa, Sylvia Morais de

Preliminary X-ray diffraction studies of apo maize aldose reductase at 2.0 Å resolution are reported. Maize aldose reductase (AR) is a member of the aldo-keto reductase superfamily. In contrast to human AR, maize AR seems to prefer the conversion of sorbitol into glucose. The apoenzyme was crystallized in space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 47.2, b = 54.5, c = 100.6 Å and one molecule in the asymmetric unit. Synchrotron X-ray diffraction data were collected and a final resolution limit of 2.0 Å was obtained after data reduction. Phasing was carried out by an automatedmore » molecular-replacement procedure and structural refinement is currently in progress. The refined structure is expected to shed light on the functional/enzymatic mechanism and the unusual activities of maize AR.« less

Na, K, Rb, and Cs Exchange in Heulandite Single-Crystals: X-Ray Structure Refinements at 100 K

NASA Astrophysics Data System (ADS)

Yang, Ping; Armbruster, Thomas

1996-04-01

The crystal structures of Na-, K-, Rb-, and Cs-exchanged varieties of the zeolite heulandite with the simplified compositionM+9Al9Si27O72·nH2O were studied by single-crystal X-ray diffraction at 100 K. The structure refinements of Na-, K-, and Rb-exchanged heulandite were performed in space groupC2/mwith resultantRvalues of 3.8, 3.0, and 4.9%, respectively. Cs-exchanged heulandite was refined in space groupC[formula], yielding anRvalue of 3.4%. X-ray single-crystal data of the Cs-exchanged variety indicated that many reflections of typeh k lwere not equivalent toh -k las expected for monoclinic symmetry. With increasing radius of the incorporated channel cations, thebaxis increases from 17.93 to 18.09 Å leading to a slight widening of the channels. The number of H2O molecules also decreases with increasing cation radius due to space limitations. Three general cation positions (II-1,C3, andB4) were found in the four exchanged heulandite samples. For Rb- and Cs-exchanged crystals, the additional cation siteA2 occurs. In Cs-exchanged heulandite symmetry lowering is due to partial Si, Al ordering in the framework accompanied with a more asymmetric arrangement of channel Cs. Only if heavy elements in the channels are present the symmetry information of the framework is enforced, thus partial Si, Al ordering can be resolved.

Application of micro-X-ray fluorescence to chemical mapping of polar ice

NASA Astrophysics Data System (ADS)

Fourcade, M. C. Morel; Barnola, J. M.; Susini, J.; Baker, R.; Durand, G.; de Angelis, M.; Duval, P.

Synchrotron-based micro-X-ray fluorescence (μXRF) equipment has been used to analyze impurities in polar ice. A customized sample holder has been developed and the μXRF equipment has been adapted with a thermal control system to keep samples unaltered during analyses. Artificial ice samples prepared from ultra-pure water were analyzed to investigate possible contamination and/or experimental artefacts. Analyses of polar ice from Antarctica (Dome C and Vostok) confirm this μXRF technique is non-destructive and sensitive. Experiments can be reproduced to confirm or refine results by focusing on interesting spots such as crystal grain boundaries or specific inclusions. Integration times and resolution can be adjusted to optimize sensitivity. Investigation of unstable particles is possible due to the short analysis time. In addition to identification of elements in impurities, μXRF is able to determine their speciations. The accuracy and reliability of the results confirm the potential of this technique for research in glaciology.

A novel molten-salt electrochemical cell for investigating the reduction of uranium dioxide to uranium metal by lithium using in situ synchrotron radiation

PubMed Central

Brown, Leon D.; Abdulaziz, Rema; Jervis, Rhodri; Bharath, Vidal; Mason, Thomas J.; Reinhard, Christina; Connor, Leigh D.; Inman, Douglas; Brett, Daniel J. L.; Shearing, Paul R.

2017-01-01

A novel electrochemical cell has been designed and built to allow for in situ energy-dispersive X-ray diffraction measurements to be made during reduction of UO2 to U metal in LiCl–KCl at 500°C. The electrochemical cell contains a recessed well at the bottom of the cell into which the working electrode sits, reducing the beam path for the X-rays through the molten-salt and maximizing the signal-to-noise ratio from the sample. Lithium metal was electrodeposited onto the UO2 working electrode by exposing the working electrode to more negative potentials than the Li deposition potential of the LiCl–KCl eutectic electrolyte. The Li metal acts as a reducing agent for the chemical reduction of UO2 to U, which appears to proceed to completion. All phases were fitted using Le Bail refinement. The cell is expected to be widely applicable to many studies involving molten-salt systems. PMID:28244437

A novel molten-salt electrochemical cell for investigating the reduction of uranium dioxide to uranium metal by lithium using in situ synchrotron radiation.

PubMed

Brown, Leon D; Abdulaziz, Rema; Jervis, Rhodri; Bharath, Vidal; Mason, Thomas J; Atwood, Robert C; Reinhard, Christina; Connor, Leigh D; Inman, Douglas; Brett, Daniel J L; Shearing, Paul R

2017-03-01

A novel electrochemical cell has been designed and built to allow for in situ energy-dispersive X-ray diffraction measurements to be made during reduction of UO 2 to U metal in LiCl-KCl at 500°C. The electrochemical cell contains a recessed well at the bottom of the cell into which the working electrode sits, reducing the beam path for the X-rays through the molten-salt and maximizing the signal-to-noise ratio from the sample. Lithium metal was electrodeposited onto the UO 2 working electrode by exposing the working electrode to more negative potentials than the Li deposition potential of the LiCl-KCl eutectic electrolyte. The Li metal acts as a reducing agent for the chemical reduction of UO 2 to U, which appears to proceed to completion. All phases were fitted using Le Bail refinement. The cell is expected to be widely applicable to many studies involving molten-salt systems.

Expression, purification, crystallization and preliminary X-ray diffraction analysis of the pectin methylesterase from the sugar cane weevil Sphenophorus levis.

PubMed

Evangelista, Danilo Elton; Schutzer de Godoy, Andre; Fonseca Pereira de Paula, Fernando; Henrique-Silva, Flavio; Polikarpov, Igor

2014-03-01

Pectin methylesterase removes the methyl groups from the main chain of pectin, the major component of the middle lamella of the plant cell wall. The enzyme is involved in plant cell-wall development, is part of the enzymatic arsenal used by microorganisms to attack plants and also has a wide range of applications in the industrial sector. Therefore, there is a considerable interest in studies of the structure and function of this enzyme. In this work, the pectin methylesterase from Sphenophorus levis was produced in Pichia pastoris and purified. Crystals belonging to the monoclinic space group C2, with unit-cell parameters a = 122.181, b = 82.213, c = 41.176 Å, β = 97.48°, were obtained by the sitting-drop vapour-diffusion method and an X-ray diffraction data set was collected to 2.1 Å resolution. Structure refinement and model building are in progress.

Gold nanoparticle contrast agents in advanced X-ray imaging technologies.

PubMed

Ahn, Sungsook; Jung, Sung Yong; Lee, Sang Joon

2013-05-17

Recently, there has been significant progress in the field of soft- and hard-X-ray imaging for a wide range of applications, both technically and scientifically, via developments in sources, optics and imaging methodologies. While one community is pursuing extensive applications of available X-ray tools, others are investigating improvements in techniques, including new optics, higher spatial resolutions and brighter compact sources. For increased image quality and more exquisite investigation on characteristic biological phenomena, contrast agents have been employed extensively in imaging technologies. Heavy metal nanoparticles are excellent absorbers of X-rays and can offer excellent improvements in medical diagnosis and X-ray imaging. In this context, the role of gold (Au) is important for advanced X-ray imaging applications. Au has a long-history in a wide range of medical applications and exhibits characteristic interactions with X-rays. Therefore, Au can offer a particular advantage as a tracer and a contrast enhancer in X-ray imaging technologies by sensing the variation in X-ray attenuation in a given sample volume. This review summarizes basic understanding on X-ray imaging from device set-up to technologies. Then this review covers recent studies in the development of X-ray imaging techniques utilizing gold nanoparticles (AuNPs) and their relevant applications, including two- and three-dimensional biological imaging, dynamical processes in a living system, single cell-based imaging and quantitative analysis of circulatory systems and so on. In addition to conventional medical applications, various novel research areas have been developed and are expected to be further developed through AuNP-based X-ray imaging technologies.

Plasma properties of hot coronal loops utilizing coordinated SMM and solar research rocket observations

NASA Technical Reports Server (NTRS)

Moses, J. Daniel

1989-01-01

Three improvements in photographic x-ray imaging techniques for solar astronomy are presented. The testing and calibration of a new film processor was conducted; the resulting product will allow photometric development of sounding rocket flight film immediately upon recovery at the missile range. Two fine grained photographic films were calibrated and flight tested to provide alternative detector choices when the need for high resolution is greater than the need for high sensitivity. An analysis technique used to obtain the characteristic curve directly from photographs of UV solar spectra were applied to the analysis of soft x-ray photographic images. The resulting procedure provides a more complete and straightforward determination of the parameters describing the x-ray characteristic curve than previous techniques. These improvements fall into the category of refinements instead of revolutions, indicating the fundamental suitability of the photographic process for x-ray imaging in solar astronomy.

Catalysis of GTP Hydrolysis by Small GTPases at Atomic Detail by Integration of X-ray Crystallography, Experimental, and Theoretical IR Spectroscopy*

PubMed Central

Rudack, Till; Jenrich, Sarah; Brucker, Sven; Vetter, Ingrid R.; Gerwert, Klaus; Kötting, Carsten

2015-01-01

Small GTPases regulate key processes in cells. Malfunction of their GTPase reaction by mutations is involved in severe diseases. Here, we compare the GTPase reaction of the slower hydrolyzing GTPase Ran with Ras. By combination of time-resolved FTIR difference spectroscopy and QM/MM simulations we elucidate that the Mg2+ coordination by the phosphate groups, which varies largely among the x-ray structures, is the same for Ran and Ras. A new x-ray structure of a Ran·RanBD1 complex with improved resolution confirmed this finding and revealed a general problem with the refinement of Mg2+ in GTPases. The Mg2+ coordination is not responsible for the much slower GTPase reaction of Ran. Instead, the location of the Tyr-39 side chain of Ran between the γ-phosphate and Gln-69 prevents the optimal positioning of the attacking water molecule by the Gln-69 relative to the γ-phosphate. This is confirmed in the RanY39A·RanBD1 crystal structure. The QM/MM simulations provide IR spectra of the catalytic center, which agree very nicely with the experimental ones. The combination of both methods can correlate spectra with structure at atomic detail. For example the FTIR difference spectra of RasA18T and RanT25A mutants show that spectral differences are mainly due to the hydrogen bond of Thr-25 to the α-phosphate in Ran. By integration of x-ray structure analysis, experimental, and theoretical IR spectroscopy the catalytic center of the x-ray structural models are further refined to sub-Å resolution, allowing an improved understanding of catalysis. PMID:26272610

Catalysis of GTP hydrolysis by small GTPases at atomic detail by integration of X-ray crystallography, experimental, and theoretical IR spectroscopy.

PubMed

Rudack, Till; Jenrich, Sarah; Brucker, Sven; Vetter, Ingrid R; Gerwert, Klaus; Kötting, Carsten

2015-10-02

Small GTPases regulate key processes in cells. Malfunction of their GTPase reaction by mutations is involved in severe diseases. Here, we compare the GTPase reaction of the slower hydrolyzing GTPase Ran with Ras. By combination of time-resolved FTIR difference spectroscopy and QM/MM simulations we elucidate that the Mg(2+) coordination by the phosphate groups, which varies largely among the x-ray structures, is the same for Ran and Ras. A new x-ray structure of a Ran·RanBD1 complex with improved resolution confirmed this finding and revealed a general problem with the refinement of Mg(2+) in GTPases. The Mg(2+) coordination is not responsible for the much slower GTPase reaction of Ran. Instead, the location of the Tyr-39 side chain of Ran between the γ-phosphate and Gln-69 prevents the optimal positioning of the attacking water molecule by the Gln-69 relative to the γ-phosphate. This is confirmed in the RanY39A·RanBD1 crystal structure. The QM/MM simulations provide IR spectra of the catalytic center, which agree very nicely with the experimental ones. The combination of both methods can correlate spectra with structure at atomic detail. For example the FTIR difference spectra of RasA18T and RanT25A mutants show that spectral differences are mainly due to the hydrogen bond of Thr-25 to the α-phosphate in Ran. By integration of x-ray structure analysis, experimental, and theoretical IR spectroscopy the catalytic center of the x-ray structural models are further refined to sub-Å resolution, allowing an improved understanding of catalysis. © 2015 by The American Society for Biochemistry and Molecular Biology, Inc.

The Mapping X-Ray Fluorescence Spectrometer (MAPX)

NASA Technical Reports Server (NTRS)

Blake, David; Sarrazin, Philippe; Bristow, Thomas; Downs, Robert; Gailhanou, Marc; Marchis, Franck; Ming, Douglas; Morris, Richard; Sole, Vincente Armando; Thompson, Kathleen;

Thermally induced phase transformation in multi-phase iron oxide nanoparticles on vacuum annealing

NASA Astrophysics Data System (ADS)

Anupama, A. V.; Keune, W.; Sahoo, B.

2017-10-01

The evolution of magnetic phases in multi-phase iron oxide nanoparticles, synthesized via the transferred arc plasma induced gas phase condensation method, was investigated by X-ray diffraction, vibrating sample magnetometry and 57Fe Mössbauer spectroscopy. The particles are proposed to be consisting of three different iron oxide phases: α-Fe2O3, γ-Fe2O3 and Fe3O4. These nanoparticles were exposed to high temperature (∼935 K) under vacuum (10-3 mbar He pressure), and the thermally induced phase transformations were investigated. The Rietveld refinement of the X-ray diffraction data corroborates the least-squares fitting of the transmission Mössbauer spectra in confirming the presence of Fe3O4, γ-Fe2O3 and α-Fe2O3 phases before the thermal treatment, while only Fe3O4 and α-Fe2O3 phases exist after thermal treatment. On thermal annealing in vacuum, conversion from γ-Fe2O3 to Fe3O4 and α-Fe2O3 was observed. Interestingly, we have observed a phase transformation occurring in the temperature range ∼498 K-538 K, which is strikingly lower than the phase transformation temperature of γ-Fe2O3 to α-Fe2O3 (573-623 K) in air. Combining the results of Rietveld refinement of X-ray diffraction patterns and Mössbauer spectroscopy, we have attributed this phase transformation to the phase conversion of a metastable "defected and strained" d-Fe3O4 phase, present in the as-prepared sample, to the α-Fe2O3 phase. Stabilization of the phases by controlling the phase transformations during the use of different iron-oxide nanoparticles is the key factor to select them for a particular application. Our investigation provides insight into the effect of temperature and chemical nature of the environment, which are the primary factors governing the phase stability, suitability and longevity of the iron oxide nanomaterials prepared by the gas-phase condensation method for various applications.

Quantum crystallographic charge density of urea

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

Wall, Michael E.

Standard X-ray crystallography methods use free-atom models to calculate mean unit-cell charge densities. Real molecules, however, have shared charge that is not captured accurately using free-atom models. To address this limitation, a charge density model of crystalline urea was calculated using high-level quantum theory and was refined against publicly available ultra-high-resolution experimental Bragg data, including the effects of atomic displacement parameters. The resulting quantum crystallographic model was compared with models obtained using spherical atom or multipole methods. Despite using only the same number of free parameters as the spherical atom model, the agreement of the quantum model with the datamore » is comparable to the multipole model. The static, theoretical crystalline charge density of the quantum model is distinct from the multipole model, indicating the quantum model provides substantially new information. Hydrogen thermal ellipsoids in the quantum model were very similar to those obtained using neutron crystallography, indicating that quantum crystallography can increase the accuracy of the X-ray crystallographic atomic displacement parameters. Lastly, the results demonstrate the feasibility and benefits of integrating fully periodic quantum charge density calculations into ultra-high-resolution X-ray crystallographic model building and refinement.« less

Quantum crystallographic charge density of urea

DOE PAGES

Wall, Michael E.

2016-06-08

Standard X-ray crystallography methods use free-atom models to calculate mean unit-cell charge densities. Real molecules, however, have shared charge that is not captured accurately using free-atom models. To address this limitation, a charge density model of crystalline urea was calculated using high-level quantum theory and was refined against publicly available ultra-high-resolution experimental Bragg data, including the effects of atomic displacement parameters. The resulting quantum crystallographic model was compared with models obtained using spherical atom or multipole methods. Despite using only the same number of free parameters as the spherical atom model, the agreement of the quantum model with the datamore » is comparable to the multipole model. The static, theoretical crystalline charge density of the quantum model is distinct from the multipole model, indicating the quantum model provides substantially new information. Hydrogen thermal ellipsoids in the quantum model were very similar to those obtained using neutron crystallography, indicating that quantum crystallography can increase the accuracy of the X-ray crystallographic atomic displacement parameters. Lastly, the results demonstrate the feasibility and benefits of integrating fully periodic quantum charge density calculations into ultra-high-resolution X-ray crystallographic model building and refinement.« less

Structure resolution by electron diffraction tomography of the complex layered iron-rich Fe-2234-type Sr{sub 5}Fe{sub 6}O{sub 15.4}

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

Lepoittevin, Christophe, E-mail: christophe.lepoittevin@neel.cnrs.fr

2016-10-15

The crystal structure of the strontium ferrite Sr{sub 5}Fe{sub 6}O{sub 15.4}, was solved by direct methods on electron diffraction tomography data acquired on a transmission electron microscope. The refined cell parameters are a=27.4047(3) Å, b=5.48590(7) Å and c=42.7442(4) Å in Fm2m symmetry. Its structure is built up from the intergrowth sequence between a quadruple perovskite-type layer with a complex rock-salt (RS)-type block. In the latter iron atoms are found in two different environments : tetragonal pyramid and tetrahedron. The structural model was refined by Rietveld method based on the powder X-ray diffraction pattern. - Highlights: • Complex structure of Sr{submore » 5}Fe{sub 6}O{sub 15.4} solved by electron diffraction tomography. • Observed Fourier maps allow determining missing oxygen atoms in the structure. • Structural model refined from powder X-ray diffraction data. • Intergrowth between quadruple perovskite layer with double rock-salt-type layer.« less

HPHT synthesis, structure and electrical properties of type-I clathrates Ba{sub 8}Al{sub x}Si{sub 46−x}

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

Liu, Binwu; Jia, Xiaopeng; Sun, Hairui

2016-01-15

Clathrate compounds Ba{sub 8}Al{sub x}Si{sub 46−x} were successfully synthesized using the method of high-pressure and high-temperature (HPHT). In this process, we used BaSi{sub 2} as one of the starting materials in place of Ba metals, which reduces the complexity of the program caused by the extremely high chemical reactivity. By using this method, the processing time was reduced from few days to an hour. X-ray diffraction and structural refinement indicated this composition crystallized in type-I clathrate phase. Bond length analysis showed the Ba atoms in small dodecahedron had spherical thermal ellipsoids while those in large tetrakaidecahedron displayed anisotropic thermal ellipsoids.more » The negative Seebeck coefficient indicated transport processes were dominated by electrons as carriers, and increased with the increasing temperature. The electrical properties, including Seebeck coefficient and Power factor, were greatly enhanced by Al substitution. - Graphical abstract: Left: The cavity structure diagram of a China-type large volume cubic high-pressure apparatus, and the Type-I clathrate structure of sample synthesized using HPHT. Middle: X-ray Rietveld refinement profile for Ba{sub 8}Si{sub 46} and element mapping for Ba{sub 8}Al{sub 16}Si{sub 30}. Right: Temperature dependence of Seebeck coefficient for Ba{sub 8}Al{sub x}Si{sub 46−x} prepared by HPHT. - Highlights: • HPHT is a simple and rapid synthetic approach. • We use BaSi{sub 2} as one of the starting materials replacing Ba metals. • The processing time reduces from few days to an hour. • Structure determination is refined by Rietveld analysis of XRD data. • Variable temperature electrical properties are characterized.« less

An Efficient Metadynamics-Based Protocol To Model the Binding Affinity and the Transition State Ensemble of G-Protein-Coupled Receptor Ligands.

PubMed

Saleh, Noureldin; Ibrahim, Passainte; Saladino, Giorgio; Gervasio, Francesco Luigi; Clark, Timothy

2017-05-22

A generally applicable metadynamics scheme for predicting the free energy profile of ligand binding to G-protein-coupled receptors (GPCRs) is described. A common and effective collective variable (CV) has been defined using the ideally placed and highly conserved Trp6.48 as a reference point for ligand-GPCR distance measurement and the common orientation of GPCRs in the cell membrane. Using this single CV together with well-tempered multiple-walker metadynamics with a funnel-like boundary allows an efficient exploration of the entire ligand binding path from the extracellular medium to the orthosteric binding site, including vestibule and intermediate sites. The protocol can be used with X-ray structures or high-quality homology models (based on a high-quality template and after thorough refinement) for the receptor and is universally applicable to agonists, antagonists, and partial and reverse agonists. The root-mean-square error (RMSE) in predicted binding free energies for 12 diverse ligands in five receptors (a total of 23 data points) is surprisingly small (less than 1 kcal mol -1 ). The RMSEs for simulations that use receptor X-ray structures and homology models are very similar.

Compound refractive X-ray lens

DOEpatents

Nygren, David R.; Cahn, Robert; Cederstrom, Bjorn; Danielsson, Mats; Vestlund, Jonas

2000-01-01

An apparatus and method for focusing X-rays. In one embodiment, his invention is a commercial-grade compound refractive X-ray lens. The commercial-grade compound refractive X-ray lens includes a volume of low-Z material. The volume of low-Z material has a first surface which is adapted to receive X-rays of commercially-applicable power emitted from a commercial-grade X-ray source. The volume of low-Z material also has a second surface from which emerge the X-rays of commercially-applicable power which were received at the first surface. Additionally, the commercial-grade compound refractive X-ray lens includes a plurality of openings which are disposed between the first surface and the second surface. The plurality of openings are oriented such that the X-rays of commercially-applicable power which are received at the first surface, pass through the volume of low-Z material and through the plurality openings. In so doing, the X-rays which emerge from the second surface are refracted to a focal point.

Ba0.06(Na,Bi)0.94Ti1-x(Ni1/3Nb2/3)xO3 ceramics: X-ray diffraction and infrared spectroscopy studies

NASA Astrophysics Data System (ADS)

Mishra, R. K.; Prasad, Ashutosh; Chandra, K. P.; Prasad, K.

2018-05-01

Non-lead ceramic samples of Ba0.06(Na0.5Bi0.5)0.94Ti1-x(Ni1/3Nb2/3)xO3; 0 ≤ x ≤ 1.0 were prepared by standard high temperature ceramic synthesis method. Rietveld refinements of X-ray diffraction data of these ceramics were carried out using FullProf software and determined their crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that Ba0.06(Na0.5Bi0.5)0.94TiO3 has a monoclinic structure with space group P4/m while B0.06(Na0.5Bi0.5)0.94(Ni1/3Nb2/3)O3 has tetragonal (pseudo-cubic) structure with space group P4/mmm. Partial replacement of Ti4+ ion by pseudo-cation (Ni1/33 +Nb2/3 5 +) 4 + resulted in the change of unit cell structure from monoclinic to tetragonal. SEM studies were carried out in order to access the quality of the prepared ceramics which showed a change in grain sizes with the increase of (Ni1/33 +Nb2/3 5 +) 4 + content. FTIR spectra confirmed the formation of perovskite type solid solutions.

The Mapping X-ray Fluorescence Spectrometer (MapX)

NASA Astrophysics Data System (ADS)

Sarrazin, P.; Blake, D. F.; Marchis, F.; Bristow, T.; Thompson, K.

2017-12-01

Many planetary surface processes leave traces of their actions as features in the size range 10s to 100s of microns. The Mapping X-ray Fluorescence Spectrometer (MapX) will provide elemental imaging at 100 micron spatial resolution, yielding elemental chemistry at a scale where many relict physical, chemical, or biological features can be imaged and interpreted in ancient rocks on planetary bodies and planetesimals. MapX is an arm-based instrument positioned on a rock or regolith with touch sensors. During an analysis, an X-ray source (tube or radioisotope) bombards the sample with X-rays or alpha-particles / gamma-rays, resulting in sample X-ray Fluorescence (XRF). X-rays emitted in the direction of an X-ray sensitive CCD imager pass through a 1:1 focusing lens (X-ray micro-pore Optic (MPO)) that projects a spatially resolved image of the X-rays onto the CCD. The CCD is operated in single photon counting mode so that the energies and positions of individual X-ray photons are recorded. In a single analysis, several thousand frames are both stored and processed in real-time. Higher level data products include single-element maps with a lateral spatial resolution of 100 microns and quantitative XRF spectra from ground- or instrument- selected Regions of Interest (ROI). XRF spectra from ROI are compared with known rock and mineral compositions to extrapolate the data to rock types and putative mineralogies. When applied to airless bodies and implemented with an appropriate radioisotope source for alpha-particle excitation, MapX will be able to analyze biogenic elements C, N, O, P, S, in addition to the cations of the rock-forming elements >Na, accessible with either X-ray or gamma-ray excitation. The MapX concept has been demonstrated with a series of lab-based prototypes and is currently under refinement and TRL maturation.

Crystallization and X-ray data analysis of the 10 kDa C-terminal lid subdomain from Caenorhabditis elegans Hsp70

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

Worrall, Liam; Walkinshaw, Malcolm D., E-mail: m.walkinshaw@ed.ac.uk

Crystals of the C-terminal 10 kDa lid subdomain from the C. elegans chaperone Hsp70 have been obtained that diffract X-rays to ∼3.5 Å and belong to space group I2{sub 1}2{sub 1}2{sub 1}. Analysis of X-ray data and initial heavy-atom phasing reveals 24 monomers in the asymmetric unit related by 432 non-crystallographic symmetry. Hsp70 is an important molecular chaperone involved in the regulation of protein folding. Crystals of the C-terminal 10 kDa helical lid domain (residues 542–640) from a Caenorhabditis elegans Hsp70 homologue have been produced that diffract X-rays to ∼3.4 Å. Crystals belong to space group I2{sub 1}2{sub 1}2{sub 1},more » with unit-cell parameters a = b = 197, c = 200 Å. The Matthews coefficient, self-rotation function and Patterson map indicate 24 monomers in the asymmetric unit, showing non-crystallographic 432 symmetry. Molecular-replacement studies using the corresponding domain from rat, the only eukaryotic homologue with a known structure, failed and a mercury derivative was obtained. Preliminary MAD phasing using SHELXD and SHARP for location and refinement of the heavy-atom substructure and SOLOMON for density modification produced interpretable maps with a clear protein–solvent boundary. Further density-modification, model-building and refinement are currently under way.« less

A revised partiality model and post-refinement algorithm for X-ray free-electron laser data

DOE PAGES

Ginn, Helen Mary; Brewster, Aaron S.; Hattne, Johan; ...

2015-05-23

Research towards using X-ray free-electron laser (XFEL) data to solve structures using experimental phasing methods such as sulfur single-wavelength anomalous dispersion (SAD) has been hampered by shortcomings in the diffraction models for X-ray diffraction from FELs. Owing to errors in the orientation matrix and overly simple partiality models, researchers have required large numbers of images to converge to reliable estimates for the structure-factor amplitudes, which may not be feasible for all biological systems. Here, data for cytoplasmic polyhedrosis virus type 17 (CPV17) collected at 1.3 Å wavelength at the Linac Coherent Light Source (LCLS) are revisited. A previously published definitionmore » of a partiality model for reflections illuminated by self-amplified spontaneous emission (SASE) pulses is built upon, which defines a fraction between 0 and 1 based on the intersection of a reflection with a spread of Ewald spheres modelled by a super-Gaussian wavelength distribution in the X-ray beam. A method of post-refinement to refine the parameters of this model is suggested. This has generated a merged data set with an overall discrepancy (by calculating theR splitvalue) of 3.15% to 1.46 Å resolution from a 7225-image data set. The atomic numbers of C, N and O atoms in the structure are distinguishable in the electron-density map. There are 13 S atoms within the 237 residues of CPV17, excluding the initial disordered methionine. These only possess 0.42 anomalous scattering electrons each at 1.3 Å wavelength, but the 12 that have single predominant positions are easily detectable in the anomalous difference Fourier map. It is hoped that these improvements will lead towards XFEL experimental phase determination and structure determination by sulfur SAD and will generally increase the utility of the method for difficult cases.« less

PyXRD v0.6.7: a free and open-source program to quantify disordered phyllosilicates using multi-specimen X-ray diffraction profile fitting

NASA Astrophysics Data System (ADS)

Dumon, M.; Van Ranst, E.

2016-01-01

This paper presents a free and open-source program called PyXRD (short for Python X-ray diffraction) to improve the quantification of complex, poly-phasic mixed-layer phyllosilicate assemblages. The validity of the program was checked by comparing its output with Sybilla v2.2.2, which shares the same mathematical formalism. The novelty of this program is the ab initio incorporation of the multi-specimen method, making it possible to share phases and (a selection of) their parameters across multiple specimens. PyXRD thus allows for modelling multiple specimens side by side, and this approach speeds up the manual refinement process significantly. To check the hypothesis that this multi-specimen set-up - as it effectively reduces the number of parameters and increases the number of observations - can also improve automatic parameter refinements, we calculated X-ray diffraction patterns for four theoretical mineral assemblages. These patterns were then used as input for one refinement employing the multi-specimen set-up and one employing the single-pattern set-ups. For all of the assemblages, PyXRD was able to reproduce or approximate the input parameters with the multi-specimen approach. Diverging solutions only occurred in single-pattern set-ups, which do not contain enough information to discern all minerals present (e.g. patterns of heated samples). Assuming a correct qualitative interpretation was made and a single pattern exists in which all phases are sufficiently discernible, the obtained results indicate a good quantification can often be obtained with just that pattern. However, these results from theoretical experiments cannot automatically be extrapolated to all real-life experiments. In any case, PyXRD has proven to be useful when X-ray diffraction patterns are modelled for complex mineral assemblages containing mixed-layer phyllosilicates with a multi-specimen approach.

Processing of Lunar Soil Simulant for Space Exploration Applications

NASA Technical Reports Server (NTRS)

Sen, Subhayu; Ray, Chandra S.; Reddy, Ramana

2005-01-01

NASA's long-term vision for space exploration includes developing human habitats and conducting scientific investigations on planetary bodies, especially on Moon and Mars. To reduce the level of up-mass processing and utilization of planetary in-situ resources is recognized as an important element of this vision. Within this scope and context, we have undertaken a general effort aimed primarily at extracting and refining metals, developing glass, glass-ceramic, or traditional ceramic type materials using lunar soil simulants. In this paper we will present preliminary results on our effort on carbothermal reduction of oxides for elemental extraction and zone refining for obtaining high purity metals. In additions we will demonstrate the possibility of developing glasses from lunar soil simulant for fixing nuclear waste from potential nuclear power generators on planetary bodies. Compositional analysis, x-ray diffraction patterns and differential thermal analysis of processed samples will be presented.

Broad-Band Measurements of Cen X-3 With XTE and CGRO

NASA Technical Reports Server (NTRS)

Vestrand, W. Thomas

1999-01-01

Centaurus X-3 has played a key role in the development of our understanding of galactic x-ray binary sources. Timing analysis of the UHURU x-ray observations for the luminous Cen X-3 source (L approximately 10(exp 38) erg/s) revealed the first evidence for coherent x-ray pulsations from an object in a binary system (Giaconni 1971; Schreier 1972). It was quickly understood that the luminous pulsed x-ray emission could be generated by the accretion of matter from a companion star onto a rotating neutron star and led to the adoption of binary star models as the fundamental model for galactic x-ray sources (e.g. Pringle and Rees 1972; Lamb 1973). Based on modeling and refined observations since the original measurements, we now believe that Cen X-3 is a high mass x-ray binary system that contains a disk-fed pulsar with a period of 4.84 seconds that is in a 2.087 day orbit around an O-star companion. Since the pulsar discovery, its period has been intermittently monitored and those studies show a long term spin-up of the pulsar punctuated by short intervals of spin-down (e.g. Finger 1994). The implied torques are thought to originate from the interaction of an accretion disk with the magnetic field of a neutron star (Ghosh and Lamb 1979).

On the release of cppxfel for processing X-ray free-electron laser images.

PubMed

Ginn, Helen Mary; Evans, Gwyndaf; Sauter, Nicholas K; Stuart, David Ian

2016-06-01

As serial femtosecond crystallography expands towards a variety of delivery methods, including chip-based methods, and smaller collected data sets, the requirement to optimize the data analysis to produce maximum structure quality is becoming increasingly pressing. Here cppxfel , a software package primarily written in C++, which showcases several data analysis techniques, is released. This software package presently indexes images using DIALS (diffraction integration for advanced light sources) and performs an initial orientation matrix refinement, followed by post-refinement of individual images against a reference data set. Cppxfel is released with the hope that the unique and useful elements of this package can be repurposed for existing software packages. However, as released, it produces high-quality crystal structures and is therefore likely to be also useful to experienced users of X-ray free-electron laser (XFEL) software who wish to maximize the information extracted from a limited number of XFEL images.

On the release of cppxfel for processing X-ray free-electron laser images

DOE PAGES

Ginn, Helen Mary; Evans, Gwyndaf; Sauter, Nicholas K.; ...

2016-05-11

As serial femtosecond crystallography expands towards a variety of delivery methods, including chip-based methods, and smaller collected data sets, the requirement to optimize the data analysis to produce maximum structure quality is becoming increasingly pressing. Herecppxfel, a software package primarily written in C++, which showcases several data analysis techniques, is released. This software package presently indexes images using DIALS (diffraction integration for advanced light sources) and performs an initial orientation matrix refinement, followed by post-refinement of individual images against a reference data set.Cppxfelis released with the hope that the unique and useful elements of this package can be repurposed formore » existing software packages. However, as released, it produces high-quality crystal structures and is therefore likely to be also useful to experienced users of X-ray free-electron laser (XFEL) software who wish to maximize the information extracted from a limited number of XFEL images.« less

Neutron and X-ray total scattering study of hydrogen disorder in fully hydrated hydrogrossular, Ca3Al2(O4H4)3

NASA Astrophysics Data System (ADS)

Keen, David A.; Keeble, Dean S.; Bennett, Thomas D.

2018-04-01

The structure of fully hydrated grossular, or katoite, contains an unusual arrangement of four O-H bonds within each O4 tetrahedra. Neutron and X-ray total scattering from a powdered deuterated sample have been measured to investigate the local arrangement of this O4D4 cluster. The O-D bond length determined directly from the pair distribution function is 0.954 Å, although the Rietveld-refined distance between average O and D positions was slightly smaller. Reverse Monte Carlo refinement of supercell models to the total scattering data show that other than the consequences of this correctly determined O-D bond length, there is little to suggest that the O4D4 structure is locally significantly different from that expected based on the average structure determined solely from Bragg diffraction.

Enhancement in electrical and magnetic properties with Ti-doping in Bi0.5La0.5Fe0.5Mn0.5O3

NASA Astrophysics Data System (ADS)

Singh, Rahul; Gupta, Prince Kumar; Kumar, Shiv; Joshi, Amish G.; Ghosh, A. K.; Patil, S.; Chatterjee, Sandip

2017-04-01

In this investigation, we have synthesized Bi0.5La0.5Fe0.5Mn0.5-xTixO3 (where x = 0 and 0.05) samples. The Rietveld refinement of X-ray diffraction (XRD) patterns shows that the systems crystallize in the orthorhombic phase with the Pnma space group. The observed Raman modes support the XRD results. The appearance of prominent A1-3 and weak E-2 modes in Bi0.5La0.5Fe0.5Mn0.45Ti0.05O3 indicates the presence of chemically more active Bi-O covalent bonds. Ferromagnetism of Bi0.5La0.5Fe0.5Mn0.5O3 is enhanced by Ti doping at the Mn-site, indicating that these particular samples might be interesting for device applications.

21 CFR 1020.40 - Cabinet x-ray systems.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Cabinet x-ray systems. 1020.40 Section 1020.40...) RADIOLOGICAL HEALTH PERFORMANCE STANDARDS FOR IONIZING RADIATION EMITTING PRODUCTS § 1020.40 Cabinet x-ray systems. (a) Applicability. The provisions of this section are applicable to cabinet x-ray systems...

21 CFR 1020.40 - Cabinet x-ray systems.

Code of Federal Regulations, 2012 CFR

2012-04-01

... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Cabinet x-ray systems. 1020.40 Section 1020.40...) RADIOLOGICAL HEALTH PERFORMANCE STANDARDS FOR IONIZING RADIATION EMITTING PRODUCTS § 1020.40 Cabinet x-ray systems. (a) Applicability. The provisions of this section are applicable to cabinet x-ray systems...

21 CFR 1020.40 - Cabinet x-ray systems.

Code of Federal Regulations, 2013 CFR

2013-04-01

... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Cabinet x-ray systems. 1020.40 Section 1020.40...) RADIOLOGICAL HEALTH PERFORMANCE STANDARDS FOR IONIZING RADIATION EMITTING PRODUCTS § 1020.40 Cabinet x-ray systems. (a) Applicability. The provisions of this section are applicable to cabinet x-ray systems...

Flexible digital x-ray technology for far-forward remote diagnostic and conformal x-ray imaging applications

NASA Astrophysics Data System (ADS)

Smith, Joseph; Marrs, Michael; Strnad, Mark; Apte, Raj B.; Bert, Julie; Allee, David; Colaneri, Nicholas; Forsythe, Eric; Morton, David

2013-05-01

Today's flat panel digital x-ray image sensors, which have been in production since the mid-1990s, are produced exclusively on glass substrates. While acceptable for use in a hospital or doctor's office, conventional glass substrate digital x-ray sensors are too fragile for use outside these controlled environments without extensive reinforcement. Reinforcement, however, significantly increases weight, bulk, and cost, making them impractical for far-forward remote diagnostic applications, which demand rugged and lightweight x-ray detectors. Additionally, glass substrate x-ray detectors are inherently rigid. This limits their use in curved or bendable, conformal x-ray imaging applications such as the non-destructive testing (NDT) of oil pipelines. However, by extending low-temperature thin-film transistor (TFT) technology previously demonstrated on plastic substrate- based electrophoretic and organic light emitting diode (OLED) flexible displays, it is now possible to manufacture durable, lightweight, as well as flexible digital x-ray detectors. In this paper, we discuss the principal technical approaches used to apply flexible display technology to two new large-area flexible digital x-ray sensors for defense, security, and industrial applications and demonstrate their imaging capabilities. Our results include a 4.8″ diagonal, 353 x 463 resolution, flexible digital x-ray detector, fabricated on a 6″ polyethylene naphthalate (PEN) plastic substrate; and a larger, 7.9″ diagonal, 720 x 640 resolution, flexible digital x-ray detector also fabricated on PEN and manufactured on a gen 2 (370 x 470 mm) substrate.

X-ray K-edge absorption spectra of Fe minerals and model compounds: II. EXAFS

NASA Astrophysics Data System (ADS)

Waychunas, Glenn A.; Brown, Gordon E.; Apted, Michael J.

1986-01-01

K-edge extended X-ray absorption fine structure (EXAFS) spectra of Fe in varying environments in a suite of well-characterized silicate and oxide minerals were collected using synchrotron radiation and analyzed using single scattering approximation theory to yield nearest neighbor Fe-O distances and coordination numbers. The partial inverse character of synthetic hercynite spinal was verified in this way. Comparison of the results from all samples with structural data from X-ray diffraction crystal structure refinements indicates that EXAFS-derived first neighbor distances are generally accurate to ±0.02 Å using only theoretically generated phase information, and may be improved over this if similar model compounds are used to determine EXAFS phase functions. Coordination numbers are accurate to ±20 percent and can be similarly improved using model compound EXAFS amplitude information. However, in particular cases the EXAFS-derived distances may be shortened, and the coordination number reduced, by the effects of static and thermal disorder or by partial overlap of the longer Fe-O first neighbor distances with second neighbor distances in the EXAFS structure function. In the former case the total information available in the EXAFS is limited by the disorder, while in the latter case more accurate results can in principle be obtained by multiple neighbor EXAFS analysis. The EXAFS and XANES spectra of Fe in Nain, Labrador osumulite and Lakeview, Oregon plagioclase are also analyzed as an example of the application of X-ray absorption spectroscopy to metal ion site occupation determination in minerals.

On Calibrations Using the Crab Nebula as a Standard Candle

NASA Technical Reports Server (NTRS)

Weisskopf, Martin; Guainazzi, Matteo; Jahoda, Keith; Shaposhnikov, Nikolai; ODell, Stephen; Zavlin, Vyacheslav; Wilson-Hodge, Colleen; Elsner, Ronald

2009-01-01

Inspired by a recent paper (Kirsch et al. 2005) on possible use of the Crab Nebula as a standard candle for calibrating X-ray response func tions, we examine possible consequences of intrinsic departures from a single (absorbed) power law upon such calibrations. We limited our analyses to three more modern X-ray instruments -- the ROSAT/PSPC, th e RXTE/PCA, and the XMM-Newton/EPIC-pn. The results are unexpected an d indicate a need to refine two of the three response functions studi ed. The implications for Chandra will be discussed.

X-Ray Wind Tomography of IGR J17252-3616

NASA Astrophysics Data System (ADS)

Manousakis, Antonios; Walter, Roland

2010-07-01

IGR J17252-3616, a highly absorbed High Mass X-ray Binary (HMXB) with Hydrogen column density NH~(2-4)×1023 cm-2, has been observed with XMM-Newton for about one month. Observations were scheduled in order to cover the orbital-phase space as much as possible. IGR J17252-3616 shows a varying column density NH and Fe Kα line when fit with simple phenomenological models. A refined orbital solution can be derived. Spectral timing analysis allows derivation of the wind properties of the massive star.

Industrial applications of automated X-ray inspection

NASA Astrophysics Data System (ADS)

Shashishekhar, N.

2015-03-01

Many industries require that 100% of manufactured parts be X-ray inspected. Factors such as high production rates, focus on inspection quality, operator fatigue and inspection cost reduction translate to an increasing need for automating the inspection process. Automated X-ray inspection involves the use of image processing algorithms and computer software for analysis and interpretation of X-ray images. This paper presents industrial applications and illustrative case studies of automated X-ray inspection in areas such as automotive castings, fuel plates, air-bag inflators and tires. It is usually necessary to employ application-specific automated inspection strategies and techniques, since each application has unique characteristics and interpretation requirements.

First centenary of Röntgen's discovery of X-rays

NASA Astrophysics Data System (ADS)

Valkovic, V.

1996-04-01

Usually it takes a decade or even several decades, from a discovery to its practical applications. This was not the case with X-rays; they were widely applied in medical and industrial radiography within a year of their discovery in 1895 by W.C. Röntgen. Today, X-ray analysis covers a wide range of techniques and fields of applications: from deduction of atomic arrangements by observation of diffraction phenomena to measurements of trace element concentration levels, distributions and maps by measuring fluorescence, X-ray attenuation or scattering. Although the contribution of analytical applications of X-rays to the present knowledge is difficult to surpass, modern application cover a wide range of activities from three-dimensional microfabrication using synchroton radiation to collecting information from the deep space by X-ray astronomy.

Changes in the chemical composition and spectroscopy of loblolly pine medium density fiberboard furnish as a function of age and refining pressure

Treesearch

Stephen S. Kelley; Thomas Elder; Leslie H. Groom

2005-01-01

Loblolly pine wood between the ages of 5-35 was refined into medium density fiberboard furnish at steam pressures from 2 to 18 bar, The effect of age and processing conditions on the properties of the fibers was assessed by wet chemical analyses, Near Infared Spectroscopy (NIR) and powder X-ray diffraction (XRD).In general ,the percentages of extractives and glucose...

[Can the local energy minimization refine the PDB structures of different resolution universally?].

PubMed

Godzi, M G; Gromova, A P; Oferkin, I V; Mironov, P V

2009-01-01

The local energy minimization was statistically validated as the refinement strategy for PDB structure pairs of different resolution. Thirteen pairs of structures with the only difference in resolution were extracted from PDB, and the structures of 11 identical proteins obtained by different X-ray diffraction techniques were represented. The distribution of RMSD value was calculated for these pairs before and after the local energy minimization of each structure. The MMFF94 field was used for energy calculations, and the quasi-Newton method was used for local energy minimization. By comparison of these two RMSD distributions, the local energy minimization was proved to statistically increase the structural differences in pairs so that it cannot be used for refinement purposes. To explore the prospects of complex refinement strategies based on energy minimization, randomized structures were obtained by moving the initial PDB structures as far as the minimized structures had been moved in a multidimensional space of atomic coordinates. For these randomized structures, the RMSD distribution was calculated and compared with that for minimized structures. The significant differences in their mean values proved the energy surface of the protein to have only few minima near the conformations of different resolution obtained by X-ray diffraction for PDB. Some other results obtained by exploring the energy surface near these conformations are also presented. These results are expected to be very useful for the development of new protein refinement strategies based on energy minimization.

From the X-rays to a reliable “low cost” computational structure of caffeic acid: DFT, MP2, HF and integrated molecular dynamics-X-ray diffraction approach to condensed phases

NASA Astrophysics Data System (ADS)

Lombardo, Giuseppe M.; Portalone, Gustavo; Colapietro, Marcello; Rescifina, Antonio; Punzo, Francesco

2011-05-01

The ability of caffeic acid to act as antioxidant against hyperoxo-radicals as well as its recently found therapeutic properties in the treatment of hepatocarcinoma, still make this compound, more than 20 years later the refinement of its crystal structure, object of study. It belongs to the vast family of humic substances, which play a key role in the biodegradation processes and easily form complexes with ions widely diffused in the environment. This class of compounds is therefore interesting for potential environmental chemistry applications concerning the possible complexation of heavy metals. Our study focused on the characterization of caffeic acid as a starting necessary step, which will be followed in the future by the application of our findings on the study of the properties of caffeate anion interaction with heavy metal ions. To reach this goal, we applied a low cost approach - in terms of computational time and resources - aimed at the achievement of a high resolution, robust and trustable structure using the X-ray single crystal data, recollected with a higher resolution, as touchstone for a detailed check. A comparison between the calculations carried out with density functional theory (DFT), Hartree-Fock (HF) method and post SCF second order Møller-Plesset perturbation method (MP2), at the 6-31G ** level of the theory, molecular mechanics (MM) and molecular dynamics (MD) was performed. As a consequence we explained on one hand the possible reasons for the pitfalls of the DFT approach and on the other the benefits of using a good and robust force field developed for condensed phases, as AMBER, with MM and MD. The reliability of the latter, highlighted by the overall agreement extended up to the anisotropic displacement parameters calculated by means of MD and the ones gathered by X-ray measurements, makes it very promising for the above-mentioned goals.

Generation Mechanisms UV and X-ray Emissions During SL9 Impact

NASA Technical Reports Server (NTRS)

Waite, J. Hunter, Jr.

1997-01-01

The purpose of this grant was to study the ultraviolet and X-ray emissions associated with the impact of comet Shoemaker-Levy 9 with Jupiter. The University of Michigan task was primarily focused on theoretical calculations. The NAGW-4788 subtask was to be largely devoted to determining the constraints placed by the X-ray observations on the physical mechanisms responsible for the generation of the X-rays. Author summarized below the ROSAT observations and suggest a physical mechanism that can plausibly account for the observed emissions. It is hoped that the full set of activities can be completed at a later date. Further analysis of the ROSAT data acquired at the time of the impact was necessary to define the observational constraints on the magnetospheric-ionospheric processes involved in the excitation of the X-ray emissions associated with the fragment impacts. This analysis centered around improvements in the pointing accuracy and improvements in the timing information. Additional pointing information was made possible by the identification of the optical counterparts to the X-ray sources in the ROSAT field-of-view. Due to the large number of worldwide observers of the impacts, a serendipitous visible plate image from an observer in Venezuela provided a very accurate location of the present position of the X-ray source, virtually eliminating pointing errors in the data. Once refined, the pointing indicated that the two observed X-ray brightenings that were highly correlated in time with the K and P2 events were brightenings of the X-ray aurora (as identified in images prior to the impact).Appendix A "ROSAT observations of X-ray emissions from Jupiter during the impact of comet Shoemaker-Levy 9' also included.

X-ray comb generation from nuclear-resonance-stabilized x-ray free-electron laser oscillator for fundamental physics and precision metrology

DOE PAGES

Adams, B.  W.; Kim, K. -J.

2015-03-31

An x-ray free-electron laser oscillator (XFELO) is a next-generation x-ray source, similar to free-electron laser oscillators at VUV and longer wavelengths but using crystals as high-reflectivity x-ray mirrors. Each output pulse from an XFELO is fully coherent with high spectral purity. The temporal coherence length can further be increased drastically, from picoseconds to microseconds or even longer, by phase-locking successive XFELO output pulses, using the narrow nuclear resonance lines of nuclei such as ⁵⁷Fe as a reference. We show that the phase fluctuation due to the seismic activities is controllable and that due to spontaneous emission is small. The fluctuationmore » of electron-bunch spacing contributes mainly to the envelope fluctuation but not to the phase fluctuation. By counting the number of standing-wave maxima formed by the output of the nuclear-resonance-stabilized (NRS) XFELO over an optically known length, the wavelength of the nuclear resonance can be accurately measured, possibly leading to a new length or frequency standard at x-ray wavelengths. A NRS-XFELO will be an ideal source for experimental x-ray quantum optics as well as other fundamental physics. The technique can be refined for other, narrower resonances such as ¹⁸¹Ta or ⁴⁵Sc.« less

Evaluation of partial coherence correction in X-ray ptychography

DOE PAGES

Burdet, Nicolas; Shi, Xiaowen; Parks, Daniel; ...

2015-02-23

Coherent X-ray Diffraction Imaging (CDI) and X-ray ptychography both heavily rely on the high degree of spatial coherence of the X-ray illumination for sufficient experimental data quality for reconstruction convergence. Nevertheless, the majority of the available synchrotron undulator sources have a limited degree of partial coherence, leading to reduced data quality and a lower speckle contrast in the coherent diffraction patterns. It is still an open question whether experimentalists should compromise the coherence properties of an X-ray source in exchange for a higher flux density at a sample, especially when some materials of scientific interest are relatively weak scatterers. Amore » previous study has suggested that in CDI, the best strategy for the study of strong phase objects is to maintain a high degree of coherence of the illuminating X-rays because of the broadening of solution space resulting from the strong phase structures. In this article, we demonstrate the first systematic analysis of the effectiveness of partial coherence correction in ptychography as a function of the coherence properties, degree of complexity of illumination (degree of phase diversity of the probe) and sample phase complexity. We have also performed analysis of how well ptychographic algorithms refine X-ray probe and complex coherence functions when those variables are unknown at the start of reconstructions, for noise-free simulated data, in the case of both real-valued and highly-complex objects.« less

Methods for coherent lensless imaging and X-ray wavefront measurements

NASA Astrophysics Data System (ADS)

Guizar Sicairos, Manuel

X-ray diffractive imaging is set apart from other high-resolution imaging techniques (e.g. scanning electron or atomic force microscopy) for its high penetration depth, which enables tomographic 3D imaging of thick samples and buried structures. Furthermore, using short x-ray pulses, it enables the capability to take ultrafast snapshots, giving a unique opportunity to probe nanoscale dynamics at femtosecond time scales. In this thesis we present improvements to phase retrieval algorithms, assess their performance through numerical simulations, and develop new methods for both imaging and wavefront measurement. Building on the original work by Faulkner and Rodenburg, we developed an improved reconstruction algorithm for phase retrieval with transverse translations of the object relative to the illumination beam. Based on gradient-based nonlinear optimization, this algorithm is capable of estimating the object, and at the same time refining the initial knowledge of the incident illumination and the object translations. The advantages of this algorithm over the original iterative transform approach are shown through numerical simulations. Phase retrieval has already shown substantial success in wavefront sensing at optical wavelengths. Although in principle the algorithms can be used at any wavelength, in practice the focus-diversity mechanism that makes optical phase retrieval robust is not practical to implement for x-rays. In this thesis we also describe the novel application of phase retrieval with transverse translations to the problem of x-ray wavefront sensing. This approach allows the characterization of the complex-valued x-ray field in-situ and at-wavelength and has several practical and algorithmic advantages over conventional focused beam measurement techniques. A few of these advantages include improved robustness through diverse measurements, reconstruction from far-field intensity measurements only, and significant relaxation of experimental requirements over other beam characterization approaches. Furthermore, we show that a one-dimensional version of this technique can be used to characterize an x-ray line focus produced by a cylindrical focusing element. We provide experimental demonstrations of the latter at hard x-ray wavelengths, where we have characterized the beams focused by a kinoform lens and an elliptical mirror. In both experiments the reconstructions exhibited good agreement with independent measurements, and in the latter a small mirror misalignment was inferred from the phase retrieval reconstruction. These experiments pave the way for the application of robust phase retrieval algorithms for in-situ alignment and performance characterization of x-ray optics for nanofocusing. We also present a study on how transverse translations help with the well-known uniqueness problem of one-dimensional phase retrieval. We also present a novel method for x-ray holography that is capable of reconstructing an image using an off-axis extended reference in a non-iterative computation, greatly generalizing an earlier approach by Podorov et al. The approach, based on the numerical application of derivatives on the field autocorrelation, was developed from first mathematical principles. We conducted a thorough theoretical study to develop technical and intuitive understanding of this technique and derived sufficient separation conditions required for an artifact-free reconstruction. We studied the effects of missing information in the Fourier domain, and of an imperfect reference, and we provide a signal-to-noise ratio comparison with the more traditional approach of Fourier transform holography. We demonstrated this new holographic approach through proof-of-principle optical experiments and later experimentally at soft x-ray wavelengths, where we compared its performance to Fourier transform holography, iterative phase retrieval and state-of-the-art zone-plate x-ray imaging techniques (scanning and full-field). Finally, we present a demonstration of the technique using a single 20 fs pulse from a high-harmonic table-top source. Holography with an extended reference is shown to provide fast, good quality images that are robust to noise and artifacts that arise from missing information due to a beam stop. (Abstract shortened by UMI.)

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.

Effect of cobalt doping on structural and optical properties of nanocrystalline La0.8Pb0.2CrO3 orthochromite

NASA Astrophysics Data System (ADS)

Zarrin, Naima; Shahidhusain

2018-04-01

We have synthesized nanocrystalline La0.8Pb0.2Cr1-xCoxO3 (0≤x≤0.3) through sol-gel process and studied their structural and optical properties. X-ray diffraction patterns reveal that the samples conform in the orthorhombic crystal symmetry with Pnma space group. Structural parameters are refined by Rietveld Refinement using Fullprof software. Lattice parameters and unit cell volume of doped samples are found to decrease with increase in Co doping. The optical energy band gapdecreases whereas Urbach energy increases with the increase in Co content.

Raman effect, structural and dielectric properties of sol-gel synthesized polycrystalline GaFe{sub 1-x}Zr{sub x}O{sub 3} (0≤x≤0.15)

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

Kumar, Rajeev, E-mail: rajeevgiitk@gmail.com; Mall, Ashish Kumar; Gupta, Rajeev

2016-05-23

Polycrystalline ceramic samples of Zirconium (Zr)-doped GaFeO{sub 3} (GaFe{sub 1-x}Zr{sub x}O{sub 3}) were studied using powder X-ray diffraction, complex impedance spectroscopy and Raman spectroscopic measurements to understand the effect of Zr doping on the structural and dielectric properties. The samples with varying Zr content were prepared by Sol-Gel method. X-ray data analysis confirmed the formation of single phase material without formation of any secondary phases and all are crystallized in Pc2{sub 1}n orthorhombic symmetry. Rietveld refinement of the X-ray data suggested an increase in the lattice constants due to size effect and decreases on x = 0.15 due to themore » effect of change in interplanner spacing. Impedance studies on the samples showed that the dielectric constant increases while loss tangent decrease as the Zr content increases. Raman scattering on GaFe{sub 1-x}Zr{sub x}O{sub 3} (x = 0, 0.05, 0.10, & 0.15) used to understand the composition dependence on phonon modes at room temperature. On Zr doping, Raman modes frequencies shifts to lower energies consistent with the X-ray data.« less

Structure refinement of Zn and Pr-doped Y-Ba-Cu-oxides

NASA Astrophysics Data System (ADS)

Naik, M. S.; Sarode, P. R.; Priolkar, K. R.; Prabhu, R. B.

2018-05-01

Superconducting compounds of composition Y0.9 Pr0.1Ba2 [Cu1-yZny]3O7-δ (0 ≤ y ≤ 0.10) have been synthesized. The structure of these materials has been studied using powder X-ray diffraction technique and refinement has been carried out by using Rietveld refinement procedure. It has been shown that all these compounds crystallize in orthorhombic structure with slight change in c parameter. Increase of parameter O(2) and decrease of parameter O(3)suggest the changes in the Cu-O2 plane of these orthorhombic materials on Zn substitution.

Probing the accuracy and precision of Hirshfeld atom refinement with HARt interfaced with Olex2

PubMed Central

Fugel, Malte; Hathwar, Venkatesha R.; Turner, Michael J.; Howard, Judith A. K.

2018-01-01

Hirshfeld atom refinement (HAR) is a novel X-ray structure refinement technique that employs aspherical atomic scattering factors obtained from stockholder partitioning of a theoretically determined tailor-made static electron density. HAR overcomes many of the known limitations of independent atom modelling (IAM), such as too short element–hydrogen distances, r(X—H), or too large atomic displacement parameters (ADPs). This study probes the accuracy and precision of anisotropic hydrogen and non-hydrogen ADPs and of r(X—H) values obtained from HAR. These quantities are compared and found to agree with those obtained from (i) accurate neutron diffraction data measured at the same temperatures as the X-ray data and (ii) multipole modelling (MM), an established alternative method for interpreting X-ray diffraction data with the help of aspherical atomic scattering factors. Results are presented for three chemically different systems: the aromatic hydro­carbon rubrene (orthorhombic 5,6,11,12-tetra­phenyl­tetracene), a co-crystal of zwitterionic betaine, imidazolium cations and picrate anions (BIPa), and the salt potassium hydrogen oxalate (KHOx). The non-hydrogen HAR-ADPs are as accurate and precise as the MM-ADPs. Both show excellent agreement with the neutron-based values and are superior to IAM-ADPs. The anisotropic hydrogen HAR-ADPs show a somewhat larger deviation from neutron-based values than the hydrogen SHADE-ADPs used in MM. Element–hydrogen bond lengths from HAR are in excellent agreement with those obtained from neutron diffraction experiments, although they are somewhat less precise. The residual density contour maps after HAR show fewer features than those after MM. Calculating the static electron density with the def2-TZVP basis set instead of the simpler def2-SVP one does not improve the refinement results significantly. All HARs were performed within the recently introduced HARt option implemented in the Olex2 program. They are easily launched inside its graphical user interface following a conventional IAM. PMID:29354269

Crystal structure and europium luminescence of NaMgH3-xFx

NASA Astrophysics Data System (ADS)

Pflug, Christian; Franz, Alexandra; Kohlmann, Holger

2018-02-01

The solid solution series NaMgH3-xFx (x = 0, 0.5, 1, 1.5, 2, 2.5, 3) was synthesized by solid-state reactions under hydrogen gas pressure from binary ionic hydrides, fluorides and magnesium. Rietveld refinement based on X-ray powder diffraction data revealed the GdFeO3-structure type for all compounds and a trend of lattice parameters according to Vegard's law. The anion distribution in NaMgD2F and NaMgD1.5F1.5 was found to be statistical by Rietveld refinement based on neutron powder diffraction data. Photoluminescence measurements on europium(II) substituted NaMgH3-xFx revealed a strong red shift of the emission wavelength (λem = 665 nm for NaMgH2F:Eu) in comparison to violet emitting NaMgF3:Eu.

Investigation of multiferroic behavior on flakes-like BiFeO{sub 3}

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

Sheikh, Javed R.; Gaikwad, Vishwajit M.; Acharya, Smita A., E-mail: saha275@yahoo.com

2016-05-23

In present work, multiferroic BiFeO{sub 3} was synthesized by hydrothermal route. The rhombohedral structure was confirmed X-ray diffraction pattern and data fitted with Reitveld refinement using Full-Prof software suite. SEM micrograph shows flake like morphology. Frequency and temperature dependence of dielectric constant and dielectric loss were studied and detected enhancement in dielectric constant. The magnetic measurement indicates antiferromagnetic nature of BFO. P-E curve shows ferroelectic hysteresis loop with remanent polarization (2Pr) 0.3518 µC/cm{sup 2}. The dielectric anomaly observed near T{sub N} can be assigned to magnetoelectric coupling which is useful in device application.

Hydrogen atoms in protein structures: high-resolution X-ray diffraction structure of the DFPase

PubMed Central

2013-01-01

Background Hydrogen atoms represent about half of the total number of atoms in proteins and are often involved in substrate recognition and catalysis. Unfortunately, X-ray protein crystallography at usual resolution fails to access directly their positioning, mainly because light atoms display weak contributions to diffraction. However, sub-Ångstrom diffraction data, careful modeling and a proper refinement strategy can allow the positioning of a significant part of hydrogen atoms. Results A comprehensive study on the X-ray structure of the diisopropyl-fluorophosphatase (DFPase) was performed, and the hydrogen atoms were modeled, including those of solvent molecules. This model was compared to the available neutron structure of DFPase, and differences in the protein and the active site solvation were noticed. Conclusions A further examination of the DFPase X-ray structure provides substantial evidence about the presence of an activated water molecule that may constitute an interesting piece of information as regard to the enzymatic hydrolysis mechanism. PMID:23915572

Ginga observations of the dipping low-mass X-ray binaries XB 1916-053 and EXO 1748-676

NASA Technical Reports Server (NTRS)

Smale, Alan P.; Mukai, Koji; Williams, O. R.; Jones, Mark H.; Corbet, Robin H. D.

1992-01-01

Ginga observations of XB 1916-053 and EXO 0748-676, low-mass X-ray binaries with pronounced dips of variable depth and duration in their X-ray light curves, are reported. Periodicity studies of XB-1916-053 show results consistent with those from previous Ginga observations, specifically, that the derived X-ray period is shorter than the optical period by about 1 percent. This problem is discussed, and a more refined model for the system is described. Three bursts were detected during the observation of XB 1916-053, the second of which occurred during a dip. Spectral analysis suggests that the second burst caused an almost instantaneous ionization of the absorbing medium in the line of sight. This material then returned to its equilibrium state on the same time scale as the burst decay. Loose limits are placed upon the possible clumpiness of the material responsible for the accretion disk structure in XB 1916-053 and EXO 0748-676.

Model-based Approaches for the Determination of Lipid Bilayer Structure from Small-Angle Neutron and X-ray Scattering Data

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

Heberle, Frederick A; Pan, Jianjun; Standaert, Robert F

2012-01-01

Some of our recent work has resulted in the detailed structures of fully hydrated, fluid phase phosphatidylcholine (PC) and phosphatidylglycerol (PG) bilayers. These structures were obtained from the joint refinement of small-angle neutron and X-ray data using the scattering density profile (SDP) models developed by Ku erka et al. (Ku erka et al. 2012; Ku erka et al. 2008). In this review, we first discuss models for the standalone analysis of neutron or X-ray scattering data from bilayers, and assess the strengths and weaknesses inherent in these models. In particular, it is recognized that standalone data do not contain enoughmore » information to fully resolve the structure of inherently disordered fluid bilayers, and therefore may not provide a robust determination of bilayer structural parameters, including the much sought after area per lipid. We then discuss the development of matter density-based models (including the SDP model) that allow for the joint refinement of different contrast neutron and X-ray data sets, as well as the implementation of local volume conservation in the unit cell (i.e., ideal packing). Such models provide natural definitions of bilayer thicknesses (most importantly the hydrophobic and Luzzati thicknesses) in terms of Gibbs dividing surfaces, and thus allow for the robust determination of lipid areas through equivalent slab relationships between bilayer thickness and lipid volume. In the final section of this review, we discuss some of the significant findings/features pertaining to structures of PC and PG bilayers as determined from SDP model analyses.« less

Digital model for X-ray diffraction with application to composition and strain determination in strained InAs/GaSb superlattices

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

Meng, Yifei; Kim, Honggyu; Zuo, Jian-Min

2014-07-07

We propose a digital model for high quality superlattices by including fluctuations in the superlattice periods. The composition and strain profiles are assumed to be coherent and persist throughout the superlattice. Using this model, we have significantly improved the fit with experimental X-ray diffraction data recorded from the nominal InAs/GaSb superlattice. The lattice spacing of individual layers inside the superlattice and the extent of interfacial intermixing are refined by including both (002) and (004) and their satellite peaks in the fitting. For the InAs/GaSb strained layer superlattice, results show: (i) the GaSb-on-InAs interface is chemically sharper than the InAs-on-GaSb interface,more » (ii) the GaSb layers experience compressive strain with In incorporation, (iii) there are interfacial strain associated with InSb-like bonds in GaSb and GaAs-like bonds in InAs, (iv) Sb substitutes a significant amount of In inside InAs layer near the InAs-on-GaSb interface. For support, we show that the composition profiles determined by X-ray diffraction are in good agreement with those obtained from atom probe tomography measurement. Comparison with the kinetic growth model shows a good agreement in terms of the composition profiles of anions, while the kinetic model underestimates the intermixing of cations.« less

Structural Mineral Physics at Extreme Conditions

NASA Astrophysics Data System (ADS)

Chariton, S.; Dubrovinsky, L. S.; Dubrovinskaia, N.

2017-12-01

Laser heating techniques in diamond anvil cells (DACs) cover a wide pressure-temperature range - above 300 GPa and up to 5000 K. Recent advantages in on-line laser heating techniques resulted in a significant improvement of reliability of in situ X-ray powder diffraction studies in laser-heated DACs, which have become routine at a number of synchrotron facilities including specialized beam-lines at the 3rd generation synchrotrons. However, until recently, existing DAC laser-heating systems could not be used for structural X-ray diffraction studies aimed at structural refinements, i.e. measuring of the diffraction intensities, and not only at determining of lattice parameters. The reason is that in existing DAC laser-heating facilities the laser beam enters the cell at a fixed angle, and a partial rotation of the DAC, as required in monochromatic structural X-ray diffraction experiments, results in a loss of the target crystal and may be even dangerous if the powerful laser light starts to scatter in arbitrary directions by the diamond anvils. In order to overcome this problem we have develop a portable laser heating system and implement it at different diffraction beam lines. We demonstrate the application of this system for simultaneous high-pressure and high-temperature powder and single crystal diffraction studies using examples of studies of chemical and phase relations in the Fe-O system, transition metals carbonates, and silicate perovskites.

Application of a Sub-set of Skinfold Sites for Ultrasound Measurement of Subcutaneous Adiposity and Percentage Body Fat Estimation in Athletes.

PubMed

O'Neill, D C; Cronin, O; O'Neill, S B; Woods, T; Keohane, D M; Molloy, M G; Falvey, E C

2016-05-01

Body composition assessment is an integral feature of elite sport as optimization facilitates successful performance. This study aims to refine the use of B-mode ultrasound in the assessment of athlete body composition by determining suitable sites for measurement. 67 elite athletes recruited from the Human Performance Laboratory, University College Cork, Ireland, underwent dual measurement of body composition. Subcutaneous adipose tissue thickness at 7 anatomical sites were measured using ultrasound and compared to percentage body fat values determined using Dual-Energy X-ray Absorptiometry. Multiple linear regressions were performed and an equation to predict percentage body fat was derived. The present study found subcutaneous adipose tissue depths at the triceps, biceps, anterior thigh and supraspinale sites correlated significantly with percentage body fat by X-ray absorptiometry (all p<0.05). Summation of the depths at these locations correlated strongly with percentage body fat by Dual-Energy X-ray Absorptiometry (R²=0.879). The triceps, biceps, anterior thigh and supraspinale sites are suitable anatomical landmarks for the estimation of %BF using B-mode ultrasound. Use of B-mode ultrasound in the assessment of athlete body composition confers many benefits including lack of ionising radiation and its potential to be used as a portable field tool. © Georg Thieme Verlag KG Stuttgart · New York.

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

Matthews, D.L.; Rosen, M.D.

One of the elusive dreams of laser physicists has been the development of an x-ray laser. After 25 years of waiting, the x-ray laser has at last entered the scientific scene, although those now in operation are still laboratory prototypes. They produce soft x rays down to about five nanometers. X-ray lasers retain the usual characteristics of their optical counterparts: a very tight beam, spatial and temporal coherence, and extreme brightness. Present x-ray lasers are nearly 100 times brighter that the next most powerful x-ray source in the world: the electron synchrotron. Although Lawrence Livermore National Laboratory (LLNL) is widelymore » known for its hard-x-ray laser program which has potential applications in the Strategic Defense Initiative, the soft x-ray lasers have no direct military applications. These lasers, and the scientific tools that result from their development, may one day have a place in the design and diagnosis of both laser fusion and hard x-ray lasers. The soft x-ray lasers now in operation at the LLNL have shown great promise but are still in the primitive state. Once x-ray lasers become reliable, efficient, and economical, they will have several important applications. Chief among them might be the creation of holograms of microscopic biological structures too small to be investigated with visible light. 5 figs.« less

Toward Improved Description of DNA Backbone: Revisiting Epsilon and Zeta Torsion Force Field Parameters

PubMed Central

Zgarbová, Marie; Luque, F. Javier; Šponer, Jiří; Cheatham, Thomas E.; Otyepka, Michal; Jurečka, Petr

2013-01-01

We present a refinement of the backbone torsion parameters ε and ζ of the Cornell et al. AMBER force field for DNA simulations. The new parameters, denoted as εζOL1, were derived from quantum-mechanical calculations with inclusion of conformation-dependent solvation effects according to the recently reported methodology (J. Chem. Theory Comput. 2012, 7(9), 2886-2902). The performance of the refined parameters was analyzed by means of extended molecular dynamics (MD) simulations for several representative systems. The results showed that the εζOL1 refinement improves the backbone description of B-DNA double helices and G-DNA stem. In B-DNA simulations, we observed an average increase of the helical twist and narrowing of the major groove, thus achieving better agreement with X-ray and solution NMR data. The balance between populations of BI and BII backbone substates was shifted towards the BII state, in better agreement with ensemble-refined solution experimental results. Furthermore, the refined parameters decreased the backbone RMS deviations in B-DNA MD simulations. In the antiparallel guanine quadruplex (G-DNA) the εζOL1 modification improved the description of non-canonical α/γ backbone substates, which were shown to be coupled to the ε/ζ torsion potential. Thus, the refinement is suggested as a possible alternative to the current ε/ζ torsion potential, which may enable more accurate modeling of nucleic acids. However, long-term testing is recommended before its routine application in DNA simulations. PMID:24058302

The X-ray halo of an extremely luminous LSB disk galaxy

NASA Technical Reports Server (NTRS)

Weiner, Benjamin J.

2004-01-01

We are continuing to refine our upper limit on emission from halo gas in Malin 2. The upper limit is, of course, below the detected flux, but is made more difficult to quantify by the disk and possible AGN sources. We are also exploring spectral and spatial-size constraints to help separate the sources of emission. On the theory side, more recent work on the X-ray halo luminosity from halo gas leftover from galaxy formation has lowered the prediction for disk galaxies (e.g. Toft et al. 2002, MNRAS, 335, 799). While our upper limit is well below the original prediction, refinements in model have moved the theoretical goalposts, so that the observation may be consistent with newer models. A recent theoretical development, which our observations of Malin 2 appear to support, is that a substantial amount of mass can be accreted onto galaxies without being heated at a virial shock. The previous standard theory was that gas accreting into a halo hits a virial shock and is heated to high temperatures, which could produce X-ray halos in massive galaxies. Recent models show that "smooth accretion" of matter bypasses the virial shocking (Murali e t al. 2002, ApJ, 571, 1; Birnboim & Dekel 2003, MNRAS, 345, 349). Additionally, new hydrodynamical simulations of galaxy mergers by UCSC graduate student T. J. Cox show that hot gas halos can be created by gas blown out from the merger, taking up orbital energy of the merging galaxies (Cox et al. 2004, ApJ, 607, L87). If mergers rather than virial shocking are the origin of hot gas halos, the existence of an X-ray halo should depend more on past merger activity than halo mass. Then it makes sense that elliptical galaxies and poor groups with ellipticals, which are probably formed in mergers, have X-ray gas halos; while a giant, quiescent LSB disk galaxy like Malin 2, which has never suffered a major merger, does not have an X-ray halo. While both the observational expectations and theoretical models have changed since we began this project, which has forced us to re-evaluate the goals, we are pressing forward to firm up the observations and put them in context of the current models for X-ray halos of massive galaxies.

Review of the applications of x-ray refraction and the x-ray waveguide phenomenon to estimation of film structures.

PubMed

Hayashi, Kouichi

2010-12-01

Based on our previous work, I review the applications of x-ray refraction and the x-ray waveguide phenomenon to organic and inorganic thin films in the present paper. Under grazing incidence conditions, observations of refracted x-rays and guided x-rays due to the x-ray waveguide phenomenon provide information about thin film structures, and thus have potential as alternative methods to x-ray reflectivity. To date, we have measured the spectra of the refracted x-rays and guided x-rays from end faces of thin films using white incident x-ray beams, and utilized them for the determination of film density and thickness. Some of this work is summarized in the present paper. At the end of this paper, I describe our recent achievement in this field, namely the in situ measurement of guided x-rays during the film degradation process due to strong synchrotron radiation damage. Moreover, I discuss the perspective of the present technique from the viewpoint of micro-characterization and real-time estimation of thin films.

Potential for Imaging Engineered Tissues with X-Ray Phase Contrast

PubMed Central

Appel, Alyssa; Anastasio, Mark A.

2011-01-01

As the field of tissue engineering advances, it is crucial to develop imaging methods capable of providing detailed three-dimensional information on tissue structure. X-ray imaging techniques based on phase-contrast (PC) have great potential for a number of biomedical applications due to their ability to provide information about soft tissue structure without exogenous contrast agents. X-ray PC techniques retain the excellent spatial resolution, tissue penetration, and calcified tissue contrast of conventional X-ray techniques while providing drastically improved imaging of soft tissue and biomaterials. This suggests that X-ray PC techniques are very promising for evaluation of engineered tissues. In this review, four different implementations of X-ray PC imaging are described and applications to tissues of relevance to tissue engineering reviewed. In addition, recent applications of X-ray PC to the evaluation of biomaterial scaffolds and engineered tissues are presented and areas for further development and application of these techniques are discussed. Imaging techniques based on X-ray PC have significant potential for improving our ability to image and characterize engineered tissues, and their continued development and optimization could have significant impact on the field of tissue engineering. PMID:21682604

An improved ring removal procedure for in-line x-ray phase contrast tomography

NASA Astrophysics Data System (ADS)

Massimi, Lorenzo; Brun, Francesco; Fratini, Michela; Bukreeva, Inna; Cedola, Alessia

2018-02-01

The suppression of ring artifacts in x-ray computed tomography (CT) is a required step in practical applications; it can be addressed by introducing refined digital low pass filters within the reconstruction process. However, these filters may introduce additional ringing artifacts when simultaneously imaging pure phase objects and elements having a non-negligible absorption coefficient. Ringing originates at sharp interfaces, due to the truncation of spatial high frequencies, and severely affects qualitative and quantitative analysis of the reconstructed slices. In this work, we discuss the causes of ringing artifacts, and present a general compensation procedure to account for it. The proposed procedure has been tested with CT datasets of the mouse central nervous system acquired at different synchrotron radiation facilities. The results demonstrate that the proposed method compensates for ringing artifacts induced by low pass ring removal filters. The effectiveness of the ring suppression filters is not altered; the proposed method can thus be considered as a framework to improve the ring removal step, regardless of the specific filter adopted or the imaged sample.

An improved ring removal procedure for in-line x-ray phase contrast tomography.

PubMed

Massimi, Lorenzo; Brun, Francesco; Fratini, Michela; Bukreeva, Inna; Cedola, Alessia

2018-02-12

The suppression of ring artifacts in x-ray computed tomography (CT) is a required step in practical applications; it can be addressed by introducing refined digital low pass filters within the reconstruction process. However, these filters may introduce additional ringing artifacts when simultaneously imaging pure phase objects and elements having a non-negligible absorption coefficient. Ringing originates at sharp interfaces, due to the truncation of spatial high frequencies, and severely affects qualitative and quantitative analysis of the reconstructed slices. In this work, we discuss the causes of ringing artifacts, and present a general compensation procedure to account for it. The proposed procedure has been tested with CT datasets of the mouse central nervous system acquired at different synchrotron radiation facilities. The results demonstrate that the proposed method compensates for ringing artifacts induced by low pass ring removal filters. The effectiveness of the ring suppression filters is not altered; the proposed method can thus be considered as a framework to improve the ring removal step, regardless of the specific filter adopted or the imaged sample.

Use of a solar panel as a directionally sensitive large-area radiation monitor for direct and scattered x-rays and gamma-rays.

PubMed

Abdul-Majid, S

1987-01-01

The characteristics of a 25.4 X 91 cm solar cell panel used as an x-ray and gamma-ray radiation monitor are presented. Applications for monitoring the primary x-ray beam are described at different values of operating currents and voltages as well as for directional dependence of scattered radiation. Other applications in gamma-ray radiography are also given. The detector showed linear response to both x-ray and gamma-ray exposures. The equipment is rigid, easy to use, relatively inexpensive and requires no power supply or any complex electronic equipment.

Localizing intracavitary brachytherapy applicators from cone-beam CT x-ray projections via a novel iterative forward projection matching algorithm.

PubMed

Pokhrel, Damodar; Murphy, Martin J; Todor, Dorin A; Weiss, Elisabeth; Williamson, Jeffrey F

2011-02-01

To present a novel method for reconstructing the 3D pose (position and orientation) of radio-opaque applicators of known but arbitrary shape from a small set of 2D x-ray projections in support of intraoperative brachytherapy planning. The generalized iterative forward projection matching (gIFPM) algorithm finds the six degree-of-freedom pose of an arbitrary rigid object by minimizing the sum-of-squared-intensity differences (SSQD) between the computed and experimentally acquired autosegmented projection of the objects. Starting with an initial estimate of the object's pose, gIFPM iteratively refines the pose parameters (3D position and three Euler angles) until the SSQD converges. The object, here specialized to a Fletcher-Weeks intracavitary brachytherapy (ICB) applicator, is represented by a fine mesh of discrete points derived from complex combinatorial geometric models of the actual applicators. Three pairs of computed and measured projection images with known imaging geometry are used. Projection images of an intrauterine tandem and colpostats were acquired from an ACUITY cone-beam CT digital simulator. An image postprocessing step was performed to create blurred binary applicators only images. To quantify gIFPM accuracy, the reconstructed 3D pose of the applicator model was forward projected and overlaid with the measured images and empirically calculated the nearest-neighbor applicator positional difference for each image pair. In the numerical simulations, the tandem and colpostats positions (x,y,z) and orientations (alpha, beta, gamma) were estimated with accuracies of 0.6 mm and 2 degrees, respectively. For experimentally acquired images of actual applicators, the residual 2D registration error was less than 1.8 mm for each image pair, corresponding to about 1 mm positioning accuracy at isocenter, with a total computation time of less than 1.5 min on a 1 GHz processor. This work describes a novel, accurate, fast, and completely automatic method to localize radio-opaque applicators of arbitrary shape from measured 2D x-ray projections. The results demonstrate approximately 1 mm accuracy while compared against the measured applicator projections. No lateral film is needed. By localizing the applicator internal structure as well as radioactive sources, the effect of intra-applicator and interapplicator attenuation can be included in the resultant dose calculations. Further validation tests using clinically acquired tandem and colpostats images will be performed for the accurate and robust applicator/sources localization in ICB patients.

Localizing intracavitary brachytherapy applicators from cone-beam CT x-ray projections via a novel iterative forward projection matching algorithm

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

Pokhrel, Damodar; Murphy, Martin J.; Todor, Dorin A.

2011-02-15

Purpose: To present a novel method for reconstructing the 3D pose (position and orientation) of radio-opaque applicators of known but arbitrary shape from a small set of 2D x-ray projections in support of intraoperative brachytherapy planning. Methods: The generalized iterative forward projection matching (gIFPM) algorithm finds the six degree-of-freedom pose of an arbitrary rigid object by minimizing the sum-of-squared-intensity differences (SSQD) between the computed and experimentally acquired autosegmented projection of the objects. Starting with an initial estimate of the object's pose, gIFPM iteratively refines the pose parameters (3D position and three Euler angles) until the SSQD converges. The object, heremore » specialized to a Fletcher-Weeks intracavitary brachytherapy (ICB) applicator, is represented by a fine mesh of discrete points derived from complex combinatorial geometric models of the actual applicators. Three pairs of computed and measured projection images with known imaging geometry are used. Projection images of an intrauterine tandem and colpostats were acquired from an ACUITY cone-beam CT digital simulator. An image postprocessing step was performed to create blurred binary applicators only images. To quantify gIFPM accuracy, the reconstructed 3D pose of the applicator model was forward projected and overlaid with the measured images and empirically calculated the nearest-neighbor applicator positional difference for each image pair. Results: In the numerical simulations, the tandem and colpostats positions (x,y,z) and orientations ({alpha},{beta},{gamma}) were estimated with accuracies of 0.6 mm and 2 deg., respectively. For experimentally acquired images of actual applicators, the residual 2D registration error was less than 1.8 mm for each image pair, corresponding to about 1 mm positioning accuracy at isocenter, with a total computation time of less than 1.5 min on a 1 GHz processor. Conclusions: This work describes a novel, accurate, fast, and completely automatic method to localize radio-opaque applicators of arbitrary shape from measured 2D x-ray projections. The results demonstrate {approx}1 mm accuracy while compared against the measured applicator projections. No lateral film is needed. By localizing the applicator internal structure as well as radioactive sources, the effect of intra-applicator and interapplicator attenuation can be included in the resultant dose calculations. Further validation tests using clinically acquired tandem and colpostats images will be performed for the accurate and robust applicator/sources localization in ICB patients.« less

Relevance of 2D radiographic texture analysis for the assessment of 3D bone micro-architecture

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

Apostol, Lian; Boudousq, Vincent; Basset, Oliver

Although the diagnosis of osteoporosis is mainly based on dual x-ray absorptiometry, it has been shown that trabecular bone micro-architecture is also an important factor in regard to fracture risk. In vivo, techniques based on high-resolution x-ray radiography associated to texture analysis have been proposed to investigate bone micro-architecture, but their relevance for giving pertinent 3D information is unclear. Thirty-three calcaneus and femoral neck bone samples including the cortical shells (diameter: 14 mm, height: 30-40 mm) were imaged using 3D-synchrotron x-ray micro-CT at the ESRF. The 3D reconstructed images with a cubic voxel size of 15 {mu}m were further usedmore » for two purposes: (1) quantification of three-dimensional trabecular bone micro-architecture (2) simulation of realistic x-ray radiographs under different acquisition conditions. The simulated x-ray radiographs were then analyzed using a large variety of texture analysis methods (co-occurrence, spectral density, fractal, morphology, etc.). The range of micro-architecture parameters was in agreement with previous studies and rather large, suggesting that the population was representative. More than 350 texture parameters were tested. A small number of them were selected based on their correlation to micro-architectural morphometric parameters. Using this subset of texture parameters, multiple regression allowed one to predict up to 93% of the variance of micro-architecture parameters using three texture features. 2D texture features predicting 3D micro-architecture parameters other than BV/TV were identified. The methodology proposed for evaluating the relationships between 3D micro-architecture and 2D texture parameters may also be used for optimizing the conditions for radiographic imaging. Further work will include the application of the method to physical radiographs. In the future, this approach could be used in combination with DXA to refine osteoporosis diagnosis.« less

Diamond x-ray optics: Transparent, resilient, high-resolution, and wavefront preserving

DOE PAGES

Shvyd’ko, Yuri; Blank, Vladimir; Terentyev, Sergey

2017-06-09

Diamond features a unique combination of outstanding physical properties perfect for numerous x-ray optics applications, where traditional materials such as silicon fail to perform. In the last two decades, impressive progress has been achieved in synthesizing diamond with high crystalline perfection, in manufacturing efficient, resilient, high-resolution, wavefront-preserving diamond optical components, and in implementing them in cutting-edge x-ray instruments. Diamond optics are essential for tailoring x-rays to the most challenging needs of x-ray research. Furthermore, they are becoming vital for the generation of fully coherent hard x-rays by seeded x-ray free-electron lasers. In this article, we review progress in manufacturing flawlessmore » diamond crystal components and their applications in diverse x-ray optical devices, such as x-ray monochromators, beam splitters, high-reflectance backscattering mirrors, lenses, phase plates, diffraction gratings, bent-crystal spectrographs, and windows.« less

The 2.35 year itch of Cygnus OB2 #9. I. Optical and X-ray monitoring

NASA Astrophysics Data System (ADS)

Nazé, Y.; Mahy, L.; Damerdji, Y.; Kobulnicky, H. A.; Pittard, J. M.; Parkin, E. R.; Absil, O.; Blomme, R.

2012-10-01

Context. Nonthermal radio emission in massive stars is expected to arise in wind-wind collisions occurring inside a binary system. One such case, the O-type star Cyg OB2 #9, was proven to be a binary only four years ago, but the orbital parameters remained uncertain. The periastron passage of 2011 was the first one to be observable under good conditions since the discovery of binarity. Aims: In this context, we have organized a large monitoring campaign to refine the orbital solution and to study the wind-wind collision. Methods: This paper presents the analysis of optical spectroscopic data, as well as of a dedicated X-ray monitoring performed with Swift and XMM-Newton. Results: In light of our refined orbital solution, Cyg OB2 #9 appears as a massive O+O binary with a long period and high eccentricity; its components (O5-5.5I for the primary and O3-4III for the secondary) have similar masses and similar luminosities. The new data also provide the first evidence that a wind-wind collision is present in the system. In the optical domain, the broad Hα line varies, displaying enhanced absorption and emission components at periastron. X-ray observations yield the unambiguous signature of an adiabatic collision, because as the stars approach periastron, the X-ray luminosity closely follows the 1/D variation expected in that case. The X-ray spectrum appears, however, slightly softer at periastron, which is probably related to winds colliding at slightly lower speeds at that time. Conclusions: It is the first time that such a variation has been detected in O+O systems, and the first case where the wind-wind collision is found to remain adiabatic even at periastron passage. Based on observations collected at OHP, with Swift, and with XMM-Newton.Tables 1 and 2 are available in electronic form at http://www.aanda.org

Structural, Physical, and Compositional Analysis of Lunar Simulants and Regolith

NASA Technical Reports Server (NTRS)

Greenberg, Paul; Street, Kenneth W.; Gaier, James

2008-01-01

Relative to the prior manned Apollo and unmanned robotic missions, planned Lunar initiatives are comparatively complex and longer in duration. Individual crew rotations are envisioned to span several months, and various surface systems must function in the Lunar environment for periods of years. As a consequence, an increased understanding of the surface environment is required to engineer and test the associated materials, components, and systems necessary to sustain human habitation and surface operations. The effort described here concerns the analysis of existing simulant materials, with application to Lunar return samples. The interplay between these analyses fulfills the objective of ascertaining the critical properties of regolith itself, and the parallel objective of developing suitable stimulant materials for a variety of engineering applications. Presented here are measurements of the basic physical attributes, i.e. particle size distributions and general shape factors. Also discussed are structural and chemical properties, as determined through a variety of techniques, such as optical microscopy, SEM and TEM microscopy, Mossbauer Spectroscopy, X-ray diffraction, Raman microspectroscopy, inductively coupled argon plasma emission spectroscopy and energy dispersive X-ray fluorescence mapping. A comparative description of currently available stimulant materials is discussed, with implications for more detailed analyses, as well as the requirements for continued refinement of methods for simulant production.

Structural and mechanical properties of cardiolipin lipid bilayers determined using neutron spin echo, small angle neutron and X-ray scattering, and molecular dynamics simulations

DOE PAGES

Pan, Jianjun; Cheng, Xiaolin; Sharp, Melissa; ...

2014-10-29

We report that the detailed structural and mechanical properties of a tetraoleoyl cardiolipin (TOCL) bilayer were determined using neutron spin echo (NSE) spectroscopy, small angle neutron and X-ray scattering (SANS and SAXS, respectively), and molecular dynamics (MD) simulations. We used MD simulations to develop a scattering density profile (SDP) model, which was then utilized to jointly refine SANS and SAXS data. In addition to commonly reported lipid bilayer structural parameters, component distributions were obtained, including the volume probability, electron density and neutron scattering length density.

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

PubMed

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

2014-04-01

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

Hydrocarbon fingerprinting for application in forensic geology: Review with case studies

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

Bruce, L.G.; Schmidt, G.W.

1994-11-01

Forensic geology, the application of the science to the law, has required detailed classification, identification, and fingerprinting of hydrocarbons. Currently, the best overall tool for this is a chromatogram derived from capillary column gas chromatography (GC). Just as hardness and cleavage identify rock minerals and x-ray angles help identify clay minerals, retention time on a chromatogram can help identify key hydrocarbons, such as normal paraffins. N-paraffin ranges can be used to classify hydrocarbon mixtures such as gasoline, diesel fuel, or crude oil. Refined and crude petroleum may be distinguished on a chromatogram by the range of n-paraffins in a mixture,more » the shape of the n-paraffin envelope, the presence of absence of olefins, and the presence and relative abundance of certain hydrocarbon additives. Crude oils tend to have a wide range of n-paraffins whose envelope is asymmetric and includes a tail of heavier hydrocarbons. Refined products have a more limited n-paraffin range. With some notable exceptions, such as gasoline, the envelope of most refined products is bell shaped. Olefins are an artifact of the refining process and are not present in crudes. Methylcyclohexane is relatively abundant in gasolines. Isooctane and aromatics are more abundant in premium gasolines than in condensates and crudes. Fuel additives such as tetraethyl lead, methyl tertiary butyl ether, ethyl tertiary butyl alcohol, and ethanol do not exist in crudes. This paper uses case histories to illustrate fingerprinting techniques. Case one matches the fingerprint of a plume to a specific source. Case two eliminates casing-head condensate as the source of a plume and tags processed natural-gas liquids as the probable source. Case three illustrates how other organic compounds may be mistakenly identified as hydrocarbon contamination, and case four differentiates refined products.« less

Recent applications of hard x-ray photoelectron spectroscopy

DOE PAGES

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

2016-05-05

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

Generation of the Submicron Soft X-Ray Beam Using a Fresnel Zone Plate

NASA Astrophysics Data System (ADS)

Nishikino, M.; Kawazome, H.; Tanaka, M.; Kishimoto, M.; Hasegawa, N.; Ochi, Y.; Kawachi, T.; Sukegawa, K.; Yamatani, H.; Nagashima, K.; Kato, Y.

We have developed a fully coherent x-ray laser at 13.9 nm and the application research has been started. The generation of submicron x-ray beam is important for the application of high intensity x-ray beam, such as the non-linear optics, the material science, and the biology. The submicron x-ray bee am is generated by the soft x-ray laser with using a Fresnel zone plate. The spot diameter is estimated about 680 nm (290 nm at FWHM) by the theoretical calculation. In this experiment, the diameter of the x-ray beam is measured by the knife-edge scan. The diameter and the intensity are estimated 730 nm (310 nm at FWHM) and 3x1011 W/cm2, respectively.

X-Ray Detector for 1 to 30 keV

NASA Technical Reports Server (NTRS)

Alcorn, G.; Jackson, J., Jr; Grant, P.; Marshall, F.

1983-01-01

Array of silicon X-ray detecting diodes measures photon energy and provides image of X-ray pattern. Regardless of thickness of new X-ray detector, depletion region extends through it. Impinging X-rays generate electrons in quantities proportional to X-ray energy. X-ray detector is mated to chargecoupled-device array for image generation and processing. Useful in industrial part inspection, pulsed-plasma research and medical application.

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.

X-ray Diffraction and Rietveld Refinement in Deferrified Clays for Forensic Science.

PubMed

Prandel, Luis V; Melo, Vander de F; Brinatti, André M; Saab, Sérgio da C; Salvador, Fábio A S

2018-01-01

Soil vestiges might provide information about a crime scene. The Rietveld method with X-ray diffraction data (RM-XRD) is a nondestructive technique that makes it possible to characterize minerals present in the soils. Soil clays from the metropolitan region of Curitiba (Brazil) were submitted to DCB treatment and analyzed using XRD with CuK α radiation in the step-scan mode (0.02° 2θ/5 s). The GSAS+EXPGUI software was used for RM refinement. The RM-XRD results, together with the principal component analysis (PCA) (52.6% total variance), showed the kaolinite predominance in most analyzed samples and the highest quartz contents in "site 1." Higher anatase, and gibbsite and muscovite contents influenced discrimination, mainly in "site 3" and "site 1," respectively. These results were enough to discriminate clays of four sites and two horizons using a reduced amount of sample showing that the technique can be applied to the investigation into soil vestiges. © 2017 American Academy of Forensic Sciences.

Applications of phase-contrast x-ray imaging to medicine using an x-ray interferometer

NASA Astrophysics Data System (ADS)

Momose, Atsushi; Yoneyama, Akio; Takeda, Tohoru; Itai, Yuji; Tu, Jinhong; Hirano, Keiichi

1999-10-01

We are investigating possible medical applications of phase- contrast X-ray imaging using an X-ray interferometer. This paper introduces the strategy of the research project and the present status. The main subject is to broaden the observation area to enable in vivo observation. For this purpose, large X-ray interferometers were developed, and 2.5 cm X 1.5 cm interference patterns were generated using synchrotron X-rays. An improvement of the spatial resolution is also included in the project, and an X-ray interferometer designed for high-resolution phase-contrast X-ray imaging was fabricated and tested. In parallel with the instrumental developments, various soft tissues are observed by phase- contrast X-ray CT to find correspondence between the generated contrast and our histological knowledge. The observation done so far suggests that cancerous tissues are differentiated from normal tissues and that blood can produce phase contrast. Furthermore, this project includes exploring materials that modulate phase contrast for selective imaging.

X-ray free-electron laser oscillator with nuclear-resonant cavity stabilization and quantum-optical applications

DOE PAGES

Adams, Bernhard W.; Kim, Kwang -Je

2016-08-09

Here, x-ray free-electron-laser oscillators with nuclear-resonant cavity stabilization (NRS-XFELO) hold the promise for providing x-rays with unprecedented coherence properties that will enable interesting quantum-optical and metrological applications. Among these are atom optics with x-ray-based optical elements providing high momentum transfer, or a frequency standard far surpassing the best state-of the-art atomic clocks.

Compton backscattered collimated x-ray source

DOEpatents

Ruth, R.D.; Huang, Z.

1998-10-20

A high-intensity, inexpensive and collimated x-ray source is disclosed for applications such as x-ray lithography is disclosed. An intense pulse from a high power laser, stored in a high-finesse resonator, repetitively collides nearly head-on with and Compton backscatters off a bunched electron beam, having relatively low energy and circulating in a compact storage ring. Both the laser and the electron beams are tightly focused and matched at the interaction region inside the optical resonator. The laser-electron interaction not only gives rise to x-rays at the desired wavelength, but also cools and stabilizes the electrons against intrabeam scattering and Coulomb repulsion with each other in the storage ring. This cooling provides a compact, intense bunch of electrons suitable for many applications. In particular, a sufficient amount of x-rays can be generated by this device to make it an excellent and flexible Compton backscattered x-ray (CBX) source for high throughput x-ray lithography and many other applications. 4 figs.

Compton backscattered collimated x-ray source

DOEpatents

Ruth, Ronald D.; Huang, Zhirong

1998-01-01

A high-intensity, inexpensive and collimated x-ray source for applications such as x-ray lithography is disclosed. An intense pulse from a high power laser, stored in a high-finesse resonator, repetitively collides nearly head-on with and Compton backscatters off a bunched electron beam, having relatively low energy and circulating in a compact storage ring. Both the laser and the electron beams are tightly focused and matched at the interaction region inside the optical resonator. The laser-electron interaction not only gives rise to x-rays at the desired wavelength, but also cools and stabilizes the electrons against intrabeam scattering and Coulomb repulsion with each other in the storage ring. This cooling provides a compact, intense bunch of electrons suitable for many applications. In particular, a sufficient amount of x-rays can be generated by this device to make it an excellent and flexible Compton backscattered x-ray (CBX) source for high throughput x-ray lithography and many other applications.

Compton backscattered collmated X-ray source

DOEpatents

Ruth, Ronald D.; Huang, Zhirong

2000-01-01

A high-intensity, inexpensive and collimated x-ray source for applications such as x-ray lithography is disclosed. An intense pulse from a high power laser, stored in a high-finesse resonator, repetitively collides nearly head-on with and Compton backscatters off a bunched electron beam, having relatively low energy and circulating in a compact storage ring. Both the laser and the electron beams are tightly focused and matched at the interaction region inside the optical resonator. The laser-electron interaction not only gives rise to x-rays at the desired wavelength, but also cools and stabilizes the electrons against intrabeam scattering and Coulomb repulsion with each other in the storage ring. This cooling provides a compact, intense bunch of electrons suitable for many applications. In particular, a sufficient amount of x-rays can be generated by this device to make it an excellent and flexible Compton backscattered x-ray (CBX) source for high throughput x-ray lithography and many other applications.

Application of stereo x-ray photogrammetry (SRM) in the determination of absorbed dose values during intracavitary radiation therapy

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

van Kleffens, H.J.; Star, W.M.

1979-04-01

The method of stereo x-ray photogrammetry is described, using a stereo x-ray comparator, as well as some clinical applications. The x-ray equipment consists of two x-ray tubes and a pneumatically driven cassette changer, developed to reduce effects of patient or organ motion between stero radiographs. The accuracy of the set-up is demonstated with measurements on a geometrical model and on a gelatine phantom containing radium needles. The clinical use is reported in determining dose rates to points of the intestinal wall during intracavitary radiotherapy of gynecological cancer. In a number of cases the stereo measurements have resulted in a changemore » in the application time or in the charge or position of the applicator, possibly preventing later complications, as a result of a high dose. Future applications for implant dosimetry (/sup 192/Ir, /sup 125/I) are suggested.« 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

The Refined Shock Velocity of the X-Ray Filaments in the RCW 86 Northeast Rim

NASA Technical Reports Server (NTRS)

Yamaguchi, Hiroya; Katsuda, Satoru; Castro, Daniel; Williams, Brian J.; Lopez, Laura A.; Slane, Patrick O.; Smith, Randall K.; Petre, Robert

2017-01-01

A precise measurement of shock velocities is crucial for constraining the mechanism and efficiency of cosmic-ray (CR) acceleration at supernova remnant (SNR) shock fronts. The northeastern rim of the SNR RCW 86 is thought to be a particularly efficient CR acceleration site, owing to the recent result in which an extremely high shock velocity of 6000 km s1 was claimed. Here, we revisit the same SNR rim with the Chandra X-ray Observatory, 11 years after the first observation. This longer baseline than previously available allows us to determine a more accurate proper motion of the nonthermal X-ray filament, revealing a much lower velocity of 3000 340 km s1 (and even slower at a brighter region). Although the value has dropped to one-half of that from the previous X-ray measurement, it is still higher than the mean velocity of the H filaments in this region (1200 km s1). This discrepancy implies that the filaments bright in nonthermal X-rays and H emission trace different velocity components, and thus a CR pressure constrained by combining the X-ray kinematics and the H spectroscopy can easily be overestimated. We also measure the proper motion of the thermal X-ray filament immediately to the south of the nonthermal one. The inferred velocity (720 360 km s1) is significantly lower than that of the nonthermal filament, suggesting the presence of denser ambient material, possibly a wall formed by a wind from the progenitor, which has drastically slowed down the shock.

Protein Structure Validation and Refinement Using Amide Proton Chemical Shifts Derived from Quantum Mechanics

PubMed Central

Christensen, Anders S.; Linnet, Troels E.; Borg, Mikael; Boomsma, Wouter; Lindorff-Larsen, Kresten; Hamelryck, Thomas; Jensen, Jan H.

2013-01-01

We present the ProCS method for the rapid and accurate prediction of protein backbone amide proton chemical shifts - sensitive probes of the geometry of key hydrogen bonds that determine protein structure. ProCS is parameterized against quantum mechanical (QM) calculations and reproduces high level QM results obtained for a small protein with an RMSD of 0.25 ppm (r = 0.94). ProCS is interfaced with the PHAISTOS protein simulation program and is used to infer statistical protein ensembles that reflect experimentally measured amide proton chemical shift values. Such chemical shift-based structural refinements, starting from high-resolution X-ray structures of Protein G, ubiquitin, and SMN Tudor Domain, result in average chemical shifts, hydrogen bond geometries, and trans-hydrogen bond (h3 JNC') spin-spin coupling constants that are in excellent agreement with experiment. We show that the structural sensitivity of the QM-based amide proton chemical shift predictions is needed to obtain this agreement. The ProCS method thus offers a powerful new tool for refining the structures of hydrogen bonding networks to high accuracy with many potential applications such as protein flexibility in ligand binding. PMID:24391900

Phase-contrast x-ray computed tomography for biological imaging

NASA Astrophysics Data System (ADS)

Momose, Atsushi; Takeda, Tohoru; Itai, Yuji

1997-10-01

We have shown so far that 3D structures in biological sot tissues such as cancer can be revealed by phase-contrast x- ray computed tomography using an x-ray interferometer. As a next step, we aim at applications of this technique to in vivo observation, including radiographic applications. For this purpose, the size of view field is desired to be more than a few centimeters. Therefore, a larger x-ray interferometer should be used with x-rays of higher energy. We have evaluated the optimal x-ray energy from an aspect of does as a function of sample size. Moreover, desired spatial resolution to an image sensor is discussed as functions of x-ray energy and sample size, basing on a requirement in the analysis of interference fringes.

Local structural and chemical ordering of nanosized Pt3±δCo probed by multiple-scattering x-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Greco, Giorgia; Witkowska, Agnieszka; Principi, Emiliano; Minicucci, Marco; di Cicco, Andrea

2011-04-01

This work reports a detailed investigation of the local structure and chemical disorder of a Pt3±δCo thin film and Pt3±δCo nanoparticles. We have used a combination of techniques including x-ray absorption spectroscopy (XAS), x-ray diffraction (XRD), and high-resolution transmission electron microscopy (TEM). High-quality XAS spectra at the Co K edge and Pt L3 edge have been analyzed using double-edge multiple-scattering data analysis. Structural extended x-ray absorption fine structure (EXAFS) refinements have been performed accounting for the reduction of the coordination numbers and degeneracy of three-atom configurations, resulting from the measured size distribution and stoichiometry. The important effect of chemical ordering on pair and three-atom configurations has been studied using computer simulations based on a simple model accounting for substitutional disorder, defined by an order parameter s. It has been found that individual EXAFS signals related to the minority species (Co) are extremely sensitive to substitutional disorder so their intensities, especially those of the collinear three-atom configurations, can be used as a measure of the ordering level. The thin film has been found to be chemically disordered (s⩽0.4), in agreement with previous estimates. The Pt3±δCo nanoalloy has been found to be partially ordered (s=0.6±0.1) while the local structure around Co atoms is characterized by a higher level of structural disorder as compared to the bulk-like thin film. The robust approach for nanomaterial characterization used in this work combining different techniques can, in principle, be applied for structural refinements of any binary nanocrystalline functional system.

Crystal structure and X-ray photoemission spectroscopic study of A{sub 2}LaMO{sub 6} [A=Ba, Ca; M=Nb, Ta

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

Dutta, Alo, E-mail: alo_dutta@yahoo.com; Saha, Sujoy; Kumari, Premlata

2015-09-15

The X-ray photoemission spectroscopic (XPS) study of the double perovskite oxides A{sub 2}LaMO{sub 6} [A=Ba, Ca; M=Nb, Ta] synthesized by the solid-state reaction technique has been carried out to investigate the nature of the chemical state of the constituent ions and the bonding between them. The Rietveld refinement of the X-ray diffraction patterns suggests the monoclinic crystal structure of all the materials at room temperature. The negative and positive chemical shifts of the core level XPS spectrum of O-1s and Nb-3d{sub 3/2}/Ta-4f{sub 5/2} respectively suggest the covalent bonding between Nb/Ta cations and O ion. The change of the bonding strengthmore » between the anion and the cations from one material to another has been analyzed. The vibrational property of the materials is investigated using the room temperature Raman spectra. A large covalency of Ta-based compound than Nb compound is confirmed from the relative shifting of the Raman modes of the materials. - Graphical abstract: Crystal structure of two perovskite oxides CLN and CLT is investigated. XPS study confirms the two different co-ordination environments of Ca and covalent bonding between B-site cations and O-ion. - Highlights: • Ordered perovskite structure obtained by Rietveld refinement of XRD patterns. • Study of nature of chemical bonding by X-ray photoemission spectroscopy. • Opposite chemical shift of d-states of Nb/Ta with respect to O. • Covalent bonding between d-states of Nb/Ta and O. • Relative Raman shifts of CLN and CLT substantiate the more covalent character of Ta than Nb.« less

Structural, magnetic, and Mössbauer spectroscopy of Cu substituted M-type hexaferrites

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

Awadallah, Ahmad, E-mail: ahmadmoh@yahoo.co; Mahmood, Sami H., E-mail: s.mahmood@ju.edu.jo; Maswadeh, Yazan, E-mail: nawabra251@gmail.com

2016-02-15

Highlights: • Single BaM hexaferrite structural phases with Cu substations were prepared. • The magnetocrystalline anisotropy decreased with Cu substitution. • The coercivity was significantly modified while the magnetization remained high. • Hexaferrites with 0.2–0.4 Cu possess properties suitable for magnetic recording. • Ionic distributions from structural refinement agreed with Mössbauer spectroscopy. - Abstract: BaFe{sub 12−x}Cu{sub x}O{sub 19} hexaferrites were prepared using ball milling and sintering at 1100 °C. Refinement of the X-ray diffraction patterns was carried out to determine the structural parameters and the ionic distribution over the crystallographic sites. The preferential site occupation and valence state of Cumore » was consistent with the results obtained from the analysis of Mössbauer spectra. Further, the magnetic parameters of the samples were discussed in light of the structural and Mössbauer analyses. The magnetic phase transition temperature was found to decrease with the level of Cu substitution, in accordance with the reduction of the superexchange interactions. Further, the magnetic softening of the hexaferrite and the significant reduction in magnetocrystalline anisotropy with Cu substitution was consistent with the ionic distribution in the lattice. This study clearly demonstrated the feasibility of using a simple method to fabricate hexaferrites with a modified coercivity, while maintain the saturation magnetization high enough for practical applications.« less

NMR Crystallography of Enzyme Active Sites: Probing Chemically-Detailed, Three-Dimensional Structure in Tryptophan Synthase

PubMed Central

Dunn, Michael F.

2013-01-01

Conspectus NMR crystallography – the synergistic combination of X-ray diffraction, solid-state NMR spectroscopy, and computational chemistry – offers unprecedented insight into three-dimensional, chemically-detailed structure. From its initial role in refining diffraction data of organic and inorganic solids, NMR crystallography is now being developed for application to active sites in biomolecules, where it reveals chemically-rich detail concerning the interactions between enzyme site residues and the reacting substrate that is not achievable when X-ray, NMR, or computational methodologies are applied in isolation. For example, typical X-ray crystal structures (1.5 to 2.5 Å resolution) of enzyme-bound intermediates identify possible hydrogen-bonding interactions between site residues and substrate, but do not directly identify the protonation state of either. Solid-state NMR can provide chemical shifts for selected atoms of enzyme-substrate complexes, but without a larger structural framework in which to interpret them, only empirical correlations with local chemical structure are possible. Ab initio calculations and molecular mechanics can build models for enzymatic processes, but rely on chemical details that must be specified. Together, however, X-ray diffraction, solid-state NMR spectroscopy, and computational chemistry can provide consistent and testable models for structure and function of enzyme active sites: X-ray crystallography provides a coarse framework upon which models of the active site can be developed using computational chemistry; these models can be distinguished by comparison of their calculated NMR chemical shifts with the results of solid-state NMR spectroscopy experiments. Conceptually, each technique is a puzzle piece offering a generous view of the big picture. Only when correctly pieced together, however, can they reveal the big picture at highest resolution. In this Account, we detail our first steps in the development of NMR crystallography for application to enzyme catalysis. We begin with a brief introduction to NMR crystallography and then define the process that we have employed to probe the active site in the β-subunit of tryptophan synthase with unprecedented atomic-level resolution. This approach has resulted in a novel structural hypothesis for the protonation state of the quinonoid intermediate in tryptophan synthase and its surprising role in directing the next step in the catalysis of L-Trp formation. PMID:23537227

Correlated high-resolution x-ray diffraction photoluminescence and atom probe tomography analysis of continuous and discontinuous In xGa 1-xN quantum wells

DOE PAGES

Ren, Xiaochen; Riley, James R.; Koleske, Daniel; ...

2015-07-14

In this study, atom probe tomography (APT) is used to characterize the influence of hydrogen dosing duringGaN barrier growth on the indium distribution of In xGa 1-xN quantum wells, and correlatedmicro-photoluminescence is used to measure changes in the emission spectrum and efficiency. We found that relative to the control growth, hydrogen dosing leads to a 50% increase in emission intensity arising from discontinuous quantum wells that are narrower, of lower indium content, and with more abrupt interfaces. Additionally, simulations of carrier distributions based on APT composition profiles indicate that the greater carrier confinement leads to an increased radiative recombination rate.more » Furthermore, APT analysis of quantum well profiles enables refinement of x-ray diffractionanalysis for more accurate nondestructive measurements of composition.« less

Structural and Microstructural Correlations of Physical Properties in Natural Almandine-Pyrope Solid Solution: Al70Py29

NASA Astrophysics Data System (ADS)

Sibi, N.; Subodh, G.

2017-12-01

Garnets are naturally occurring minerals with the general formula X3Y2Z3O12 having various applications. In the present study, the structural and physical properties of a garnet mineral obtained from Indian Rare Earth Ltd., Manavalakurichi, Tamil Nadu, India were comprehensively investigated. The compositional analysis using electron probe micro analysis (EPMA) revealed that the mineral belongs to almandine-pyrope solid solution (Al70Py29) with the chemical formula (Fe1.72Mg0.8Mn0.01Ca0.02) (Fe0.04Al2.36) Si2.93O12. Rietveld refinement of the x-ray diffraction pattern confirms that the space group is Ia{ - }\\overline{3} d with refined cubic lattice parameter a = 11.550(4) Å. The refined occupancy values of multiple cations in the dodecahedral and octahedral sites are in agreement with the EPMA data. Fourier transform infrared and FT Raman spectra show bands corresponding to almandine-pyrope solid solution. Peak splitting of IR and Raman bands confirms presence of multiple cations in the dodecahedral site. Thermogravimetric/differential thermal analysis shows that the mineral is stable up to 600°C in spite of the presence of Fe2+ ions. Low temperature magnetic susceptibility data is in agreement with the amount of Fe2+ ions present in the mineral. The dielectric constant of the mineral varied from 6 to 16.5 when sintered at temperatures ranging from 600°C to 1250°C.

Structural studies of the HIV-1 accessory protein Vpu in langmuir monolayers: synchrotron X-ray reflectivity.

PubMed Central

Zheng, S; Strzalka, J; Ma, C; Opella, S J; Ocko, B M; Blasie, J K

2001-01-01

Vpu is an 81 amino acid integral membrane protein encoded by the HIV-1 genome with a N-terminal hydrophobic domain and a C-terminal hydrophilic domain. It enhances the release of virus from the infected cell and triggers degradation of the virus receptor CD4. Langmuir monolayers of mixtures of Vpu and the phospholipid 1,2-dilignoceroyl-sn-glycero-3-phosphocholine (DLgPC) at the water-air interface were studied by synchrotron radiation-based x-ray reflectivity over a range of mole ratios at constant surface pressure and for several surface pressures at a maximal mole ratio of Vpu/DLgPC. Analysis of the x-ray reflectivity data by both slab model-refinement and model-independent box-refinement methods firmly establish the monolayer electron density profiles. The electron density profiles as a function of increasing Vpu/DLgPC mole ratio at a constant, relatively high surface pressure indicated that the amphipathic helices of the cytoplasmic domain lie on the surface of the phospholipid headgroups and the hydrophobic transmembrane helix is oriented approximately normal to the plane of monolayer within the phospholipid hydrocarbon chain layer. At maximal Vpu/DLgPC mole ratio, the tilt of the transmembrane helix with respect to the monolayer normal decreases with increasing surface pressure and the conformation of the cytoplasmic domain varies substantially with surface pressure. PMID:11259297

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.

Use of electron cyclotron resonance x-ray source for nondestructive testing application

NASA Astrophysics Data System (ADS)

Baskaran, R.; Selvakumaran, T. S.

2006-03-01

Electron cyclotron resonance (ECR) technique is being used for generating x rays in the low-energy region (<150keV). Recently, the source is used for the calibration of thermoluminescent dosimetry (TLD) badges. In order to qualify the ECR x-ray source for imaging application, the source should give uniform flux over the area under study. Lead collimation arrangement is made to get uniform flux. The flux profile is measured using a teletector at different distance from the port and uniform field region of 10×10cm2 has been marked at 20cm from the x-ray exit port. A digital-to-analog converter (DAC) circuit pack is used for examining the source performance. The required dose for nondestructive testing examination has been estimated using a hospital x-ray machine and it is found to be 0.05mSv. Our source experimental parameters are tuned and the DAC circuit pack was exposed for nearly 7min to get the required dose value. The ECR x-ray source operating parameters are argon pressure: 10-5Torr, microwave power: 350W, and coil current: 0A. The effective energy of the x-ray spectrum is nearly 40keV. The x-ray images obtained from ECR x-ray source and hospital medical radiography machine are compared. It is found that the image obtained from ECR x-ray source is suitable for NDT application.

PROBING X-RAY ABSORPTION AND OPTICAL EXTINCTION IN THE INTERSTELLAR MEDIUM USING CHANDRA OBSERVATIONS OF SUPERNOVA REMNANTS

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

Foight, Dillon R.; Slane, Patrick O.; Güver, Tolga

We present a comprehensive study of interstellar X-ray extinction using the extensive Chandra supernova remnant (SNR) archive and use our results to refine the empirical relation between the hydrogen column density and optical extinction. In our analysis, we make use of the large, uniform data sample to assess various systematic uncertainties in the measurement of the interstellar X-ray absorption. Specifically, we address systematic uncertainties that originate from (i) the emission models used to fit SNR spectra; (ii) the spatial variations within individual remnants; (iii) the physical conditions of the remnant such as composition, temperature, and non-equilibrium regions; and (iv) themore » model used for the absorption of X-rays in the interstellar medium. Using a Bayesian framework to quantify these systematic uncertainties, and combining the resulting hydrogen column density measurements with the measurements of optical extinction toward the same remnants, we find the empirical relation N {sub H} = (2.87 ± 0.12) × 10{sup 21} A {sub V} cm{sup 2}, which is significantly higher than the previous measurements.« less

Role of Molecular Structure on X-ray Diffraction in Thermotropic Uniaxial and Biaxial Nematic Liquid Crystal Phases

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

Acharya, Bharat R.; Kang, Shin-Woong; Prasad, Veena

2009-08-27

X-ray diffraction is one of the most definitive methods to determine the structure of condensed matter phases, and it has been applied to unequivocally infer the structures of conventional calamitic and lyotropic liquid crystals. With the advent of bent-core and tetrapodic mesogens and the discovery of the biaxial nematic phase in them, the experimental results require more careful interpretation and analysis. Here, we present ab-initio calculations of X-ray diffraction patterns in the isotropic, uniaxial nematic, and biaxial nematic phases of bent-core mesogens. A simple Meier-Saupe-like molecular distribution function is employed to describe both aligned and unaligned mesophases. The distribution functionmore » is decomposed into two, polar and azimuthal, distribution functions to calculate the effect of the evolution of uniaxial and biaxial nematic orientational order. The calculations provide satisfactory semiquantitative interpretations of experimental results. The calculations presented here should provide a pathway to more refined and quantitative analysis of X-ray diffraction data from the biaxial nematic phase.« less

Role of Molecular Structure on X-ray Diffraction in Uniaxial and Biaxial Phases of Thermotropic Liquid Crystals

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

Acharya, Bharat R.; Kang, Shin-Woong; Prasad, Veena

2009-04-29

X-ray diffraction is one of the most definitive methods to determine the structure of condensed matter phases, and it has been applied to unequivocally infer the structures of conventional calamitic and lyotropic liquid crystals. With the advent of bent-core and tetrapodic mesogens and the discovery of the biaxial nematic phase in them, the experimental results require more careful interpretation and analysis. Here, we present ab-initio calculations of X-ray diffraction patterns in the isotropic, uniaxial nematic, and biaxial nematic phases of bent-core mesogens. A simple Meier-Saupe-like molecular distribution function is employed to describe both aligned and unaligned mesophases. The distribution functionmore » is decomposed into two, polar and azimuthal, distribution functions to calculate the effect of the evolution of uniaxial and biaxial nematic orientational order. The calculations provide satisfactory semiquantitative interpretations of experimental results. The calculations presented here should provide a pathway to more refined and quantitative analysis of X-ray diffraction data from the biaxial nematic phase.« less

The Mapping X-Ray Fluorescence Spectrometer (mapx)

NASA Astrophysics Data System (ADS)

Blake, D. F.; Sarrazin, P.; Bristow, T.; Downs, R. T.; Gailhanou, M.; Marchis, F.; Ming, D. W.; Morris, R. V.; Sole, V. A.; Thompson, K.; Walter, P.; Wilson, M.; Yen, A. S.; Webb, S.

2016-12-01

MapX will provide elemental imaging at ≤100 µm spatial resolution over 2.5 X 2.5 cm areas, yielding elemental chemistry at or below the scale length where many relict physical, chemical, and biological features can be imaged and interpreted in ancient rocks. MapX is a full-frame spectroscopic imager positioned on soil or regolith with touch sensors. During an analysis, an X-ray source (tube or radioisotope) bombards the sample surface with X-rays or α-particles / γ-rays, resulting in sample X-ray Fluorescence (XRF). Fluoresced X-rays pass through an X-ray lens (X-ray µ-Pore Optic, "MPO") that projects a spatially resolved image of the X-rays onto a CCD. The CCD is operated in single photon counting mode so that the positions and energies of individual photons are retained. In a single analysis, several thousand frames are stored and processed. A MapX experiment provides elemental maps having a spatial resolution of ≤100 µm and quantitative XRF spectra from Regions of Interest (ROI) 2 cm ≤ x ≤ 100 µm. ROI are compared with known rock and mineral compositions to extrapolate the data to rock types and putative mineralogies. The MapX geometry is being refined with ray-tracing simulations and with synchrotron experiments at SLAC. Source requirements are being determined through Monte Carlo modeling and experiment using XMIMSIM [1], GEANT4 [2] and PyMca [3] and a dedicated XRF test fixture. A flow-down of requirements for both tube and radioisotope sources is being developed from these experiments. In addition to Mars lander and rover missions, MapX could be used for landed science on other airless bodies (Phobos/Deimos, Comet nucleus, asteroids, the Earth's moon, and the icy satellites of the outer planets, including Europa. [1] Schoonjans, T. et al.(2012). Spectrachim. Acta Part B, 70, 10-23. [2] Agostinelli, S. et al. (2003). Nucl. Instr. and Methods in Phys. Research A, 506, 250-303. [3] V.A. Solé et al. (2007). Spectrochim. Acta Part B, 62, 63-68.

Synthesis and crystal structure determination of yttrium ultraphosphate YP 5O 14

NASA Astrophysics Data System (ADS)

Mbarek, A.; Graia, M.; Chadeyron, G.; Zambon, D.; Bouaziz, J.; Fourati, M.

2009-03-01

The crystal structure of monoclinic YP 5O 14 (space group C2/ c, a=12.919(2) Å, b=12.796(4) Å, c=12.457(2) Å, β=91.30(1)°, Z=8) has been refined from single-crystal X-ray diffraction data. Full-matrix least-squares refinement on F2 using 2249 independent reflections for 183 refinable parameters results in a final R value of 0.027 ( ωR=0.069). The structure is isotypic with HoP 5O 14. This structure is built up from infinite layers of PO 4 tetrahedra linked through isolated YO 8 polyhedra. The three-dimensional cohesion of the framework results from Y-O-P bridges. This crystal structure refinement leads to the calculated X-ray diffraction powder pattern of this monoclinic polymorph, which has been the starting point of a thorough study of the solid-state synthesis of this ultraphosphate. This investigation further leads to a better outstanding of features observed during the synthesis of powdered samples. The thermal behavior of this ultraphosphate has been studied by DTA and TGA analyses. The infrared and Raman spectroscopic characterizations have been carried out on polycrystalline samples. The luminescence properties of the Eu 3+ ion incorporated in the monoclinic C2/ c polymorph of YP 5O 14 as local structural probe show that in YP 5O 14: 5% Eu 3+ sample, the Eu 3+ ions are distributed over the two Y 3+ crystallographic sites of C 2 symmetry of this structure.

Grain Refinement by Authigenic Inoculation Inherited from the Medium-Range Order Structure of Ni-Cr-W Superalloy

NASA Astrophysics Data System (ADS)

Gao, Zhongtang; Hu, Rui; Guo, Wei; Zhang, Chuanwei

2018-04-01

The combination of liquidus casting and thermal control solidification furnace was applied to obtain a fine-grained ingot. A rapid quenching method and x-ray diffraction measurement were used to investigate the effect of authigenic inoculation on grain refinement. The structure factor S(Q) of liquid Ni-Cr-W superalloy at 1400 °C (Liquidus temperature) and bright-field image of the microstructures quenched from 1400 °C have been measured by the high-temperature x-ray diffractometer and the transmission electron microscopy (TEM), respectively. The results show that a pre-peak exists on a S(Q) curve at the liquidus temperature. The clusters of atom in rapidly quenched microstructures obtained by isothermal heat treatment at 1400 °C were studied using TEM. Meanwhile, the effect of isothermal different temperatures on rapidly quenched microstructures was studied. The results also show that there are only the globular, equiaxed grains distributed in the solidification structure. These particles are inherited from the medium-range order structure, which is beneficial for grain refinement. The normalized work-hardening rate-strain curve indicates the work-hardening rate of fine grain is higher than that of conventional grain at the same temperature and the same deformation.

Grain Refinement by Authigenic Inoculation Inherited from the Medium-Range Order Structure of Ni-Cr-W Superalloy

NASA Astrophysics Data System (ADS)

Gao, Zhongtang; Hu, Rui; Guo, Wei; Zhang, Chuanwei

2018-05-01

The combination of liquidus casting and thermal control solidification furnace was applied to obtain a fine-grained ingot. A rapid quenching method and x-ray diffraction measurement were used to investigate the effect of authigenic inoculation on grain refinement. The structure factor S( Q) of liquid Ni -Cr-W superalloy at 1400 °C (Liquidus temperature) and bright-field image of the microstructures quenched from 1400 °C have been measured by the high-temperature x-ray diffractometer and the transmission electron microscopy (TEM), respectively. The results show that a pre-peak exists on a S( Q) curve at the liquidus temperature. The clusters of atom in rapidly quenched microstructures obtained by isothermal heat treatment at 1400 °C were studied using TEM. Meanwhile, the effect of isothermal different temperatures on rapidly quenched microstructures was studied. The results also show that there are only the globular, equiaxed grains distributed in the solidification structure. These particles are inherited from the medium-range order structure, which is beneficial for grain refinement. The normalized work-hardening rate-strain curve indicates the work-hardening rate of fine grain is higher than that of conventional grain at the same temperature and the same deformation.

Incorporation of Cadmium and Nickel into Ferrite Spinel Solid Solution: X-ray Diffraction and X-ray Absorption Fine Structure Analyses.

PubMed

Su, Minhua; Liao, Changzhong; Chan, Tingshan; Shih, Kaimin; Xiao, Tangfu; Chen, Diyun; Kong, Lingjun; Song, Gang

2018-01-16

The feasibility of incorporating Cd and Ni in hematite was studied by investigating the interaction mechanism for the formation of Cd x Ni 1-x Fe 2 O 4 solid solutions (CNFs) from CdO, NiO, and α-Fe 2 O 3 . X-ray diffraction results showed that the CNFs crystallized into spinel structures with increasing lattice parameters as the Cd content in the precursors was increased. Cd 2+ ions were found to occupy the tetrahedral sites, as evidenced by Rietveld refinement and extended X-ray absorption fine structure analyses. The incorporation of Cd and Ni into ferrite spinel solid solution strongly relied on the processing parameters. The incorporation of Cd and Ni into the CNFs was greater at high x values (0.7 < x ≤ 1.0) than at low x values (0.0 ≤ x ≤ 0.7). A feasible treatment technique based on the investigated mechanism of CNF formation was developed, involving thermal treatment of waste sludge containing Cd and Ni. Both of these metals in the waste sludge were successfully incorporated into a ferrite spinel solid solution, and the concentrations of leached Cd and Ni from this solid solution were substantially reduced, stabilizing at low levels. This research offers a highly promising approach for treating the Cd and Ni content frequently encountered in electronic waste and its treatment residues.

Investigation on temporal evolution of the grain refinement in copper under high strain rate loading via in-situ synchrotron measurement and predictive modeling

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

Shah, Pooja Nitin; Shin, Yung C.; Sun, Tao

Synchrotron X-rays are integrated with a modified Kolsky tension bar to conduct in situ tracking of the grain refinement mechanism operating during the dynamic deformation of metals. Copper with an initial average grain size of 36 μm is refined to 6.3 μm when loaded at a constant high strain rate of 1200 s -1. The synchrotron measurements revealed the temporal evolution of the grain refinement mechanism in terms of the initiation and rate of refinement throughout the loading test. A multiscale coupled probabilistic cellular automata based recrystallization model has been developed to predict the microstructural evolution occurring during dynamic deformationmore » processes. The model accurately predicts the initiation of the grain refinement mechanism with a predicted final average grain size of 2.4 μm. As a result, the model also accurately predicts the temporal evolution in terms of the initiation and extent of refinement when compared with the experimental results.« less

Investigation on temporal evolution of the grain refinement in copper under high strain rate loading via in-situ synchrotron measurement and predictive modeling

DOE PAGES

Shah, Pooja Nitin; Shin, Yung C.; Sun, Tao

2017-10-03

Synchrotron X-rays are integrated with a modified Kolsky tension bar to conduct in situ tracking of the grain refinement mechanism operating during the dynamic deformation of metals. Copper with an initial average grain size of 36 μm is refined to 6.3 μm when loaded at a constant high strain rate of 1200 s -1. The synchrotron measurements revealed the temporal evolution of the grain refinement mechanism in terms of the initiation and rate of refinement throughout the loading test. A multiscale coupled probabilistic cellular automata based recrystallization model has been developed to predict the microstructural evolution occurring during dynamic deformationmore » processes. The model accurately predicts the initiation of the grain refinement mechanism with a predicted final average grain size of 2.4 μm. As a result, the model also accurately predicts the temporal evolution in terms of the initiation and extent of refinement when compared with the experimental results.« less

Method and apparatus for digitally based high speed x-ray spectrometer

DOEpatents

Warburton, W.K.; Hubbard, B.

1997-11-04

A high speed, digitally based, signal processing system which accepts input data from a detector-preamplifier and produces a spectral analysis of the x-rays illuminating the detector. The system achieves high throughputs at low cost by dividing the required digital processing steps between a ``hardwired`` processor implemented in combinatorial digital logic, which detects the presence of the x-ray signals in the digitized data stream and extracts filtered estimates of their amplitudes, and a programmable digital signal processing computer, which refines the filtered amplitude estimates and bins them to produce the desired spectral analysis. One set of algorithms allow this hybrid system to match the resolution of analog systems while operating at much higher data rates. A second set of algorithms implemented in the processor allow the system to be self calibrating as well. The same processor also handles the interface to an external control computer. 19 figs.

Method and apparatus for digitally based high speed x-ray spectrometer

DOEpatents

Warburton, William K.; Hubbard, Bradley

1997-01-01

A high speed, digitally based, signal processing system which accepts input data from a detector-preamplifier and produces a spectral analysis of the x-rays illuminating the detector. The system achieves high throughputs at low cost by dividing the required digital processing steps between a "hardwired" processor implemented in combinatorial digital logic, which detects the presence of the x-ray signals in the digitized data stream and extracts filtered estimates of their amplitudes, and a programmable digital signal processing computer, which refines the filtered amplitude estimates and bins them to produce the desired spectral analysis. One set of algorithms allow this hybrid system to match the resolution of analog systems while operating at much higher data rates. A second set of algorithms implemented in the processor allow the system to be self calibrating as well. The same processor also handles the interface to an external control computer.

VizieR Online Data Catalog: Multiwavelength photometry of CDFS X-ray sources (Brusa+, 2009)

NASA Astrophysics Data System (ADS)

Brusa, M.; Fiore, F.; Santini, P.; Grazian, A.; Comastri, A.; Zamorani, G.; Hasinger, G.; Merloni, A.; Civano, F.; Fontana, A.; Mainieri, V.

2010-03-01

The co-evolution of host galaxies and the active black holes which reside in their centre is one of the most important topics in modern observational cosmology. Here we present a study of the properties of obscured active galactic nuclei (AGN) detected in the CDFS 1 Ms observation and their host galaxies. We limited the analysis to the MUSIC area, for which deep K-band observations obtained with ISAAC@VLT are available, ensuring accurate identifications of the counterparts of the X-ray sources as well as reliable determination of photometric redshifts and galaxy parameters, such as stellar masses and star formation rates. In particular, we: 1) refined the X-ray/infrared/optical association of 179 sources in the MUSIC area detected in the Chandra observation; 2) studied the host galaxies observed and rest frame colors and properties. (2 data files).

Improvement of thermoelectric properties and their correlations with electron effective mass in Cu1.98SxSe1-x.

PubMed

Zhao, Lanling; Fei, Frank Yun; Wang, Jun; Wang, Funing; Wang, Chunlei; Li, Jichao; Wang, Jiyang; Cheng, Zhenxiang; Dou, Shixue; Wang, Xiaolin

2017-01-16

Sulphur doping effects on the crystal structures, thermoelectric properties, density-of-states, and effective mass in Cu 1.98 S x Se 1-x were studied based on the electrical and thermal transport property measurements, and first-principles calculations. The X-ray diffraction patterns and Rietveld refinements indicate that room temperature Cu 1.98 S x Se 1-x (x = 0, 0.02, 0.08, 0.16) and Cu 1.98 S x Se 1-x (x = 0.8, 0.9, 1.0) have the same crystal structure as monoclinic-Cu 2 Se and orthorhombic-Cu 2 S, respectively. Sulphur doping can greatly enhance zT values when x is in the range of 0.8≤ × ≤1.0. Furthermore, all doped samples show stable thermoelectric compatibility factors over a broad temperature range from 700 to 1000 K, which could greatly benefit their practical applications. First-principles calculations indicate that both the electron density-of-sates and the effective mass for all the compounds exhibit non-monotonic sulphur doping dependence. It is concluded that the overall thermoelectric performance of the Cu 1.98 S x Se 1-x system is mainly correlated with the electron effective mass and the density-of-states.

Wide-area phase-contrast X-ray imaging using large X-ray interferometers

NASA Astrophysics Data System (ADS)

Momose, Atsushi; Takeda, Tohoru; Yoneyama, Akio; Koyama, Ichiro; Itai, Yuji

2001-07-01

Large X-ray interferometers are developed for phase-contrast X-ray imaging aiming at medical applications. A monolithic X-ray interferometer and a separate one are studied, and currently a 25 mm×20 mm view area can be generated. This paper describes the strategy of our research program and some recent developments.

Computed tomography of x-ray images using neural networks

NASA Astrophysics Data System (ADS)

Allred, Lloyd G.; Jones, Martin H.; Sheats, Matthew J.; Davis, Anthony W.

2000-03-01

Traditional CT reconstruction is done using the technique of Filtered Backprojection. While this technique is widely employed in industrial and medical applications, it is not generally understood that FB has a fundamental flaw. Gibbs phenomena states any Fourier reconstruction will produce errors in the vicinity of all discontinuities, and that the error will equal 28 percent of the discontinuity. A number of years back, one of the authors proposed a biological perception model whereby biological neural networks perceive 3D images from stereo vision. The perception model proports an internal hard-wired neural network which emulates the external physical process. A process is repeated whereby erroneous unknown internal values are used to generate an emulated signal with is compared to external sensed data, generating an error signal. Feedback from the error signal is then sued to update the erroneous internal values. The process is repeated until the error signal no longer decrease. It was soon realized that the same method could be used to obtain CT from x-rays without having to do Fourier transforms. Neural networks have the additional potential for handling non-linearities and missing data. The technique has been applied to some coral images, collected at the Los Alamos high-energy x-ray facility. The initial images show considerable promise, in some instances showing more detail than the FB images obtained from the same data. Although routine production using this new method would require a massively parallel computer, the method shows promise, especially where refined detail is required.

Capture and X-ray diffraction studies of protein microcrystals in a microfluidic trap array

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

Lyubimov, Artem Y.; Stanford University, Stanford, CA 94305; Stanford University, Stanford, CA 94305

A microfluidic platform has been developed for the capture and X-ray analysis of protein microcrystals, affording a means to improve the efficiency of XFEL and synchrotron experiments. X-ray free-electron lasers (XFELs) promise to enable the collection of interpretable diffraction data from samples that are refractory to data collection at synchrotron sources. At present, however, more efficient sample-delivery methods that minimize the consumption of microcrystalline material are needed to allow the application of XFEL sources to a wide range of challenging structural targets of biological importance. Here, a microfluidic chip is presented in which microcrystals can be captured at fixed, addressablemore » points in a trap array from a small volume (<10 µl) of a pre-existing slurry grown off-chip. The device can be mounted on a standard goniostat for conducting diffraction experiments at room temperature without the need for flash-cooling. Proof-of-principle tests with a model system (hen egg-white lysozyme) demonstrated the high efficiency of the microfluidic approach for crystal harvesting, permitting the collection of sufficient data from only 265 single-crystal still images to permit determination and refinement of the structure of the protein. This work shows that microfluidic capture devices can be readily used to facilitate data collection from protein microcrystals grown in traditional laboratory formats, enabling analysis when cryopreservation is problematic or when only small numbers of crystals are available. Such microfluidic capture devices may also be useful for data collection at synchrotron sources.« less

Investigation of thermally evaporated high resistive B-doped amorphous selenium alloy films and metal contact studies

NASA Astrophysics Data System (ADS)

Oner, Cihan; Nguyen, Khai V.; Pak, Rahmi O.; Mannan, Mohammad A.; Mandal, Krishna C.

2015-08-01

Amorphous selenium (a-Se) alloy materials with arsenic, chlorine, boron, and lithium doping were synthesized for room temperature nuclear radiation detector applications using an optimized alloy composition for enhanced charge transport properties. A multi-step synthetic process has been implemented to first synthesize Se-As and Se-Cl master alloys from zone-refined Se (~ 7N), and then synthesized the final alloys for thermally evaporated large-area thin-film deposition on oxidized aluminum (Al/Al2O3) and indium tin oxide (ITO) coated glass substrates. Material purity, morphology, and compositional characteristics of the alloy materials and films were examined using glow discharge mass spectroscopy (GDMS), inductively coupled plasma mass spectroscopy (ICP-MS), differential scanning calorimetry (DSC), x-ray photoelectron spectroscopy (XPS), x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive analysis by x-rays (EDAX). Current-Voltage (I-V) measurements were carried out to confirm very high resistivity of the alloy thin-films. We have further investigated the junction properties of the alloy films with a wide variety of metals with different work functions (Au, Ni, W, Pd, Cu, Mo, In, and Sn). The aim was to investigate whether the choice of metal can improve the performance of fabricated detectors by minimizing the dark leakage current. For various metal contacts, we have found significant dependencies of metal work functions on current transients by applying voltages from -800 V to +1000 V.

In-situ microscale through-silicon via strain measurements by synchrotron x-ray microdiffraction exploring the physics behind data interpretation

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

Liu, Xi; School of Electrical and Computer Engineering, Georgia Institute of Technology, Atlanta, Georgia 30332; Thadesar, Paragkumar A.

2014-09-15

In-situ microscale thermomechanical strain measurements have been performed in combination with synchrotron x-ray microdiffraction to understand the fundamental cause of failures in microelectronics devices with through-silicon vias. The physics behind the raster scan and data analysis of the measured strain distribution maps is explored utilizing the energies of indexed reflections from the measured data and applying them for beam intensity analysis and effective penetration depth determination. Moreover, a statistical analysis is performed for the beam intensity and strain distributions along the beam penetration path to account for the factors affecting peak search and strain refinement procedure.

Purification, isolation, crystallization, and preliminary X-ray diffraction study of the BTB domain of the centrosomal protein 190 from Drosophila melanogaster

NASA Astrophysics Data System (ADS)

Boyko, K. M.; Nikolaeva, A. Yu.; Kachalova, G. S.; Bonchuk, A. N.; Popov, V. O.

2017-11-01

The spatial organization of the genome is controlled by a special class of architectural proteins, including proteins containing BTB domains that are able to dimerize or multimerize. The centrosomal protein 190 is one of such architectural proteins. The purification, crystallization, and preliminary X-ray diffraction study of the BTB domain of the centrosomal protein 190 are reported. The crystallization conditions were found by the vapor-diffusion technique. The crystals diffracted to 1.5 Å resolution and belonged to sp. gr. P3221. The structure was solved by the molecular replacement method. The structure refinement is currently underway.

X-ray diffraction study of Penicillium Vitale catalase in the complex with aminotriazole

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

Borovik, A. A.; Grebenko, A. I.; Melik-Adamyan, V. R., E-mail: mawr@ns.crys.ras.ru

2011-07-15

The three-dimensional structure of the enzyme catalase from Penicillium vitale in a complex with the inhibitor aminotriazole was solved and refined by protein X-ray crystallography methods. An analysis of the three-dimensional structure of the complex showed that the inhibition of the enzyme occurs as a result of the covalent binding of aminotriazole to the amino-acid residue His64 in the active site of the enzyme. An investigation of the three-dimensional structure of the complex resulted in the amino-acid residues being more precisely identified. The binding sites of saccharide residues and calcium ions in the protein molecule were found.

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.

Synthesis and X-ray structural investigation of (5R*,6S*)-1-benzoyl-5-methylthio-6-methoxy-1-azapenam

NASA Astrophysics Data System (ADS)

Krajewski, J. W.; Gluziński, P.; Grochowski, E.; Pupek, K.; Mishnyov, A.; Kemme, A.

1992-08-01

The compound (5R*,6S*)-1-benzoyl-5-methylthio-6-methoxy-1-azapenam ( 3) has been synthesized and its structure investigated by X-ray diffraction. The compound crystallizes in a monoclinic system, space group Cc, Z = 4, a = 12.01(1), b = 16.51(1), c = 8.048(6) Å, β = 115.87(6)°. The structure was solved by direct methods and refined by a full-matrix, least-squares procedure to give R = 0.070, Rw = 0.046, w = 1.34/(σ 2F). The expected cis configuration around the β-lactam ring was fully confirmed.

Solving local structure around dopants in metal nanoparticles with ab initio modeling of X-ray absorption near edge structure

DOE PAGES

Timoshenko, J.; Shivhare, A.; Scott, R. W.; ...

2016-06-30

We adopted ab-initio X-ray Absorption Near Edge Structure (XANES) modelling for structural refinement of local environments around metal impurities in a large variety of materials. Our method enables both direct modelling, where the candidate structures are known, and the inverse modelling, where the unknown structural motifs are deciphered from the experimental spectra. We present also estimates of systematic errors, and their influence on the stability and accuracy of the obtained results. We illustrate our approach by following the evolution of local environment of palladium atoms in palladium-doped gold thiolate clusters upon chemical and thermal treatments.

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.

A 6 second periodic X-ray source in Carina

NASA Technical Reports Server (NTRS)

Seward, F. D.; Charles, P. A.; Smale, A. P.

1986-01-01

A serendipitous source, 1E 1048.1-5937, was discovered during Einstein imaging observations of the Carina nebula. On July 13, 1979, this source had an intensity of 0.14 IPC counts/s, and the signal was 65 percent pulsed with a period of 6.44 s. An earlier observation failed to detect any source with strength greater than 1/10 the above signal. The source is therefore highly variable, perhaps transient. An Exosat observation of this source on June 20, 1985 confirmed the pulse period and refined the source position to an accuracy of 10 arcsec. On the basis of the position, the source is tentatively identified with a V = 19 optical counterpart. The X-ray spectrum is best fitted by a power law with photon index = 2.26 and a column density of 1.6 x 10 to the 22nd atoms/sq cm. The X-ray characteristics are consistent with an accretion-powered Be star binary.

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

NASA Technical Reports Server (NTRS)

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

X-ray emission from galaxies - The distribution of low-luminosity X-ray sources in the Galactic Centre region

NASA Astrophysics Data System (ADS)

Heard, Victoria; Warwick, Robert

2012-09-01

We report a study of the extended X-ray emission observed in the Galactic Centre (GC) region based on archival XMM-Newton data. The GC diffuse emission can be decomposed into three distinct components: the emission from low-luminosity point sources; the fluorescence of (and reflection from) dense molecular material; and soft (kT ~1 keV), diffuse thermal plasma emission most likely energised by supernova explosions. Here, we examine the emission due to unresolved point sources. We show that this source component accounts for the bulk of the 6.7-keV and 6.9-keV line emission. We fit the surface brightness distribution evident in these lines with an empirical 2-d model, which we then compare with a prediction derived from a 3-d mass model for the old stellar population in the GC region. We find that the X-ray surface brightness declines more rapidly with angular offset from Sgr A* than the mass-model prediction. One interpretation is that the X-ray luminosity per solar mass characterising the GC source population is increasing towards the GC. Alternatively, some refinement of the mass-distribution within the nuclear stellar disc may be required. The unresolved X-ray source population is most likely dominated by magnetic CVs. We use the X-ray observations to set constraints on the number density of such sources in the GC region. Our analysis does not support the premise that the GC is pervaded by very hot (~ 7.5 keV) thermal plasma, which is truly diffuse in nature.

Synchrotron X-ray diffraction study of the Ba{sub 1−x}SrSnO{sub 3} solid solution

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

Prodjosantoso, Anti K., E-mail: Prodjosantoso@yahoo.com; Zhou, Qingdi; Kennedy, Brendan J.

At room temperature the sequence of phases with increasing amounts of strontium in the stannate perovskite system Ba{sub 1−x}SrSnO{sub 3} has been established from high resolution synchrotron X-ray powder diffraction. The observed sequence orthorhombic (Pbnm), orthorhombic (Ibmm), tetragonal (I4/mcm), and cubic (Pm3-bar m) is a consequence of the sequential introduction of cooperative tilting of the corner sharing SnO{sub 6} octahedra. The cell volume changes smoothly across the series with no obvious discontinuities associated with the phase transitions. - Graphical abstract: Portions of the synchrotron X-ray diffraction profiles (λ=0.82453 Å) from selected Ba{sub 1−x}Sr{sub x}SnO{sub 3} samples together with the resultsmore » of fitting by the Rietveld method. Highlights: ► Structures of the stannate perovskites Ba{sub 1−x}SrSnO{sub 3} refined from synchrotron XRD. ► The sequence Pm3-bar m→I4/mcm→Ibmm→Pbnm results from tilting of the octahedra. ► The tilting maintains optimal bonding of the cations seen from the BVS analysis.« less

Report on the 18th International Conference on X-ray and Inner-Shell Processes (X99).

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

Gemmell, D. S.; Physics

2000-01-01

The 18th conference of the series served as a forum for discussing fundamental issues in the field of x-ray and inner-shell processes and their application in various disciplines of science and technology. Special emphasis was given to the opportunities offered by modern synchrotron x-ray sources. The program included plenary talks, progress reports and poster presentations relating to new developments in the field of x-ray and inner-shell processes. The range of topics included: X-ray interactions with atoms, molecules, clusters, surfaces and solids; Decay processes for inner-shell vacancies; X-ray absorption and emission spectroscopy - Photoionization processes; Phenomena associated with highly charged ionsmore » and collisions with energetic particles; Electron-spin and -momentum spectroscopy; X-ray scattering and spectroscopy in the study of magnetic systems; Applications in materials science, biology, geosciences, and other disciplines; Elastic and inelastic x-ray scattering processes in atoms and molecules; Threshold phenomena (post-collision interaction, resonant Raman processes, etc.); Nuclear absorption and scattering of x-rays; 'Fourth-generation' x-ray sources; Processes exploiting the polarization and coherence properties of x-ray beams; Developments in experimental techniques (x-ray optics, temporal techniques, detectors); Microscopy, spectromicroscopy, and various imaging techniques; Non-linear processes and x-ray lasers; Ionization and excitation induced by charged particles and by x-rays; and Exotic atoms (including 'hollow' atoms and atoms that contain 'exotic' particles).« less

Multistep modeling of protein structure: application towards refinement of tyr-tRNA synthetase

NASA Technical Reports Server (NTRS)

Srinivasan, S.; Shibata, M.; Roychoudhury, M.; Rein, R.

1987-01-01

The scope of multistep modeling (MSM) is expanding by adding a least-squares minimization step in the procedure to fit backbone reconstruction consistent with a set of C-alpha coordinates. The analytical solution of Phi and Psi angles, that fits a C-alpha x-ray coordinate is used for tyr-tRNA synthetase. Phi and Psi angles for the region where the above mentioned method fails, are obtained by minimizing the difference in C-alpha distances between the computed model and the crystal structure in a least-squares sense. We present a stepwise application of this part of MSM to the determination of the complete backbone geometry of the 321 N terminal residues of tyrosine tRNA synthetase to a root mean square deviation of 0.47 angstroms from the crystallographic C-alpha coordinates.

Current developments and tests of small x-ray optical systems for space applications

NASA Astrophysics Data System (ADS)

Pina, L.; Hudec, R.; Inneman, A.; Doubravová, D.; Marsikova, V.

2017-05-01

The paper addresses the X-ray monitoring for astrophysical applications. A novel approach based on the use of 1D and 2D "Lobster eye" optics in combination with Timepix X-ray detector in the energy range 3 - 40 keV was further studied. Wide-field optical system of this type has not been used in space yet. Designed wide-field optical system combined with Timepix X-ray detector is described together with latest experimental results obtained during laboratory tests. 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 the only solution in cases where intensity of impinging X-ray radiation is below the sensitivity of the detector, e.g. while monitoring astrophysical objects in space, or phenomena in the Earth's atmosphere. The optical system is considered to be used in a student rocket experiment.

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

Local structure in LaMnO3 and CaMnO3 perovskites: A quantitative structural refinement of Mn K -edge XANES data

NASA Astrophysics Data System (ADS)

Monesi, C.; Meneghini, C.; Bardelli, F.; Benfatto, M.; Mobilio, S.; Manju, U.; Sarma, D. D.

2005-11-01

Hole-doped perovskites such as La1-xCaxMnO3 present special magnetic and magnetotransport properties, and it is commonly accepted that the local atomic structure around Mn ions plays a crucial role in determining these peculiar features. Therefore experimental techniques directly probing the local atomic structure, like x-ray absorption spectroscopy (XAS), have been widely exploited to deeply understand the physics of these compounds. Quantitative XAS analysis usually concerns the extended region [extended x-ray absorption fine structure (EXAFS)] of the absorption spectra. The near-edge region [x-ray absorption near-edge spectroscopy (XANES)] of XAS spectra can provide detailed complementary information on the electronic structure and local atomic topology around the absorber. However, the complexity of the XANES analysis usually prevents a quantitative understanding of the data. This work exploits the recently developed MXAN code to achieve a quantitative structural refinement of the Mn K -edge XANES of LaMnO3 and CaMnO3 compounds; they are the end compounds of the doped manganite series LaxCa1-xMnO3 . The results derived from the EXAFS and XANES analyses are in good agreement, demonstrating that a quantitative picture of the local structure can be obtained from XANES in these crystalline compounds. Moreover, the quantitative XANES analysis provides topological information not directly achievable from EXAFS data analysis. This work demonstrates that combining the analysis of extended and near-edge regions of Mn K -edge XAS spectra could provide a complete and accurate description of Mn local atomic environment in these compounds.

X-ray microscopy with high-resolution zone plates: recent developments

NASA Astrophysics Data System (ADS)

Schneider, Gerd; Wilhein, Thomas; Niemann, Bastian; Guttman, P.; Schliebe, T.; Lehr, J.; Aschoff, H.; Thieme, Juergen; Rudolph, Dietbert M.; Schmahl, Guenther A.

1995-09-01

In order to expand the applications of x-ray microscopy, developments in the fields of zone plate technology, specimen preparation and imaging techniques have been made. A new cross- linked polymer chain electron beam resist allows us to record zone plate pattern down to 19 nm outermost zone width. High resolution zone plates in germanium with outermost zone widths down to 19 nm have been developed. In addition, phase zone plates in nickel down to 30 nm zone width have been made by electroplating. In order to enhance the image contrast for weak absorbing objects, the phase contrast method for x-ray microscopy was developed and implemented on the Gottingen x-ray microscope at BESSY. The effects of x ray absorption on the structure of biological specimen limits the maximum applicable radiation dose and therefore the achievable signal to noise ratio for an artifact-free x-ray image. To improve the stability especially of biological specimen, a cryogenic object chamber has been developed and tested. It turns out that at the operating temperature T less than or equal to 130 K unfixed biological specimen can be exposed to a radiation dose of 109 - 1010 Gy without any observable structural changes. A multiple-angle viewing stage allows us to take stereoscopic images with the x-ray microscope, giving a 3D-impression of the object. As an example for the applications of x-ray microscopy in biology, erythrocytes infected by malaria parasite have been examined. Studies of the aggregation of hematite by sodium sulfate gives an example for the application of x-ray microscopy in the field of colloid research.

Philip A. Parilla | NREL

Science.gov Websites

atomic layer deposition for applications. He also manages the majority of X-ray characterization equipment at NREL, specifically X-ray diffraction and X-ray fluorescence instrumentation. Additionally, he for EERE's Hydrogen Storage program. He is also an expert in X-ray diffraction and X-ray fluorescence

Template For Aiming An X-Ray Machine

NASA Technical Reports Server (NTRS)

Morphet, W. J.

1994-01-01

Relatively inexpensive template helps in aligning x-ray machine with phenolic ring to be inspected for flaws. Phenolic ring in original application part of rocket nozzle. Concept also applicable to x-ray inspection of other rings. Template contains alignment holes for adjusting orientation, plus target spot for adjusting lateral position, of laser spotting beam. (Laser spotting beam coincides with the x-ray beam, turned on later, after alignment completed.) Use of template decreases positioning time and error, providing consistent sensitivity for detection of flaws.

Application of MEMS-based x-ray optics as tuneable nanosecond choppers

NASA Astrophysics Data System (ADS)

Chen, Pice; Walko, Donald A.; Jung, Il Woong; Li, Zhilong; Gao, Ya; Shenoy, Gopal K.; Lopez, Daniel; Wang, Jin

2017-08-01

Time-resolved synchrotron x-ray measurements often rely on using a mechanical chopper to isolate a set of x-ray pulses. We have started the development of micro electromechanical systems (MEMS)-based x-ray optics, as an alternate method to manipulate x-ray beams. In the application of x-ray pulse isolation, we recently achieved a pulse-picking time window of half a nanosecond, which is more than 100 times faster than mechanical choppers can achieve. The MEMS device consists of a comb-drive silicon micromirror, designed for efficiently diffracting an x-ray beam during oscillation. The MEMS devices were operated in Bragg geometry and their oscillation was synchronized to x-ray pulses, with a frequency matching subharmonics of the cycling frequency of x-ray pulses. The microscale structure of the silicon mirror in terms of the curvature and the quality of crystallinity ensures a narrow angular spread of the Bragg reflection. With the discussion of factors determining the diffractive time window, this report showed our approaches to narrow down the time window to half a nanosecond. The short diffractive time window will allow us to select single x-ray pulse out of a train of pulses from synchrotron radiation facilities.

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.

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.

Inter-satellites x-ray communication system

NASA Astrophysics Data System (ADS)

Mou, Huan; Li, Bao-quan

2017-02-01

An inter-satellite X-ray communication system is presented in this paper. X-ray has a strong penetrating power without almost attenuation for transmission in outer space when the energy of X-ray photons is more than 10KeV and the atmospheric pressure is lower than 10-1 Pa, so it is convincing of x-ray communication in inter-satellite communication and deep space exploration. Additionally, using X-ray photons as information carriers can be used in some communication applications that laser communication and radio frequency (RF) communication are not available, such as ionization blackout area communication. The inter-satellites X-ray communication system, including the grid modulated X-ray source, the high-sensitivity X-ray detector and the transmitting and receiving antenna, is described explicitly. As the X-ray transmitter, a vacuum-sealed miniature modulated X-ray source has been fabricated via the single-step brazing process in a vacuum furnace. Pulse modulation of X-rays, by means of controlling the voltage value of the grid electrode, is realized. Three focusing electrodes, meanwhile, are used to make the electron beam converge and finally 150μm focusing spot diameter is obtained. The X-ray detector based on silicon avalanche photodiodes (APDs) is chosen as the communication receiver on account of its high temporal resolution and non-vacuum operating environment. Furthermore, considering x-ray emission characteristic and communication distance of X-rays, the multilayer nested rotary parabolic optics is picked out as transmitting and receiving antenna. And as a new concept of the space communication, there will be more important scientific significance and application prospects, called "Next-Generation Communications".

A case for ZnO nanowire field emitter arrays in advanced x-ray source applications

NASA Astrophysics Data System (ADS)

Robinson, Vance S.; Bergkvist, Magnus; Chen, Daokun; Chen, Jun; Huang, Mengbing

2016-09-01

Reviewing current efforts in X-ray source miniaturization reveals a broad spectrum of applications: Portable and/or remote nondestructive evaluation, high throughput protein crystallography, invasive radiotherapy, monitoring fluid flow and particulate generation in situ, and portable radiography devices for battle-front or large scale disaster triage scenarios. For the most part, all of these applications are being addressed with a top-down approach aimed at improving portability, weight and size. That is, the existing system or a critical sub-component is shrunk in some manner in order to miniaturize the overall package. In parallel to top-down x-ray source miniaturization, more recent efforts leverage field emission and semiconductor device fabrication techniques to achieve small scale x-ray sources via a bottom-up approach where phenomena effective at a micro/nanoscale are coordinated for macro-scale effect. The bottom-up approach holds potential to address all the applications previously mentioned but its entitlement extends into new applications with much more ground-breaking potential. One such bottom-up application is the distributed x-ray source platform. In the medical space, using an array of microscale x-ray sources instead of a single source promises significant reductions in patient dose as well as smaller feature detectability and fewer image artifacts. Cold cathode field emitters are ideal for this application because they can be gated electrostatically or via photonic excitation, they do not generate excessive heat like other common electron emitters, they have higher brightness and they are relatively compact. This document describes how ZnO nanowire field emitter arrays are well suited for distributed x-ray source applications because they hold promise in each of the following critical areas: emission stability, simple scalable fabrication, performance, radiation resistance and photonic coupling.

Novel visualization studies of lignocellulosic oxidation chemistry by application of C-near edge X-ray absorption fine structure spectroscopy

Treesearch

Douglas G. Mancosky; Lucian A. Lucia; Hiroki Nanko; Sue Wirick; Alan W. Rudie; Robert Braun

2005-01-01

The research presented herein is the first attempt to probe the chemical nature of lignocellulosic samples by the application of carbon near edge X-ray absorption fine structure spectroscopy (C-NEXAFS). C-NEXAFS is a soft X-ray technique that principally provides selective interrogation of discrete atomic moieties using photoelectrons of variable energies. The X1A beam...

Development and Applications Of Photosensitive Device Systems To Studies Of Biological And Organic Materials

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

Gruner, Sol

2012-01-20

The primary focus of the grant is the development of new x-ray detectors for biological and materials work at synchrotron sources, especially Pixel Array Detectors (PADs), and the training of students via research applications to problems in biophysics and materials science using novel x-ray methods. This Final Progress Report provides a high-level overview of the most important accomplishments. These major areas of accomplishment include: (1) Development and application of x-ray Pixel Array Detectors; (2) Development and application of methods of high pressure x-ray crystallography as applied to proteins; (3) Studies on the synthesis and structure of novel mesophase materials derivedmore » from block co-polymers.« less

Design of a normal incidence multilayer imaging X-ray microscope

NASA Astrophysics Data System (ADS)

Shealy, David L.; Gabardi, David R.; Hoover, Richard B.; Walker, Arthur B. C., Jr.; Lindblom, Joakim F.

Normal incidence multilayer Cassegrain X-ray telescopes were flown on the Stanford/MSFC Rocket X-ray Spectroheliograph. These instruments produced high spatial resolution images of the sun and conclusively demonstrated that doubly reflecting multilayer X-ray optical systems are feasible. The images indicated that aplanatic imaging soft X-ray/EUV microscopes should be achievable using multilayer optics technology. A doubly reflecting normal incidence multilayer imaging X-ray microscope based on the Schwarzschild configuration has been designed. The design of the microscope and the results of the optical system ray trace analysis are discussed. High resolution aplanatic imaging X-ray microscopes using normal incidence multilayer X-ray mirrors should have many important applications in advanced X-ray astronomical instrumentation, X-ray lithography, biological, biomedical, metallurgical, and laser fusion research.

NMRe: a web server for NMR protein structure refinement with high-quality structure validation scores.

PubMed

Ryu, Hyojung; Lim, GyuTae; Sung, Bong Hyun; Lee, Jinhyuk

2016-02-15

Protein structure refinement is a necessary step for the study of protein function. In particular, some nuclear magnetic resonance (NMR) structures are of lower quality than X-ray crystallographic structures. Here, we present NMRe, a web-based server for NMR structure refinement. The previously developed knowledge-based energy function STAP (Statistical Torsion Angle Potential) was used for NMRe refinement. With STAP, NMRe provides two refinement protocols using two types of distance restraints. If a user provides NOE (Nuclear Overhauser Effect) data, the refinement is performed with the NOE distance restraints as a conventional NMR structure refinement. Additionally, NMRe generates NOE-like distance restraints based on the inter-hydrogen distances derived from the input structure. The efficiency of NMRe refinement was validated on 20 NMR structures. Most of the quality assessment scores of the refined NMR structures were better than those of the original structures. The refinement results are provided as a three-dimensional structure view, a secondary structure scheme, and numerical and graphical structure validation scores. NMRe is available at http://psb.kobic.re.kr/nmre/. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com.

X-Ray Lasers

ERIC Educational Resources Information Center

Chapline, George; Wood, Lowell

1975-01-01

Outlines the prospects of generating coherent x rays using high-power lasers and indentifies problem areas in their development. Indicates possible applications for coherent x rays in the fields of chemistry, biology, and crystallography. (GS)

DFT energy optimization of a large carbohydrate: cyclomaltohexaicosaose (CA-26)

USDA-ARS?s Scientific Manuscript database

CA-26 is the largest cyclodextrin (546 atoms) for which refined X-ray structural data is available. Because of its size, 26 D-glucose residues, it is beyond the scope of study of most ab initio or density functional methods, and to date has only been computationally examined using empirical force fi...

A combined temperature-dependent electron and single-crystal X-ray diffraction study of the fresnoite compound Rb 2V 4+V 25+O 8

NASA Astrophysics Data System (ADS)

Withers, Ray L.; Höche, Thomas; Liu, Yun; Esmaeilzadeh, Saeid; Keding, Ralf; Sales, Brian

2004-10-01

High-purity Rb2V3O8 has been grown and temperature-dependent electron and single-crystal X-ray diffraction used to carefully investigate its fresnoite-type reciprocal lattice. In contrast to other recently investigated representatives of the fresnoite family of compounds, Rb2V3O8 is not incommensurately modulated with an incommensurate basal plane primary modulation wave vector given by q∼0.3 <110>*. A careful low-temperature electron diffraction study has, however, revealed the existence of weak incommensurate satellite reflections characterized by the primitive primary modulation wave vector q1∼0.16c*. The reciprocal space positioning of these incommensurate satellite reflections, the overall (3+1)-d superspace group symmetry, as well as the shapes of the refined displacement ellipsoids determined from single-crystal XRD refinement, are all consistent with their arising from a distinct type of condensed rigid unit modes (RUMs) of distortion of the Rb2V3O8 parent structure.

Recent developments of x-ray lithography in Canada

NASA Astrophysics Data System (ADS)

Chaker, Mohamed; Boily, Stephane; Ginovker, A.; Jean, Alain; Kieffer, Jean-Claude; Mercier, P. P.; Pepin, Henri; Leung, Pak; Currie, John F.; Lafontaine, Hugues

1991-08-01

An overview of current activities in Canada is reported, including x-ray lithography studies based on laser plasma sources and x-ray mask development. In particular, the application of laser plasma sources for x-ray lithography is discussed, taking into account the industrial requirement and the present state of laser technology. The authors describe the development of silicon carbide membranes for x-ray lithography application. SiC films were prepared using either a 100 kHz plasma-enhanced chemical vapor deposition (PECVD) system or a laser ablation technique. These membranes have a relatively large diameter (> 1 in.) and a high optical transparency (> 50%). Experimental studies on stresses in tungsten films deposited with triode sputtering are reported.

NMR crystallography of α-poly(L-lactide).

PubMed

Pawlak, Tomasz; Jaworska, Magdalena; Potrzebowski, Marek J

2013-03-07

A complementary approach that combines NMR measurements, analysis of X-ray and neutron powder diffraction data and advanced quantum mechanical calculations was employed to study the α-polymorph of L-polylactide. Such a strategy, which is known as NMR crystallography, to the best of our knowledge, is used here for the first time for the fine refinement of the crystal structure of a synthetic polymer. The GIPAW method was used to compute the NMR shielding parameters for the different models, which included the α-PLLA structure obtained by 2-dimensional wide-angle X-ray diffraction (WAXD) at -150 °C (model M1) and at 25 °C (model M2), neutron diffraction (WAND) measurements (model M3) and the fully optimized geometry of the PLLA chains in the unit cell with defined size (model M4). The influence of changes in the chain conformation on the (13)C σ(ii) NMR shielding parameters is shown. The correlation between the σ(ii) and δ(ii) values for the M1-M4 models revealed that the M4 model provided the best fit. Moreover, a comparison of the experimental (13)C NMR spectra with the spectra calculated using the M1-M4 models strongly supports the data for the M4 model. The GIPAW method, via verification using NMR measurements, was shown to be capable of the fine refinement of the crystal structures of polymers when coarse X-ray diffraction data for powdered samples are available.

Technological aspects of GEM detector design and assembling for soft x-ray application

NASA Astrophysics Data System (ADS)

Kowalska-Strzeciwilk, E.; Chernyshova, M.

2016-09-01

Various types of Micro Pattern Gas Detectors (MPGDs) found applications as tracking detectors in high energy particle physics experiments and as well as imaging detectors, especially for soft X-rays. These detectors offer several advantages like high count rate capability, good spatial and energy resolution, low cost and possibility of constructing large area detectors with very small dead area. Construction, like the triple Gas Electron Multiplier (GEM) detector has become a standard detector, which is widely used for different imaging applications. Some examples of such applications are: monitoring the impurity in plasma, imaging system for mapping of some parameters like pigment distributions using X-ray fluorescence technique[1], proton range radiography system for quality assurance in hadron therapy. Measuring of the Soft X-Ray (SXR) radiation of magnetic fusion plasma is a standard way of accessing valuable information, for example, about particle transport and MHD. The paper is focused on the design of GEM based soft Xray radiation detecting system which is under development. It is dedicated to study soft X-ray emission of plasma radiation with focus on tungsten emission lines energy region. The paper presents the designing, construction and assembling of a prototype of two triple-GEM detectors for soft-X ray application on the WEST device.

Multilayer and grazing incidence X-ray/EUV optics; Proceedings of the Meeting, San Diego, CA, July 22-24, 1991

NASA Technical Reports Server (NTRS)

Hoover, Richard B. (Editor)

1992-01-01

The present conference discusses the Advanced X-ray Astrophysics Facility (AXAF) calibration by means of synchrotron radiation and its X-ray reflectivity, X-ray scattering measurements from thin-foil X-ray mirrors, lobster-eye X-ray optics using microchannel plates, space-based interferometry at EUV and soft X-ray wavelengths, a water-window imaging X-ray telescope, a graded d-spacing multilayer telescope for high energy X-ray astronomy, photographic films for the multispectral solar telescope array, a soft X-ray ion chamber, and the development of hard X-ray optics. Also discussed are X-ray spectroscopy with multilayered optics, a slit aperture for monitoring X-ray experiments, an objective double-crystal spectrometer, a Ly-alpha coronagraph/polarimeter, tungsten/boron nitride multilayers for XUV optical applications, the evaluation of reflectors for soft X-ray optics, the manufacture of elastically bent crystals and multilayer mirrors, and selective photodevices for the VUV.

Comparison of corrosion behavior between coarse grained and nano/ultrafine grained alloy 690

NASA Astrophysics Data System (ADS)

Jinlong, Lv; Tongxiang, Liang; Chen, Wang; Ting, Guo

2016-01-01

The effect of grain refinement on corrosion resistance of alloy 690 was investigated. The electron work function value of coarse grained alloy 690 was higher than that of nano/ultrafine grained one. The grain refinement reduced the electron work function of alloy 690. The passive films formed on coarse grained and nano/ultrafine grained alloy 690 in borate buffer solution were studied by potentiodynamic curves and electrochemical impedance spectroscopy and X-ray photoelectron spectroscopy. The results showed that the grain refinement improved corrosion resistance of alloy 690. This was attributed to the fact that grain refinement promoted the enrichment of Cr2O3 and inhibited Cr(OH)3 in the passive film. More Cr2O3 in passive film could significantly improve the corrosion resistance of the nano/ultrafine grained alloy 690.

X-ray and neutron interrogation of air cargo for mobile applications

NASA Astrophysics Data System (ADS)

Van Liew, Seth

2015-06-01

A system for scanning break-bulk cargo for mobile applications is presented. This combines a 140 kV multi-view, multi-energy X-ray system with 2.5 MeV neutrons. The system uses dual energy X-ray radiography with neutron radiography. The X-ray and neutron systems were designed to be collocated in a mobile environment. Various materials were interrogated with the intent of distinguishing threat materials such as explosives from similar benign materials. In particular, the identification of threats and bengins with nearly identical effective atomic numbers has been demonstrated.

X-Ray Backscatter Imaging for Aerospace Applications

NASA Astrophysics Data System (ADS)

Shedlock, Daniel; Edwards, Talion; Toh, Chin

2011-06-01

Scatter x-ray imaging (SXI) is a real time, digital, x-ray backscatter imaging technique that allows radiographs to be taken from one side of an object. This x-ray backscatter imaging technique offers many advantages over conventional transmission radiography that include single-sided access and extremely low radiation fields compared to conventional open source industrial radiography. Examples of some applications include the detection of corrosion, foreign object debris, water intrusion, cracking, impact damage and leak detection in a variety of material such as aluminum, composites, honeycomb structures, and titanium.

On the viability of exploiting L-shell fluorescence for X-ray polarimetry

NASA Technical Reports Server (NTRS)

Weisskopf, M. C.; Sutherland, P. G.; Elsner, R. F.; Ramsey, B. D.

1985-01-01

It has been suggested that one may build an X-ray polarimeter by exploiting the polarization dependence of the angular distribution of L-shell fluorescence photons. In this paper the sensitivity of this approach to polarimetry is examined theoretically. The calculations are applied to several detection schemes using imaging proportional counters that would have direct application in X-ray astronomy. It is found, however, that the sensitivity of this method for measuring X-ray polarization is too low to be of use for other than laboratory applications.

Feasibility studies on explosive detection and homeland security applications using a neutron and x-ray combined computed tomography system

NASA Astrophysics Data System (ADS)

Sinha, V.; Srivastava, A.; Lee, H. K.; Liu, X.

2013-05-01

The successful creation and operation of a neutron and X-ray combined computed tomography (NXCT) system has been demonstrated by researchers at the Missouri University of Science and Technology. The NXCT system has numerous applications in the field of material characterization and object identification in materials with a mixture of atomic numbers represented. Presently, the feasibility studies have been performed for explosive detection and homeland security applications, particularly in concealed material detection and determination of the light atomic number materials. These materials cannot be detected using traditional X-ray imaging. The new system has the capability to provide complete structural and compositional information due to the complementary nature of X-ray and neutron interactions with materials. The design of the NXCT system facilitates simultaneous and instantaneous imaging operation, promising enhanced detection capabilities of explosive materials, low atomic number materials and illicit materials for homeland security applications. In addition, a sample positioning system allowing the user to remotely and automatically manipulate the sample makes the system viable for commercial applications. Several explosives and weapon simulants have been imaged and the results are provided. The fusion algorithms which combine the data from the neutron and X-ray imaging produce superior images. This paper is a compete overview of the NXCT system for feasibility studies of explosive detection and homeland security applications. The design of the system, operation, algorithm development, and detection schemes are provided. This is the first combined neutron and X-ray computed tomography system in operation. Furthermore, the method of fusing neutron and X-ray images together is a new approach which provides high contrast images of the desired object. The system could serve as a standardized tool in nondestructive testing of many applications, especially in explosives detection and homeland security research.

On the Use of Dynamical Diffraction Theory To Refine Crystal Structure from Electron Diffraction Data: Application to KLa5O5(VO4)2, a Material with Promising Luminescent Properties.

PubMed

Colmont, Marie; Palatinus, Lukas; Huvé, Marielle; Kabbour, Houria; Saitzek, Sébastien; Djelal, Nora; Roussel, Pascal

2016-03-07

A new lanthanum oxide, KLa5O5(VO4)2, was synthesized using a flux growth technique that involved solid-state reaction under an air atmosphere at 900 °C. The crystal structure was solved and refined using an innovative approach recently established and based on three-dimensional (3D) electron diffraction data, using precession of the electron beam and then validated against Rietveld refinement and denisty functional theory (DFT) calculations. It crystallizes in a monoclinic unit cell with space group C2/m and has unit cell parameters of a = 20.2282(14) Å, b = 5.8639(4) Å, c = 12.6060(9) Å, and β = 117.64(1)°. Its structure is built on Cresnel-like two-dimensional (2D) units (La5O5) of 4*3 (OLa4) tetrahedra, which run parallel to (001) plane, being surrounded by isolated VO4 tetrahedra. Four isolated vanadate groups create channels that host K(+) ions. Substitution of K(+) cations by another alkali metal is possible, going from lithium to rubidium. Li substitution led to a similar phase with a primitive monoclinic unit cell. A complementary selected area electron diffraction (SAED) study highlighted diffuse streaks associated with stacking faults observed on high-resolution electron microscopy (HREM) images of the lithium compound. Finally, preliminary catalytic tests for ethanol oxidation are reported, as well as luminescence evidence. This paper also describes how solid-state chemists can take advantages of recent progresses in electron crystallography, assisted by DFT calculations and powder X-ray diffraction (PXRD) refinements, to propose new structural types with potential applications to the physicist community.

Magnetism in La{sub 0.7}Sr{sub 0.3}Mn{sub 1-x}Co{sub x}O{sub 3} (0 ≤ x ≤ 1)

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

Kumar, Ashutosh, E-mail: ashutosh.pph13@iitp.ac.in; Sharma, Himanshu; Tomy, C. V.

2016-05-23

We study the structural and magnetic properties of La{sub 0.7}Sr{sub 0.3}Mn{sub 1-x}Co{sub x}O{sub 3} (0 ≤ x ≤ 1). Rietveld refinement of X-ray Diffraction (XRD) pattern suggests phase purity of the polycrystalline samples with R-3c space group. Interplay of Ferromagnetic (FM) and Antiferromagnetic (AFM) interaction upon Co substitution at Mn site in La{sub 0.7}Sr{sub 0.3}MnO{sub 3} is evident from magnetic measurements. There is an optimal cobalt substitution at which the coercive field is maximum.

Potential application of X-ray communication through a plasma sheath encountered during spacecraft reentry into earth's atmosphere

NASA Astrophysics Data System (ADS)

Li, Huan; Tang, Xiaobin; Hang, Shuang; Liu, Yunpeng; Chen, Da

2017-03-01

Rapid progress in exploiting X-ray science has fueled its potential application in communication networks as a carrier wave for transmitting information through a plasma sheath during spacecraft reentry into earth's atmosphere. In this study, we addressed the physical transmission process of X-rays in the reentry plasma sheath and near-earth space theoretically. The interactions between the X-rays and reentry plasma sheath were investigated through the theoretical Wentzel-Kramers-Brillouin method, and the Monte Carlo simulation was employed to explore the transmission properties of X-rays in the near-earth space. The simulation results indicated that X-ray transmission was not influenced by the reentry plasma sheath compared with regular RF signals, and adopting various X-ray energies according to different spacecraft reentry altitudes is imperative when using X-ray uplink communication especially in the near-earth space. Additionally, the performance of the X-ray communication system was evaluated by applying the additive white Gaussian noise, Rayleigh fading channel, and plasma sheath channel. The Doppler shift, as a result of spacecraft velocity changes, was also calculated through the Matlab Simulink simulation, and various plasma sheath environments have no significant influence on X-ray communication owing to its exceedingly high carrier frequency.

Diagnostic X-ray sources-present and future

NASA Astrophysics Data System (ADS)

Behling, Rolf; Grüner, Florian

2018-01-01

This paper compares very different physical principles of X-ray production to spur ideation. Since more than 120 years, bremsstrahlung from X-ray tubes has been the workhorse of medical diagnostics. Generated by X-ray segments comprised of X-ray tubes and high-voltage generators in the various medical systems, X-ray photons in the spectral range between about 16 keV and 150 keV deliver information about anatomy and function of human patients and in pre-clinical animal studies. Despite of strides to employ the wave nature of X-rays as phase sensitive means, commercial diagnostic X-ray systems available until the time of writing still rely exclusively on measuring the attenuation and scattering of X-rays by matter. Significant activities in research aim at building highly brilliant short pulse X-ray sources, based on e.g. synchrotron radiation, free electron lasers and/or laser wake-field acceleration of electrons followed by wiggling with magnetic structures or Thomson scattering in bunches of light. While both approaches, non-brilliant and brilliant sources, have different scope of application, we speculate that a combination may expand the efficacy in medical application. At this point, however, severe technical and commercial difficulties hinder closing this gap. This article may inspire further development and spark innovation in this important field.

Motionless phase stepping in X-ray phase contrast imaging with a compact source

PubMed Central

Miao, Houxun; Chen, Lei; Bennett, Eric E.; Adamo, Nick M.; Gomella, Andrew A.; DeLuca, Alexa M.; Patel, Ajay; Morgan, Nicole Y.; Wen, Han

2013-01-01

X-ray phase contrast imaging offers a way to visualize the internal structures of an object without the need to deposit significant radiation, and thereby alleviate the main concern in X-ray diagnostic imaging procedures today. Grating-based differential phase contrast imaging techniques are compatible with compact X-ray sources, which is a key requirement for the majority of clinical X-ray modalities. However, these methods are substantially limited by the need for mechanical phase stepping. We describe an electromagnetic phase-stepping method that eliminates mechanical motion, thus removing the constraints in speed, accuracy, and flexibility. The method is broadly applicable to both projection and tomography imaging modes. The transition from mechanical to electromagnetic scanning should greatly facilitate the translation of X-ray phase contrast techniques into mainstream applications. PMID:24218599

Development of a Carbon Nanotube-Based Micro-CT and its Applications in Preclinical Research

NASA Astrophysics Data System (ADS)

Burk, Laurel May

Due to the dependence of researchers on mouse models for the study of human disease, diagnostic tools available in the clinic must be modified for use on these much smaller subjects. In addition to high spatial resolution, cardiac and lung imaging of mice presents extreme temporal challenges, and physiological gating methods must be developed in order to image these organs without motion blur. Commercially available micro-CT imaging devices are equipped with conventional thermionic x-ray sources and have a limited temporal response and are not ideal for in vivo small animal studies. Recent development of a field-emission x-ray source with carbon nanotube (CNT) cathode in our lab presented the opportunity to create a micro-CT device well-suited for in vivo lung and cardiac imaging of murine models for human disease. The goal of this thesis work was to present such a device, to develop and refine protocols which allow high resolution in vivo imaging of free-breathing mice, and to demonstrate the use of this new imaging tool for the study many different disease models. In Chapter 1, I provide background information about x-rays, CT imaging, and small animal micro-CT. In Chapter 2, CNT-based x-ray sources are explained, and details of a micro-focus x-ray tube specialized for micro-CT imaging are presented. In Chapter 3, the first and second generation CNT micro-CT devices are characterized, and successful respiratory- and cardiac-gated live animal imaging on normal, wild-type mice is achieved. In Chapter 4, respiratory-gated imaging of mouse disease models is demonstrated, limitations to the method are discussed, and a new contactless respiration sensor is presented which addresses many of these limitations. In Chapter 5, cardiac-gated imaging of disease models is demonstrated, including studies of aortic calcification, left ventricular hypertrophy, and myocardial infarction. In Chapter 6, several methods for image and system improvement are explored, and radiation therapy-related micro-CT imaging is present. Finally, in Chapter 7 I discuss future directions for this research and for the CNT micro-CT.

Dose-rate plays a significant role in synchrotron radiation X-ray-induced damage of rodent testes.

PubMed

Chen, Heyu; Wang, Ban; Wang, Caixia; Cao, Wei; Zhang, Jie; Ma, Yingxin; Hong, Yunyi; Fu, Shen; Wu, Fan; Ying, Weihai

2016-01-01

Synchrotron radiation (SR) X-ray has significant potential for applications in medical imaging and cancer treatment. However, the mechanisms underlying SR X-ray-induced tissue damage remain unclear. Previous studies on regular X-ray-induced tissue damage have suggested that dose-rate could affect radiation damage. Because SR X-ray has exceedingly high dose-rate compared to regular X-ray, it remains to be determined if dose-rate may affect SR X-ray-induced tissue damage. We used rodent testes as a model to investigate the role of dose-rate in SR X-ray-induced tissue damage. One day after SR X-ray irradiation, we determined the effects of the irradiation of the same dosage at two different dose-rates, 0.11 Gy/s and 1.1 Gy/s, on TUNEL signals, caspase-3 activation and DNA double-strand breaks (DSBs) of the testes. Compared to those produced by the irradiation at 0.11 Gy/s, irradiation at 1.1 Gy/s produced higher levels of DSBs, TUNEL signals, and caspase-3 activation in the testes. Our study has provided the first evidence suggesting that dose-rate could be a significant factor in SR X-ray-induced tissue damage, which may establish a valuable base for utilizing this factor to manipulate the tissue damage in SR X-ray-based medical applications.

Dose-rate plays a significant role in synchrotron radiation X-ray-induced damage of rodent testes

PubMed Central

Chen, Heyu; Wang, Ban; Wang, Caixia; Cao, Wei; Zhang, Jie; Ma, Yingxin; Hong, Yunyi; Fu, Shen; Wu, Fan; Ying, Weihai

2016-01-01

Synchrotron radiation (SR) X-ray has significant potential for applications in medical imaging and cancer treatment. However, the mechanisms underlying SR X-ray-induced tissue damage remain unclear. Previous studies on regular X-ray-induced tissue damage have suggested that dose-rate could affect radiation damage. Because SR X-ray has exceedingly high dose-rate compared to regular X-ray, it remains to be determined if dose-rate may affect SR X-ray-induced tissue damage. We used rodent testes as a model to investigate the role of dose-rate in SR X-ray-induced tissue damage. One day after SR X-ray irradiation, we determined the effects of the irradiation of the same dosage at two different dose-rates, 0.11 Gy/s and 1.1 Gy/s, on TUNEL signals, caspase-3 activation and DNA double-strand breaks (DSBs) of the testes. Compared to those produced by the irradiation at 0.11 Gy/s, irradiation at 1.1 Gy/s produced higher levels of DSBs, TUNEL signals, and caspase-3 activation in the testes. Our study has provided the first evidence suggesting that dose-rate could be a significant factor in SR X-ray-induced tissue damage, which may establish a valuable base for utilizing this factor to manipulate the tissue damage in SR X-ray-based medical applications. PMID:28078052

Synchrotron applications in wood preservation and deterioration

Treesearch

Barbara L. Illman

2003-01-01

Several non-intrusive synchrotron techniques are being used to detect and study wood decay. The techniques use high intensity synchrotron-generated X-rays to determine the atomic structure of materials with imaging, diffraction, and absorption. Some of the techniques are X-ray absorption near edge structure (XANES), X-ray fluorescence spectroscopy (XFS), X-ray...

Electronic structure of lead pyrophosphate

NASA Astrophysics Data System (ADS)

Suewattana, Malliga; Singh, David

2007-03-01

Lead Pyrophosphate Pb2P2O7 is of interest for potential radiation detection applications and use in long term waste storage. It forms in triclinic P1 crystals and can also be grown as glasses. We performed electronic structure calculations using the crystal structure which determined by Mullica et. al (J. Solid State Chem (1986)) using x-ray diffraction and found large forces on atoms suggesting that the refined atomic positions were not fully correct. Here we report first principles structure relaxation and a revised crystal structure for this compound. We analyze the resulting structure using pair distribution functions and discuss the implications for the electronic properties. This work was supported by DOE NA22 and the Office of Naval Research.

Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal

NASA Astrophysics Data System (ADS)

Kalita, Patricia; Specht, Paul; Root, Seth; Sinclair, Nicholas; Schuman, Adam; White, Melanie; Cornelius, Andrew L.; Smith, Jesse; Sinogeikin, Stanislav

2017-12-01

We report real-time observations of a phase transition in the ionic solid CaF2 , a model A B2 structure in high-pressure physics. Synchrotron x-ray diffraction coupled with dynamic loading to 27.7 GPa, and separately with static compression, follows, in situ, the fluorite to cotunnite structural phase transition, both on nanosecond and on minute time scales. Using Rietveld refinement techniques, we examine the kinetics and hysteresis of the transition. Our results give insight into the kinetic time scale of the fluorite-cotunnite phase transition under shock compression, which is relevant to a number of isomorphic compounds.

Crystal nucleation in metallic alloys using x-ray radiography and machine learning

PubMed Central

Arteta, Carlos; Lempitsky, Victor

2018-01-01

The crystallization of solidifying Al-Cu alloys over a wide range of conditions was studied in situ by synchrotron x-ray radiography, and the data were analyzed using a computer vision algorithm trained using machine learning. The effect of cooling rate and solute concentration on nucleation undercooling, crystal formation rate, and crystal growth rate was measured automatically for thousands of separate crystals, which was impossible to achieve manually. Nucleation undercooling distributions confirmed the efficiency of extrinsic grain refiners and gave support to the widely assumed free growth model of heterogeneous nucleation. We show that crystallization occurred in temporal and spatial bursts associated with a solute-suppressed nucleation zone. PMID:29662954

Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal

DOE PAGES

Kalita, Patricia E.; Specht, Paul Elliot; Root, Seth; ...

2017-12-21

Here, we report real-time observations of a phase transition in the ionic solid CaF 2, a model AB 2 structure in high-pressure physics. Synchrotron x-ray diffraction coupled with dynamic loading to 27.7 GPa, and separately with static compression, follows, in situ, the fluorite to cotunnite structural phase transition, both on nanosecond and on minute time scales. Using Rietveld refinement techniques, we examine the kinetics and hysteresis of the transition. Our results give insight into the kinetic time scale of the fluorite-cotunnite phase transition under shock compression, which is relevant to a number of isomorphic compounds.

Simulating 3D Stellar Winds and Diffuse X-ray Emissions from Gases in Non-equilibrium Ionization State

NASA Astrophysics Data System (ADS)

Long, Min; Sun, Wei; Niu, Shu; Zhou, Xin; Ji, Li

2017-08-01

We investigate the physical properties of stellar winds launched in super stellar clusters (SSCs). Chandra observations have detected the presence of diffuse X-ray emission caused by hot gas from such winds in SSCs, and provide the best probe for understanding interactions between the stellar winds and the complex nursery regions. However, the details of the origin of cluster winds, the mass and energy ejection, the formation of diffuse X-ray emission, the fraction of winds contribution to the distribution of diffuse X-ray emission still remain unclear. We developed a multiphysics hydrodynamic model including self-gravity, head conduction and performed 3D simulations with an unprecedented grid resolution due to adaptive mesh refinement (AMR) capability in a case study of NGC 3603, as a supplement to the analysis of the archived 500 ks Chandra observations. The synthetic emission will be computed by assuming the gas in a non-equilibrium ionization (NEI) state indicated by Chandra observation, not coronal ionization equilibrium (CIE) that most works assumed, by using a customized NEI calculation module based on AtomDB. The results will be compared to the Chandra observations.

Indirect X-ray Detectors Based on Inkjet-Printed Photodetectors with a Screen-Printed Scintillator Layer.

PubMed

Oliveira, Juliana; Correia, Vitor; Sowade, Enrico; Etxebarria, Ikerne; Rodriguez, Raul D; Mitra, Kalyan Y; Baumann, Reinhard R; Lanceros-Mendez, Senentxu

2018-04-18

Organic photodetectors (PDs) based on printing technologies will allow to expand the current field of PD applications toward large-area and flexible applications in areas such as medical imaging, security, and quality control, among others. Inkjet printing is a powerful digital tool for the deposition of smart and functional materials on various substrates, allowing the development of electronic devices such as PDs on various substrates. In this work, inkjet-printed PD arrays, based on the organic thin-film transistor architecture, have been developed and applied for the indirect detection of X-ray radiation using a scintillator ink as an X-ray absorber. The >90% increase of the photocurrent of the PDs under X-ray radiation, from about 53 nA without the scintillator film to about 102 nA with the scintillator located on top of the PD, proves the suitability of the developed printed device for X-ray detection applications.

Enhancing resolution in coherent x-ray diffraction imaging.

PubMed

Noh, Do Young; Kim, Chan; Kim, Yoonhee; Song, Changyong

2016-12-14

Achieving a resolution near 1 nm is a critical issue in coherent x-ray diffraction imaging (CDI) for applications in materials and biology. Albeit with various advantages of CDI based on synchrotrons and newly developed x-ray free electron lasers, its applications would be limited without improving resolution well below 10 nm. Here, we review the issues and efforts in improving CDI resolution including various methods for resolution determination. Enhancing diffraction signal at large diffraction angles, with the aid of interference between neighboring strong scatterers or templates, is reviewed and discussed in terms of increasing signal-to-noise ratio. In addition, we discuss errors in image reconstruction algorithms-caused by the discreteness of the Fourier transformations involved-which degrade the spatial resolution, and suggest ways to correct them. We expect this review to be useful for applications of CDI in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

Simultaneous K-edge subtraction tomography for tracing strontium using parametric X-ray radiation

NASA Astrophysics Data System (ADS)

Hayakawa, Y.; Hayakawa, K.; Kaneda, T.; Nogami, K.; Sakae, T.; Sakai, T.; Sato, I.; Takahashi, Y.; Tanaka, T.

2017-07-01

The X-ray source based on parametric X-ray radiation (PXR) has been regularly providing a coherent X-ray beam for application studies at Nihon University. Recently, three dimensional (3D) computed tomography (CT) has become one of the most important applications of the PXR source. The methodology referred to as K-edge subtraction (KES) imaging is a particularly successful application utilizing the energy selectivity of PXR. In order to demonstrate the applicability of PXR-KES, a simultaneous KES experiment for a specimen containing strontium was performed using a PXR beam having an energy near the Sr K-edge of 16.1 keV. As a result, the 3D distribution of Sr was obtained by subtraction between the two simultaneously acquired tomographic images.

Evaluation of corrosion products formed by sulfidation as inhibitors of the naphthenic corrosion of AISI-316 steel

NASA Astrophysics Data System (ADS)

Sanabria-Cala, J. A.; Montañez, N. D.; Laverde Cataño, D.; Y Peña Ballesteros, D.; Mejía, C. A.

2017-12-01

Naphthenic acids present in oil from most regions worldwide currently stand as the main responsible for the naphthenic corrosion problems, affecting the oil-refining industry. The phenomenon of sulfidation, accompanying corrosion processes brought about by naphthenic acids in high-temperature refining plant applications, takes place when the combination of sulfidic acid (H2S) with Fe forms layers of iron sulphide (FeS) on the material surface, layers with the potential to protect the material from attack by other corrosive species like naphthenic acids. This work assessed corrosion products formed by sulfidation as inhibitors of naphthenic corrosion rate in AISI-316 steel exposed to processing conditions of simulated crude oil in a dynamic autoclave. Calculation of the sulfidation and naphthenic corrosion rates were determined by gravimetry. The surfaces of the AISI-316 gravimetric coupons exposed to acid systems; were characterized morphologically by X-Ray Diffraction (XRD) and X-ray Fluorescence by Energy Dispersive Spectroscopy (EDS) combined with Scanning Electron Microscopy (SEM). One of the results obtained was the determination of an inhibiting effect of corrosion products at 250 and 300°C, where lower corrosion rate levels were detected. For the temperature of 350°C, naphthenic corrosion rates increased due to deposition of naphthenic acids on the areas where corrosion products formed by sulfidation have lower homogeneity and stability on the surface, thus accelerating the destruction of AISI-316 steel. The above provides an initial contribution to oil industry in search of new alternatives to corrosion control by the attack of naphthenic acids, from the formation of FeS layers on exposed materials in the processing of heavy crude oils with high sulphur content.

Understanding the Unusual X-Ray Emission Properties of the Massive, Close Binary WR 20a: A High Energy Window into the Stellar Wind Initiation Region

NASA Astrophysics Data System (ADS)

Montes, Gabriela; Ramirez-Ruiz, Enrico; De Colle, Fabio; Strickler, Rachel

2013-11-01

The problem of explaining the X-ray emission properties of the massive, close binary WR 20a is discussed. Located near the cluster core of Westerlund 2, WR 20a is composed of two nearly identical Wolf-Rayet stars of 82 and 83 solar masses orbiting with a period of only 3.7 days. Although Chandra observations were taken during the secondary optical eclipse, the X-ray light curve shows no signs of a flux decrement. In fact, WR 20a appears slightly more X-ray luminous and softer during the optical eclipse, opposite to what has been observed in other binary systems. To aid in our interpretation of the data, we compare with the results of hydrodynamical simulations using the adaptive mesh refinement code Mezcal which includes radiative cooling and a radiative acceleration force term. It is shown that the X-ray emission can be successfully explained in models where the wind-wind collision interface in this system occurs while the outflowing material is still being accelerated. Consequently, WR 20a serves as a critical test-case for how radiatively driven stellar winds are initiated and how they interact. Our models not only procure a robust description of current Chandra data, which cover the orbital phases between 0.3 and 0.6, but also provide detailed predictions over the entire orbit.

Half-value-layer increase owing to tungsten buildup in the x-ray tube: fact or fiction.

PubMed

Stears, J G; Felmlee, J P; Gray, J E

1986-09-01

The half-value layer (HVL) of an x-ray beam is generally believed to increase with x-ray tube use. This increase in HVL has previously been attributed to the hardening of the x-ray beam as a result of a buildup of tungsten on the x-ray tube glass window. Radiographs and HVL measurements were obtained to determine the effect of tungsten deposited on the x-ray tube windows. This work, along with the HVL data from approximately 200 functioning x-ray tubes used for all applications that were monitored for more than 8 years, indicated there is no significant increase in HVL with diagnostic x-ray tube use.

Improving the accuracy of macromolecular structure refinement at 7 Å resolution.

PubMed

Brunger, Axel T; Adams, Paul D; Fromme, Petra; Fromme, Raimund; Levitt, Michael; Schröder, Gunnar F

2012-06-06

In X-ray crystallography, molecular replacement and subsequent refinement is challenging at low resolution. We compared refinement methods using synchrotron diffraction data of photosystem I at 7.4 Å resolution, starting from different initial models with increasing deviations from the known high-resolution structure. Standard refinement spoiled the initial models, moving them further away from the true structure and leading to high R(free)-values. In contrast, DEN refinement improved even the most distant starting model as judged by R(free), atomic root-mean-square differences to the true structure, significance of features not included in the initial model, and connectivity of electron density. The best protocol was DEN refinement with initial segmented rigid-body refinement. For the most distant initial model, the fraction of atoms within 2 Å of the true structure improved from 24% to 60%. We also found a significant correlation between R(free) values and the accuracy of the model, suggesting that R(free) is useful even at low resolution. Copyright © 2012 Elsevier Ltd. All rights reserved.

Synthesis, purification and bulk crystal growth of radiation detector materials using melt growth technique

NASA Astrophysics Data System (ADS)

Surabhi, Raja Rahul Reddy

In the past decade, there has been new and increased usage of radiation-detection technologies for applications in homeland security, non-proliferation, and national defense. Most of these applications require a portable device with high gamma-ray energy resolution and detection efficiency, compact size, room-temperature operation, and low cost. Consequently, there is a renewed understanding of the material limitations for these technologies and a great demand to develop next-generation radiation-detection materials that can operate at room temperature. Mercuric iodide (HgI2), Lead iodide (PbI2), and CdZnTe (CZT) are the current leading candidates for radiation detector applications. This is because of their high atomic number and large band gap that makes them particularly well suited for fabrication of high resolution and high efficiency compact devices. PbI2 is a promising material for room temperature nuclear radiation detectors, characterized by its wide band gap (EG=2.32eV) and high-density (rho=6.2g/cm3). It has been reported that PbI2 crystal detectors are able to detect gamma-ray in the range of 1KeV-1MeV, with good energy resolution. However, PbI 2 detectors have not been studied in detail because of non-availability of high quality single crystals. This study presents the synthesis, purification, growth and characterization of PbI2 single crystals grown. In this research, solid-state synthesis technique has been utilized for obtaining PbI2 as a starting material. For the first time, a unique low-temperature purification technique has been developed to obtain high-purity starting material. The crystals were grown using 2-zone Bridgman-Stockbarger (B.S) technique wherein growth rate and temperature gradient at the solid-liquid interface were optimized. Single crystals of PbI2 were successfully grown in quartz glass ampoule under different growth conditions. Material purity was determined by measuring the elemental concentration using the Inductively coupled plasma-optical emission spectroscopy (ICP-OES). ICP-OES is utilized for estimating impurities present in the low-temperature purified material, zone refined material and melt grown PbI2 crystals. The zone-refined material contains no traceable amounts of impurities, whereas the low-temperature purified material and melt grown PbI2 crystals show very low concentration of K (potassium) and Na (sodium) impurities. Crystal characterization has been performed for determining optical properties by UV-VIS spectroscopy. The energy band gap (EG) is an important parameter for materials used for room temperature gamma-ray detector applications. The absorption peak at 530nm is a characteristic of PbI2 and corresponds to the onset of the transitions from the valence band to the exciton level. From this absorption spectrum the calculated indirect band gap of PbI 2 was 2.33+/-0.025 eV at room temperature. For measuring the electrical properties (Dielectric and I-V characteristics) of the crystal, Ag (silver) contacts are applied to both sides of the sample. Dielectric analysis on melt grown PbI2 showed that space charge polarization was dominant at lower frequencies but stabilizes at higher frequencies over different operating temperatures. On the other hand, dielectric analysis for zone-refined material space charge polarization was constant over the operating range resulting in fewer lattice defects. Therefore the low temperature purified material followed by zone-refined purification provides detector grade material with fewer lattice defects. The measured electrical resistivity for melt grown PbI2 and zone-refined material are 3.185 x 10 10 O-cm and 0.754 x 109 O-cm at room temperature along (001) plane respectively.

Improvement of thermoelectric properties and their correlations with electron effective mass in Cu1.98SxSe1−x

PubMed Central

Zhao, Lanling; Fei, Frank Yun; Wang, Jun; Wang, Funing; Wang, Chunlei; Li, Jichao; Wang, Jiyang; Cheng, Zhenxiang; Dou, Shixue; Wang, Xiaolin

2017-01-01

Sulphur doping effects on the crystal structures, thermoelectric properties, density-of-states, and effective mass in Cu1.98SxSe1−x were studied based on the electrical and thermal transport property measurements, and first-principles calculations. The X-ray diffraction patterns and Rietveld refinements indicate that room temperature Cu1.98SxSe1−x (x = 0, 0.02, 0.08, 0.16) and Cu1.98SxSe1−x (x = 0.8, 0.9, 1.0) have the same crystal structure as monoclinic-Cu2Se and orthorhombic-Cu2S, respectively. Sulphur doping can greatly enhance zT values when x is in the range of 0.8≤ × ≤1.0. Furthermore, all doped samples show stable thermoelectric compatibility factors over a broad temperature range from 700 to 1000 K, which could greatly benefit their practical applications. First-principles calculations indicate that both the electron density-of-sates and the effective mass for all the compounds exhibit non-monotonic sulphur doping dependence. It is concluded that the overall thermoelectric performance of the Cu1.98SxSe1−x system is mainly correlated with the electron effective mass and the density-of-states. PMID:28091545

Application of an X-ray Fluorescence Instrument to Helicopter Wear Debris Analysis

DTIC Science & Technology

2008-04-01

from magnesium (Mg) to uranium (U) using two X-ray detection sensors: a FOCUS 5+ detector AlX-ray tube X-ray Detector 1. Incident X-ray...zinc (Zn), whilst the PIN detector is used to detect elements from calcium (Ca) to uranium (U) [4]. Elements between calcium (Ca) to zinc (Zn) can be... carbide paper, however polishing is not a normal sample preparation requirement for the Twin-X (see Figure 16). The samples were placed polished side

a-Si:H TFT-silicon hybrid low-energy x-ray detector

DOE PAGES

Shin, Kyung -Wook; Karim, Karim S.

2017-03-15

Direct conversion crystalline silicon X-ray imagers are used for low-energy X-ray photon (4-20 keV) detection in scientific research applications such as protein crystallography. In this paper, we demonstrate a novel pixel architecture that integrates a crystalline silicon X-ray detector with a thin-film transistor amorphous silicon pixel readout circuit. We describe a simplified two-mask process to fabricate a complete imaging array and present preliminary results that show the fabricated pixel to be sensitive to 5.89-keV photons from a low activity Fe-55 gamma source. Furthermore, this paper presented can expedite the development of high spatial resolution, low cost, direct conversion imagers formore » X-ray diffraction and crystallography applications.« less

Potentiality of a small and fast dense plasma focus as hard x-ray source for radiographic applications

NASA Astrophysics Data System (ADS)

Pavez, Cristian; Pedreros, José; Zambra, Marcelo; Veloso, Felipe; Moreno, José; Ariel, Tarifeño-Saldivia; Soto, Leopoldo

2012-10-01

Currently, a new generation of small plasma foci devices is being developed and researched, motivated by its potential use as portable sources of x-ray and neutron pulsed radiation for several applications. In this work, experimental results of the accumulated x-ray dose angular distribution and characterization of the x-ray source size are presented for a small and fast plasma focus device, ‘PF-400J’ (880 nF, 40 nH, 27-29 kV, ˜350 J, T/4 ˜ 300 ns). The experimental device is operated using hydrogen as the filling gas in a discharge region limited by a volume of around 80 cm3. The x-ray radiation is monitored, shot by shot, using a scintillator-photomultiplier system located outside the vacuum chamber at 2.3 m far away from the radiation emission region. The angular x-ray dose distribution measurement shows a well-defined emission cone, with an expansion angle of 5°, which is observed around the plasma focus device symmetry axis using TLD-100 crystals. The x-ray source size measurements are obtained using two image-forming aperture techniques: for both cases, one small (pinhole) and one large for the penumbral imaging. These results are in agreement with the drilling made by the energetic electron beam coming from the pinch region. Additionally, some examples of image radiographic applications are shown in order to highlight the real possibilities of the plasma focus device as a portable x-ray source. In the light of the obtained results and the scaling laws observed in plasma foci devices, we present a discussion on the potentiality and advantages of these devices as pulsed and safe sources of x-radiation for applications.

Ultra-short wavelength x-ray system

DOEpatents

Umstadter, Donald [Ann Arbor, MI; He, Fei [Ann Arbor, MI; Lau, Yue-Ying [Potomac, MD

2008-01-22

A method and apparatus to generate a beam of coherent light including x-rays or XUV by colliding a high-intensity laser pulse with an electron beam that is accelerated by a synchronized laser pulse. Applications include x-ray and EUV lithography, protein structural analysis, plasma diagnostics, x-ray diffraction, crack analysis, non-destructive testing, surface science and ultrafast science.

X-Rays: The Inside Story (Primary). Teacher's Guide.

ERIC Educational Resources Information Center

Royal Australasian Coll. of Radiologists, Sydney (Australia).

The goal of this unit is to help children explore the aspects of X-rays and radiology in society. Students develop an understanding that X-rays are silhouette images, beneficial in health care, and a part of radiology. The history and development of X-rays as well as their applications in advancing technology are also explored. The unit is…

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.

Thin Shell, Segmented X-Ray Mirrors

NASA Technical Reports Server (NTRS)

Petre, Robert

2010-01-01

Thin foil mirrors were introduced as a means of achieving high throughput in an X-ray astronomical imaging system in applications for which high angular resolution were not necessary. Since their introduction, their high filling factor, modest mass, relative ease of construction, and modest cost have led to their use in numerous X-ray observatories, including the Broad Band X-ray Telescope, ASCA, and Suzaku. The introduction of key innovations, including epoxy replicated surfaces, multilayer coatings, and glass mirror substrates, has led to performance improvements, and in their becoming widely used for X-ray astronomical imaging at energies above 10 keV. The use of glass substrates has also led to substantial improvement in angular resolution, and thus their incorporation into the NASA concept for the International X-ray Observatory with a planned 3 in diameter aperture. This paper traces the development of foil mirrors from their inception in the 1970's through their current and anticipated future applications.

X-Pinch And Its Applications In X-ray Radiograph

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

Zou Xiaobing; Wang Xinxin; Liu Rui

2009-07-07

An X-pinch device and the related diagnostics of x-ray emission from X-pinch were briefly described. The time-resolved x-ray measurements with photoconducting diodes show that the x-ray pulse usually consists of two subnanosecond peaks with a time interval of about 0.5 ns. Being consistent with these two peaks of the x-ray pulse, two point x-ray sources of size ranging from 100 mum to 5 mum and depending on cut-off x-ray photon energy were usually observed on the pinhole pictures. The x-pinch was used as x-ray source for backlighting of the electrical explosion of single wire and the evolution of X-pinch, andmore » for phase-contrast imaging of soft biological objects such as a small shrimp and a mosquito.« 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 technological innovations in both dispersive and nondispersive spectroscopic instrumentation.

Radiation Backgrounds at Cosmic Dawn: X-Rays from Compact Binaries

NASA Astrophysics Data System (ADS)

Madau, Piero; Fragos, Tassos

2017-05-01

We compute the expected X-ray diffuse background and radiative feedback on the intergalactic medium (IGM) from X-ray binaries prior to and during the epoch of reionization. The cosmic evolution of compact binaries is followed using a population synthesis technique that treats separately neutron stars and black hole binaries in different spectral states and is calibrated to reproduce the observed X-ray properties of galaxies at z ≲ 4. Together with an updated empirical determination of the cosmic history of star formation, recent modeling of the stellar mass-metallicity relation, and a scheme for absorption by the IGM that accounts for the presence of ionized H II bubbles during the epoch of reionization, our detailed calculations provide refined predictions of the X-ray volume emissivity and filtered radiation background from “normal” galaxies at z ≳ 6. Radiative transfer effects modulate the background spectrum, which shows a characteristic peak between 1 and 2 keV. Because of the energy dependence of photoabsorption, soft X-ray photons are produced by local sources, while more energetic radiation arrives unattenuated from larger cosmological volumes. While the filtering of X-ray radiation through the IGM slightly increases the mean excess energy per photoionization, it also weakens the radiation intensity below 1 keV, lowering the mean photoionization and heating rates. Numerical integration of the rate and energy equations shows that the contribution of X-ray binaries to the ionization of the bulk IGM is negligible, with the electron fraction never exceeding 1%. Direct He I photoionizations are the main source of IGM heating, and the temperature of the largely neutral medium in between H II cavities increases above the temperature of the cosmic microwave background (CMB) only at z ≲ 10, when the volume filling factor of H II bubbles is already ≳0.1. Therefore, in this scenario, it is only at relatively late epochs that neutral intergalactic hydrogen may be observable in 21 cm emission against the CMB.

Radiation Backgrounds at Cosmic Dawn: X-Rays from Compact Binaries

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

Madau, Piero; Fragos, Tassos

We compute the expected X-ray diffuse background and radiative feedback on the intergalactic medium (IGM) from X-ray binaries prior to and during the epoch of reionization. The cosmic evolution of compact binaries is followed using a population synthesis technique that treats separately neutron stars and black hole binaries in different spectral states and is calibrated to reproduce the observed X-ray properties of galaxies at z ≲ 4. Together with an updated empirical determination of the cosmic history of star formation, recent modeling of the stellar mass–metallicity relation, and a scheme for absorption by the IGM that accounts for the presencemore » of ionized H ii bubbles during the epoch of reionization, our detailed calculations provide refined predictions of the X-ray volume emissivity and filtered radiation background from “normal” galaxies at z ≳ 6. Radiative transfer effects modulate the background spectrum, which shows a characteristic peak between 1 and 2 keV. Because of the energy dependence of photoabsorption, soft X-ray photons are produced by local sources, while more energetic radiation arrives unattenuated from larger cosmological volumes. While the filtering of X-ray radiation through the IGM slightly increases the mean excess energy per photoionization, it also weakens the radiation intensity below 1 keV, lowering the mean photoionization and heating rates. Numerical integration of the rate and energy equations shows that the contribution of X-ray binaries to the ionization of the bulk IGM is negligible, with the electron fraction never exceeding 1%. Direct He i photoionizations are the main source of IGM heating, and the temperature of the largely neutral medium in between H ii cavities increases above the temperature of the cosmic microwave background (CMB) only at z ≲ 10, when the volume filling factor of H ii bubbles is already ≳0.1. Therefore, in this scenario, it is only at relatively late epochs that neutral intergalactic hydrogen may be observable in 21 cm emission against the CMB.« less

X-ray Constrained Extremely Localized Molecular Orbitals: Theory and Critical Assessment of the New Technique.

PubMed

Genoni, Alessandro

2013-07-09

Following the X-ray constrained wave function approach proposed by Jayatilaka, we have devised a new technique that allows to extract molecular orbitals strictly localized on small molecular fragments from sets of experimental X-ray structure factors amplitudes. Since the novel strategy enables to obtain electron distributions that have quantum mechanical features and that can be easily interpreted in terms of traditional chemical concepts, the method can be also considered as a new useful tool for the determination and the analysis of charge densities from high-resolution X-ray experiments. In this paper, we describe in detail the theory of the new technique, which, in comparison to our preliminary work, has been improved both treating the effects of isotropic secondary extinctions and introducing a new protocol to halt the fitting procedure against the experimental X-ray scattering data. The performances of the novel strategy have been studied both in function of the basis-sets flexibility and in function of the quality of the considered crystallographic data. The tests performed on four different systems (α-glycine, l-cysteine, (aminomethyl)phosphonic acid and N-(trifluoromethyl)formamide) have shown that the achievement of good statistical agreements with the experimental measures mainly depends on the quality of the crystal structures (i.e., geometry positions and thermal parameters) used in the X-ray constrained calculations. Finally, given the reliable transferability of the obtained Extremely Localized Molecular Orbitals (ELMOs), we envisage to exploit the novel approach to construct new ELMOs databases suited to the development of linear-scaling methods for the refinement of macromolecular crystal structures.

Simulation tools for analyzer-based x-ray phase contrast imaging system with a conventional x-ray source

NASA Astrophysics Data System (ADS)

Caudevilla, Oriol; Zhou, Wei; Stoupin, Stanislav; Verman, Boris; Brankov, J. G.

2016-09-01

Analyzer-based X-ray phase contrast imaging (ABI) belongs to a broader family of phase-contrast (PC) X-ray imaging modalities. Unlike the conventional X-ray radiography, which measures only X-ray absorption, in PC imaging one can also measures the X-rays deflection induced by the object refractive properties. It has been shown that refraction imaging provides better contrast when imaging the soft tissue, which is of great interest in medical imaging applications. In this paper, we introduce a simulation tool specifically designed to simulate the analyzer-based X-ray phase contrast imaging system with a conventional polychromatic X-ray source. By utilizing ray tracing and basic physical principles of diffraction theory our simulation tool can predicting the X-ray beam profile shape, the energy content, the total throughput (photon count) at the detector. In addition we can evaluate imaging system point-spread function for various system configurations.

High-pressure-assisted X-ray-induced damage as a new route for materials synthesis

DOE PAGES

Evlyukhin, Egor; Kim, Eunja; Goldberger, David; ...

2018-01-01

X-ray radiation induced damage has been known for decades and has largely been viewed as a tremendous nuisance; e.g., most X-ray-related studies of organic and inorganic materials suffer X-ray damage to varying degrees. Although, recent theoretical and experimental investigation of the response of simple chemical systems to X-rays offered better understanding of the mechanistic details of X-ray induced damage, the question about useful applicability of this technique is still unclear. Furthermore we experimentally demonstrate that by tuning pressure and X-ray energy, the radiation induced damage can be controlled and used for synthesis of novel materials.

Simulations of a Molecular Cloud experiment using CRASH

NASA Astrophysics Data System (ADS)

Trantham, Matthew; Keiter, Paul; Vandervort, Robert; Drake, R. Paul; Shvarts, Dov

2017-10-01

Recent laboratory experiments explore molecular cloud radiation hydrodynamics. The experiment irradiates a gold foil with a laser producing x-rays to drive the implosion or explosion of a foam ball. The CRASH code, an Eulerian code with block-adaptive mesh refinement, multigroup diffusive radiation transport, and electron heat conduction developed at the University of Michigan to design and analyze high-energy-density experiments, is used to perform a parameter search in order to identify optically thick, optically thin and transition regimes suitable for these experiments. Specific design issues addressed by the simulations are the x-ray drive temperature, foam density, distance from the x-ray source to the ball, as well as other complicating issues such as the positioning of the stalk holding the foam ball. We present the results of this study and show ways the simulations helped improve the quality of the experiment. This work is funded by the LLNL under subcontract B614207 and NNSA-DS and SC-OFES Joint Program in High-Energy-Density Laboratory Plasmas, Grant Number DE-NA0002956.

The X-Ray Structure and Spectrum of the Pulsar Wind Nebula Surrounding PSR B1853+01 in W44

NASA Technical Reports Server (NTRS)

Petre, R.; Kuntz, K. D.; Shelton, R. L.; White, Nicholas E. (Technical Monitor)

2001-01-01

We present the result of a Chandra ACIS observation of the pulsar PSR B1853+01 and its associated pulsar wind nebula (PWN), embedded within the supernova remnant W44. A hard band ACIS map cleanly distinguishes the PWN from the thermal emission of W44. The nebula is extended in the north-south direction, with an extent about half that of the radio emission. Morphological differences between the X-ray and radio images are apparent. Spectral fitting reveals a clear difference in spectral index between the hard emission from PSR B1853+01 (Gamma approx. 1.4) and the extended nebula (Gamma approx. 2.2). The more accurate values for the X-ray flux and spectral index are used refine estimates for PWN parameters, including magnetic field strength, the average Lorentz factor gamma of the particles in the wind, the magnetization parameter sigma, and the ratio k of electrons to other particles.

The effects of rigid motions on elastic network model force constants

PubMed Central

Lezon, Timothy R.

2012-01-01

Elastic network models provide an efficient way to quickly calculate protein global dynamics from experimentally determined structures. The model’s single parameter, its force constant, determines the physical extent of equilibrium fluctuations. The values of force constants can be calculated by fitting to experimental data, but the results depend on the type of experimental data used. Here we investigate the differences between calculated values of force constants _t to data from NMR and X-ray structures. We find that X-ray B factors carry the signature of rigid-body motions, to the extent that B factors can be almost entirely accounted for by rigid motions alone. When fitting to more refined anisotropic temperature factors, the contributions of rigid motions are significantly reduced, indicating that the large contribution of rigid motions to B factors is a result of over-fitting. No correlation is found between force constants fit to NMR data and those fit to X-ray data, possibly due to the inability of NMR data to accurately capture protein dynamics. PMID:22228562

The Orbit and Position of the X-ray Pulsar XTE J1855-026: An Eclipsing Supergiant System

NASA Technical Reports Server (NTRS)

Corbet, Robin H. D.; Mukai, Koji; White, Nicholas E. (Technical Monitor)

2002-01-01

A pulse timing orbit has been obtained for the X-ray binary XTEJ1855-026 using observations made with the Proportional Counter Array on board the Rossi X-ray Timing Explorer. The mass function obtained of approximately 16 solar mass together with the detection of an extended near-total eclipse confirm that the primary star is supergiant as predicted. The orbital eccentricity is found to be very low with a best fit value of 0.04 +/- 0.02. The orbital period is also refined to be 6.0724 +/- 0.0009 days using an improved and extended light curve obtained with RXTE's All Sky Monitor. Observations with the ASCA satellite provide an improved source location of R.A.= 18 hr 55 min 31.3 sec, decl.= -02 deg 36 min 24.0 sec (2000) with an estimated systematic uncertainty of less than 12 min. A serendipitous new source, AX J1855.4-0232, was also discovered during the ASCA observations.

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 microroughness of a few 0.1 nm, and low weight (the volume density is 2.5 g cm-3 for glass and 2.3 g cm-3 for Si). Technologies are needed to be exploited; how to shape these substrates to achieve the required precise Xray optics geometries without degradations of the fine surface microroughness. Although glass and recently silicon wafers are considered to represent most promising materials for future advanced large aperture space Xray telescopes, there also exist other alternative materials worth further study such as amorphous metals and glassy carbon [1]. In order to achieve sub-arsec angular resolutions, principles of active optics have to be adopted.

Monte Carlo analysis of neutron diffuse scattering data

NASA Astrophysics Data System (ADS)

Goossens, D. J.; Heerdegen, A. P.; Welberry, T. R.; Gutmann, M. J.

2006-11-01

This paper presents a discussion of a technique developed for the analysis of neutron diffuse scattering data. The technique involves processing the data into reciprocal space sections and modelling the diffuse scattering in these sections. A Monte Carlo modelling approach is used in which the crystal energy is a function of interatomic distances between molecules and torsional rotations within molecules. The parameters of the model are the spring constants governing the interactions, as they determine the correlations which evolve when the model crystal structure is relaxed at finite temperature. When the model crystal has reached equilibrium its diffraction pattern is calculated and a χ2 goodness-of-fit test between observed and calculated data slices is performed. This allows a least-squares refinement of the fit parameters and so automated refinement can proceed. The first application of this methodology to neutron, rather than X-ray, data is outlined. The sample studied was deuterated benzil, d-benzil, C14D10O2, for which data was collected using time-of-flight Laue diffraction on SXD at ISIS.

Multiwavelength monitoring and X-ray brightening of Be X-ray binary PSR J2032+4127/MT91 213 on its approach to periastron

DOE PAGES

Ho, Wynn C. G.; Ng, C. -Y.; Lyne, Andrew G.; ...

2016-09-22

The radio and gamma-ray pulsar PSR J2032+4127 was recently found to be in a decades-long orbit with the Be star MT91 213, with the pulsar moving rapidly towards periastron. This binary shares many similar characteristics with the previously unique binary system PSR B1259-63/LS 2883. Here in this paper, we describe radio, X-ray, and optical monitoring of PSR J2032+4127/MT91 213. Our extended orbital phase coverage in radio, supplemented with Fermi LAT gamma-ray data, allows us to update and refine the orbital period to 45–50 yr and time of periastron passage to 2017 November. We analyse archival and recent Chandra and Swiftmore » observations and show that PSR J2032+4127/MT91 213 is now brighter in X-rays by a factor of ~70 since 2002 and ~20 since 2010. While the pulsar is still far from periastron, this increase in X-rays is possibly due to collisions between pulsar and Be star winds. Optical observations of the Hα emission line of the Be star suggest that the size of its circumstellar disc may be varying by ~2 over time-scales as short as 1–2 months. In conclusion, multiwavelength monitoring of PSR J2032+4127/MT91 213 will continue through periastron passage, and the system should present an interesting test case and comparison to PSR B1259-63/LS 2883.« less

South Atlantic Anomaly Entry and Exit as Measured by the X-Ray Timing Explorer

NASA Technical Reports Server (NTRS)

Smith, Evan; Stark, Michael; Giles, Barry; Antunes, Sandy; Gawne, Bill

1996-01-01

The Rossi X-ray Timing Explorer (RXTE) carries instruments that must switch off high voltages (HV) when passing through the South Atlantic Anomaly (SAA). The High Energy X-ray Timing Experiment (HEXTE) contains a particle monitor that detects the increased particle flux associated with the SAA and autonomously reduces its voltage. The Proportional Counter Array (PCA) relies on uplinked predictions of SAA entry/exit times based on ephemeris data provided by the Flight Dynamics Facility. A third instrument, the All-Sky Monitor (ASM) also uses a predicted SAA model to reduce voltage when passing through the SAA. Data collected from the HEXTE particle monitor, as well as other instrument readings near the times of SAA entry/exit offer the potential for refining models of the boundaries of the SAA. The SAA has an increased particle flux which causes high rates of detection in the RXTE instruments designed to observe x-rays. The high counting rates could degrade the PCA if HV is not reduced during SAA passages. On the other hand, PCA downtime can be minimized and the science return can be optimized by having the best possible model of the SAA boundary. Thus, the PCA team planned an extensive effort during in-orbit checkout to utilize both the HEXTE particle monitor data and instrument counting rates to refine the model of the SAA boundary. The times of SAA entry and exit are compared with the definitive epemeris to determine the precise location (latitude and longitude) of the SAA boundary. Over time, the SAA and its perimeter were mapped. The RXTE Science Operations Center is continuously working to feed back the results of this effort into the science scheduling process, improving the SAA model as it affects the RXTE instruments, thus obtaining more accurate estimates of the SAA entry/exit times.

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

High brightness x ray source for directed energy and holographic imaging applications, phase 2

NASA Astrophysics Data System (ADS)

McPherson, Armon; Rhodes, Charles K.

1992-03-01

Advances in x-ray imaging technology and x-ray sources are such that a new technology can be brought to commercialization enabling the three-dimensional (3-D) microvisualization of hydrated biological specimens. The Company is engaged in a program whose main goal is the development of a new technology for direct three dimensional (3-D) x-ray holographic imaging. It is believed that this technology will have a wide range of important applications in the defense, medical, and scientific sectors. For example, in the medical area, it is expected that biomedical science will constitute a very active and substantial market, because the application of physical technologies for the direct visualization of biological entities has had a long and extremely fruitful history.

Hydrothermal synthesis of a photovoltaic material based on CuIn0.5Ga0.5Se2

NASA Astrophysics Data System (ADS)

Castellanos Báez, Y. T.; Fuquen Peña, D. A.; Gómez-Cuaspud, J. A.; Vera-López, E.; Pineda-Triana, Y.

2017-12-01

The present work report, the synthesis and characterization of the CuIn0.5Ga0.5Se2 system (abbreviated CIGS), by the implementation of a hydrothermal route, in order to obtain a solid with appropriate properties in terms of surface, morphological and texture properties for potential applications in the design of photovoltaic cells. The synthesis was carried out using the corresponding stoichiometric quantities (Cu:In:Ga:Se 1:0.5:0.5:2), which were mixed in a Teflon vessel under stirring conditions. The homogeneous solution was treated in a steel autoclave at 300°C for 72 hours at the end of which the resulting material was characterized by X-Ray Diffraction (XRD) and Rietveld refinement. The results of the structural characterization allowed to confirm the obtaining of a chalcopyrite type structure, with a I-42 d (122) structure and cell parameters a=0.570, b=0.570, c=1.140nm, α=90, β=90, γ=90° oriented along (1 0 4) facet, detecting the presence of a secondary phases, related with CuInSe and CuIn metallic selenides, derived from synthesis process. The structural refinement allowing to validate the obtaining of a nanometric crystalline material (10-20nm) for potential applications in field of photovoltaic technology.

Application of a magnetograph and X-ray telescope to the study of coronal structure variations

NASA Technical Reports Server (NTRS)

Rust, D. M.

1980-01-01

The application of magnetographs and X-ray imaging techniques to determine the magnitude, structure, origin, and evolution of the solar coronal magnetic field is examined. The spatial and temporal resolution of the X-ray telescope is discussed and a comparison of ground based magnetogram sequences versus a magnetograph in space is presented. Skylab photographs of the evolution of transient coronal holes are provided.

Simulating the X-Ray Image Contrast to Set-Up Techniques with Desired Flaw Detectability

NASA Technical Reports Server (NTRS)

Koshti, Ajay M.

2015-01-01

The paper provides simulation data of previous work by the author in developing a model for estimating detectability of crack-like flaws in radiography. The methodology is being developed to help in implementation of NASA Special x-ray radiography qualification, but is generically applicable to radiography. The paper describes a method for characterizing X-ray detector resolution for crack detection. Applicability of ASTM E 2737 resolution requirements to the model are also discussed. The paper describes a model for simulating the detector resolution. A computer calculator application, discussed here, also performs predicted contrast and signal-to-noise ratio calculations. Results of various simulation runs in calculating x-ray flaw size parameter and image contrast for varying input parameters such as crack depth, crack width, part thickness, x-ray angle, part-to-detector distance, part-to-source distance, source sizes, and detector sensitivity and resolution are given as 3D surfaces. These results demonstrate effect of the input parameters on the flaw size parameter and the simulated image contrast of the crack. These simulations demonstrate utility of the flaw size parameter model in setting up x-ray techniques that provide desired flaw detectability in radiography. The method is applicable to film radiography, computed radiography, and digital radiography.

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

Koren, S; Bragilovski, D; Tafo, A Guemnie

Purpose: To evaluate the clinical feasibility of IntraBeam intra operative kV irradiation beam device for ocular conjunctiva treatments. The Intra-Beam system offers a 4.4 mm diameter needle applicator, that is not suitable for treatment of a large surface with limits access. We propose an adaptor that will answer to this clinical need and provide initial dosimetry. Methods: The dose distribution of the needle applicator is non uniform and hence not suitable for treatment of relatively large surfaces. We designed an adapter to the needle applicator that will filter the X-rays and produce a conformal dose distribution over the treatment areamore » while shielding surfaces to be spared. Dose distributions were simulated using FLUKA is a fully integrated particle physics Monte Carlo simulation package. Results: We designed a wedge applicator made of Polythermide window and stainless steel for collimating. We compare the dose distribution to that of the known needle and surface applicators. Conclusion: Initial dosimetry shows feasibility of this approach. While further refinements to the design may be warranted, the results support construction of a prototype and confirmation of the Monte Carlo dosimetry with measured data.« less

Purification and Crystal Growth of Lead Iodide by Physical Vapor Transport Method

NASA Technical Reports Server (NTRS)

Wright, G. W.; Cole, M.; Chen, Y.-F.; Chen, K.-T.; Chen, H.; Chattopadhyay, K.; Burger, A.

1998-01-01

Lead iodide (PbI2) is a layered compound semiconductor being developed as room temperature x- and gamma-ray detector. Compared to the more studied material, mercuric iodide, PbI2 has a higher melting temperature and no phase transition until liquid phase which are indications of better mechanical properties. In this study, the source material was purified by the zone-refining process, and the purest section was extracted from center of the the zone-refined ingot to be grown by physical vapor transport (PVT) method. The zone-refined material and as-grown crystals were characterized by optical microscopy and differential scanning calorimetry (DSC) to reveal the surface morphology, purity and stoichiometry. The results shows that both materials are near-stoichiometric composition, with the purity of the as-grown crystals higher than zone-refined materials. The resistivity of the as-grown crystal (10" Omega-cm) was derived from current-voltage (I-V) measurement, and is 10 times higher than the zone-refined materials. Detail results will be presented and discussed.

Hydrogen atoms can be located accurately and precisely by x-ray crystallography.

PubMed

Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M; Woźniak, Krzysztof; Jayatilaka, Dylan

2016-05-01

Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A-H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A-H bond lengths with those from neutron measurements for A-H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors.

Hydrogen atoms can be located accurately and precisely by x-ray crystallography

PubMed Central

Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M.; Woźniak, Krzysztof; Jayatilaka, Dylan

2016-01-01

Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A–H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A–H bond lengths with those from neutron measurements for A–H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors. PMID:27386545

From Radio to X-rays--Some 'Real' Electrical Applications.

ERIC Educational Resources Information Center

Freeman, J. C.

1986-01-01

Describes practical applications related to X-rays, ultra-violet radiation, light radiation, short-wave infra-red radiation, medium-wave infra-red radiation, long-wave infra-red radiation, microwave radiation, and radio frequency radiation. Suggests that these applications be used during instruction on electricity. (JN)

Investigation on the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ manganites

NASA Astrophysics Data System (ADS)

Arun, B.; Athira, M.; Akshay, V. R.; Sudakshina, B.; Mutta, Geeta R.; Vasundhara, M.

2018-02-01

We have investigated the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ Perovskite manganites. Rietveld refinement of the X-ray powder diffraction patterns confirms that all the studied compounds have crystallized into an orthorhombic structure with Pbnm space group. Transmission electron microscopy analysis reveals nanocrystalline compounds with crystallite size less than 50 nm. The selected area electron diffraction patterns reveal the highly crystalline nature of the compounds and energy dispersive X-ray spectroscopic analysis shows that the obtained compositions are nearly identical with the nominal one. The oxygen stoichiometry is estimated by iodometric titration method and stoichiometric compositions are confirmed by X-ray Fluorescence Spectrometry analysis. A large bifurcation is observed in the ZFC/FC curves and Arrott plots not show a linear relation but have a convex curvature nature. The temperature dependence of inverse magnetic susceptibility at higher temperature confirms the existence of ferromagnetic clusters. The experimental results reveal that the reduction of crystallite size to nano metric scale in Pr-deficient manganites adversely influences structural, magnetic and magnetocaloric properties as compared to its bulk counterparts reported earlier.

Novel wide-field x-ray optics for space

NASA Astrophysics Data System (ADS)

Hudec, René; Pína, Ladislav; Inneman, Adolf

2017-11-01

We report on the program of design and development of innovative very wide field X-ray optics for space applications. We describe the idea of wide field X-ray optics of the lobster-eye type of both Angel and Schmidt arrangements. This optics was suggested in 70ies but not yet used in space experiment due to severe manufacturing problems. The lobster-eye X-ray optics may achieve up to 180 degrees (diameter) field of view at angular resolution of order of 1 arcmin. We report on various prototypes of lobster-eye X-ray lenses based on alternative technologies (replicated double sided X-ray reflecting flats, float glass, replicated square channels etc.) as well as on their optical and X-ray tests. We also discuss the importance and performance of lobster-eye X-ray telescopes in future X-ray astronomy projects.

Advances in indirect detector systems for ultra high-speed hard X-ray imaging with synchrotron light

NASA Astrophysics Data System (ADS)

Olbinado, M. P.; Grenzer, J.; Pradel, P.; De Resseguier, T.; Vagovic, P.; Zdora, M.-C.; Guzenko, V. A.; David, C.; Rack, A.

2018-04-01

We report on indirect X-ray detector systems for various full-field, ultra high-speed X-ray imaging methodologies, such as X-ray phase-contrast radiography, diffraction topography, grating interferometry and speckle-based imaging performed at the hard X-ray imaging beamline ID19 of the European Synchrotron—ESRF. Our work highlights the versatility of indirect X-ray detectors to multiple goals such as single synchrotron pulse isolation, multiple-frame recording up to millions frames per second, high efficiency, and high spatial resolution. Besides the technical advancements, potential applications are briefly introduced and discussed.

X-ray Fluorescence Holography: Principles, Apparatus, and Applications

NASA Astrophysics Data System (ADS)

Hayashi, Kouichi; Korecki, Pawel

2018-06-01

X-ray fluorescence holography (XFH) is an atomic structure determination technique that combines the capabilities of X-ray diffraction and X-ray fluorescence spectroscopy. It provides a unique means of gaining fully three-dimensional information about the local atomic structure and lattice site positions of selected elements inside compound samples. In this work, we discuss experimental and theoretical aspects that are essential for the efficient recording and analysis of X-ray fluorescence holograms and review the most recent advances in XFH. We describe experiments performed with brilliant synchrotron radiation as well as with tabletop setups that employ conventional X-ray tubes.

X-ray Scattering Combined with Coordinate-Based Analyses for Applications in Natural and Artificial Photosynthesis

PubMed Central

Tiede, David M.; Mardis, Kristy L.; Zuo, Xiaobing

2009-01-01

Advances in x-ray light sources and detectors have created opportunities for advancing our understanding of structure and structural dynamics for supramolecular assemblies in solution by combining x-ray scattering measurement with coordinate-based modeling methods. In this review the foundations for x-ray scattering are discussed and illustrated with selected examples demonstrating the ability to correlate solution x-ray scattering measurements to molecular structure, conformation, and dynamics. These approaches are anticipated to have a broad range of applications in natural and artificial photosynthesis by offering possibilities for structure resolution for dynamic supramolecular assemblies in solution that can not be fully addressed with crystallographic techniques, and for resolving fundamental mechanisms for solar energy conversion by mapping out structure in light-excited reaction states. PMID:19636808

Simulation of a compact analyzer-based imaging system with a regular x-ray source

NASA Astrophysics Data System (ADS)

Caudevilla, Oriol; Zhou, Wei; Stoupin, Stanislav; Verman, Boris; Brankov, J. G.

2017-03-01

Analyzer-based Imaging (ABI) belongs to a broader family of phase-contrast (PC) X-ray techniques. PC measures X-ray deflection phenomena when interacting with a sample, which is known to provide higher contrast images of soft tissue than other X-ray methods. This is of high interest in the medical field, in particular for mammogram applications. This paper presents a simulation tool for table-top ABI systems using a conventional polychromatic X-ray source.

Experimental investigation of dynamic fragmentation of laser shock-loaded by soft recovery and X-ray radiography

NASA Astrophysics Data System (ADS)

Xin, Jianting; He, Weihua; Chu, Genbai; Gu, Yuqiu

2017-06-01

Dynamic fragmentation of metal under shock pressure is an important issue for both fundamental science and practical applications. And in recent decades, laser provides a promising shock loading technique for investigating the process of dynamic fragmentation under extreme condition application of high strain rate. Our group has performed experimental investigation of dynamic fragmentation under laser shock loading by soft recovery and X-ray radiography at SGC / ó prototype laser facility. The fragments under different loading pressures were recovered by PMP foam and analyzed by X-ray micro-tomography and the improved watershed method. The experiment result showed that the bilinear exponential distribution is more appropriate for representing the fragment size distribution. We also developed X-ray radiography technique. Owing to its inherent advantage over shadowgraph technique, X-ray radiography can potentially determine quantitatively material densities by measuring the X-ray transmission. Our group investigated dynamic process of microjetting by X-ray radiography technique, the recorded radiographic images show clear microjetting from the triangular grooves in the free surface of tin sample.

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.

Flash X-ray with image enhancement applied to combustion events

NASA Astrophysics Data System (ADS)

White, K. J.; McCoy, D. G.

1983-10-01

Flow visualization of interior ballistic processes by use of X-rays has placed more stringent requirements on flash X-ray techniques. The problem of improving radiographic contrast of propellants in X-ray transparent chambers was studied by devising techniques for evaluating, measuring and reducing the effects of scattering from both the test object and structures in the test area. X-ray film and processing is reviewed and techniques for evaluating and calibrating these are outlined. Finally, after X-ray techniques were optimized, the application of image enhancement processing which can improve image quality is described. This technique was applied to X-ray studies of the combustion of very high burning rate (VHBR) propellants and stick propellant charges.

Soft x-ray contact imaging of biological specimens using a laser-produced plasma as an x-ray source

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

Cheng, P.C.

The use of a laser-produced plasma as an x-ray source provides significant advantages over other types of sources for x-ray microradiography of, particularly, living biological specimens. The pulsed nature of the x-rays enables imaging of the specimen in a living state, and the small source size minimizes penumbral blurring. This makes it possible to make an exposure close to the source, thereby increasing the x-ray intensity. In this article, we will demonstrate the applications of x-ray contact microradiography in structural and developmental botany such as the localization of silica deposition and the floral morphologenesis of maize.

Probing high-redshift clusters with HST/ACS gravitational weak-lensing and Chandra x-ray observations

NASA Astrophysics Data System (ADS)

Jee, Myungkook James

2006-06-01

Clusters of galaxies, the largest gravitationally bound objects in the Universe, are useful tracers of cosmic evolution, and particularly detailed studies of still-forming clusters at high-redshifts can considerably enhance our understanding of the structure formation. We use two powerful methods that have become recently available for the study of these distant clusters: spaced- based gravitational weak-lensing and high-resolution X-ray observations. Detailed analyses of five high-redshift (0.8 < z < 1.3) clusters are presented based on the deep Advanced Camera for Surveys (ACS) and Chandra X-ray images. We show that, when the instrumental characteristics are properly understood, the newly installed ACS on the Hubble Space Telescope (HST) can detect subtle shape distortions of background galaxies down to the limiting magnitudes of the observations, which enables the mapping of the cluster dark matter in unprecedented high-resolution. The cluster masses derived from this HST /ACS weak-lensing study have been compared with those from the re-analyses of the archival Chandra X-ray data. We find that there are interesting offsets between the cluster galaxy, intracluster medium (ICM), and dark matter centroids, and possible scenarios are discussed. If the offset is confirmed to be uniquitous in other clusters, the explanation may necessitate major refinements in our current understanding of the nature of dark matter, as well as the cluster galaxy dynamics. CL0848+4452, the highest-redshift ( z = 1.27) cluster yet detected in weak-lensing, has a significant discrepancy between the weak- lensing and X-ray masses. If this trend is found to be severe and common also for other X-ray weak clusters at redshifts beyond the unity, the conventional X-ray determination of cluster mass functions, often inferred from their immediate X-ray properties such as the X-ray luminosity and temperature via the so-called mass-luminosity (M-L) and mass-temperature (M-T) relations, will become highly unstable in this redshift regime. Therefore, the relatively unbiased weak-lensing measurements of the cluster mass properties can be used to adequately calibrate the scaling relations in future high-redshift cluster investigations.

Rietveld refinement and FTIR analysis of bulk ceramic Co3-xMnxO4 compositions

NASA Astrophysics Data System (ADS)

Meena, P. L.; Kumar, Ravi; Sreenivas, K.

2013-02-01

Co3-xMnxO4 (x = 0.0, 0.6, 1.2) prepared by solid state reaction method and characterized by powder X-ray diffraction (XRD) and Fourier transform infrared (FTIR). Lattice parameters (a), oxygen parameter (u), and ionic radii of cations have been determined through Rietveld analysis. Both a and u parameters are related to expansion of octahedral site as Mn content in Co3O4. Analysis of XRD data show that Mn (x ≤ 1.2) is accommodated at the octahedral site, while retaining the cubic spinel structure. FTIR results also confirm the same and signify strong interactions due to overlapping of Co and Mn octahedra.

Combinatorial refinement of thin-film microstructure, properties and process conditions: iterative nanoscale search for self-assembled TiAlN nanolamellae.

PubMed

Zalesak, J; Todt, J; Pitonak, R; Köpf, A; Weißenbacher, R; Sartory, B; Burghammer, M; Daniel, R; Keckes, J

2016-12-01

Because of the tremendous variability of crystallite sizes and shapes in nano-materials, it is challenging to assess the corresponding size-property relationships and to identify microstructures with particular physical properties or even optimized functions. This task is especially difficult for nanomaterials formed by self-organization, where the spontaneous evolution of microstructure and properties is coupled. In this work, two compositionally graded TiAlN films were (i) grown using chemical vapour deposition by applying a varying ratio of reacting gases and (ii) subsequently analysed using cross-sectional synchrotron X-ray nanodiffraction, electron microscopy and nanoindentation in order to evaluate the microstructure and hardness depth gradients. The results indicate the formation of self-organized hexagonal-cubic and cubic-cubic nanolamellae with varying compositions and thicknesses in the range of ∼3-15 nm across the film thicknesses, depending on the actual composition of the reactive gas mixtures. On the basis of the occurrence of the nanolamellae and their correlation with the local film hardness, progressively narrower ranges of the composition and hardness were refined in three steps. The third film was produced using an AlCl 3 /TiCl 4 precursor ratio of ∼1.9, resulting in the formation of an optimized lamellar microstructure with ∼1.3 nm thick cubic Ti(Al)N and ∼12 nm thick cubic Al(Ti)N nanolamellae which exhibits a maximal hardness of ∼36 GPa and an indentation modulus of ∼522 GPa. The presented approach of an iterative nanoscale search based on the application of cross-sectional synchrotron X-ray nanodiffraction and cross-sectional nanoindentation allows one to refine the relationship between (i) varying deposition conditions, (ii) gradients of microstructure and (iii) gradients of mechanical properties in nanostructured materials prepared as thin films. This is done in a combinatorial way in order to screen a wide range of deposition conditions, while identifying those that result in the formation of a particular microstructure with optimized functional attributes.

Application of Laser Plasma Sources of Soft X-rays and Extreme Ultraviolet (EUV) in Imaging, Processing Materials and Photoionization Studies

NASA Astrophysics Data System (ADS)

Fiedorowicz, H.; Bartnik, A.; Wachulak, P. W.; Jarocki, R.; Kostecki, J.; Szczurek, M.; Ahad, I. U.; Fok, T.; Szczurek, A.; Wȩgrzyński, Ł.

In the paper we present new applications of laser plasma sources of soft X-rays and extreme ultraviolet (EUV) in various areas of plasma physics, nanotechnology and biomedical engineering. The sources are based on a gas puff target irradiated with nanosecond laser pulses from commercial Nd: YAG lasers, generating pulses with time duration from 1 to 10 ns and energies from 0.5 to 10 J at a 10 Hz repetition rate. The targets are produced with the use of a double valve system equipped with a special nozzle to form a double-stream gas puff target which allows for high conversion efficiency of laser energy into soft X-rays and EUV without degradation of the nozzle. The sources are equipped with various optical systems to collect soft X-ray and EUV radiation and form the radiation beam. New applications of these sources in imaging, including EUV tomography and soft X-ray microscopy, processing of materials and photoionization studies are presented.

Direct X-ray detection with hybrid solar cells based on organolead halide perovskites

NASA Astrophysics Data System (ADS)

Gill, Hardeep Singh; Elshahat, Bassem; Sajo, Erno; Kumar, Jayant; Kokil, Akshay; Zygmanski, Piotr; Li, Lian; Mosurkal, Ravi

2014-03-01

Organolead halide perovskite materials are attracting considerable interest due to their exceptional opto-electronic properties, such as, high charge carrier mobilities, high exciton diffusion length, high extinction coefficients and broad-band absorption. These interesting properties have enabled their application in high performance hybrid photovoltaic devices. The high Z value of their constituents also makes these materials efficient for absorbing X-rays. Here we will present on the efficient use of hybrid solar cells based on organolead perovskite materials as X-ray detectors. Hybrid solar cells based on CH3NH3PbI3 were fabricated using facile processing techniques on patterned indium tin oxide coated glass substrates. The solar cells typically had a planar configuration of ITO/CH3NH3PbI3/P3HT/Ag. High sensitivity for X-rays due to high Z value, larger carrier mobility and better charge collection was observed. Detecting X-rays with energies relevant to medical oncology applications opens up the potential for diagnostic imaging applications.

Advanced Methods of Nondestructive Inspection of Composite Structures Based on Limited Angle X-Ray Computed Tomography

NASA Astrophysics Data System (ADS)

Bostaph, Ekaterina

This research aimed to study the potential for breaking through object size limitations of current X-ray computed tomography (CT) systems by implementing a limited angle scanning technique. CT stands out among other industrial nondestructive inspection (NDI) methods due to its unique ability to perform 3D volumetric inspection, unmatched micro-focus resolution, and objectivity that allows for automated result interpretation. This work attempts to advance NDI technique to enable microstructural material characterization and structural diagnostics of composite structures, where object sizes often prohibit the application of full 360° CT. Even in situations where the objects can be accommodated within existing micro-CT configuration, achieving sufficient magnification along with full rotation may not be viable. An effort was therefore made to achieve high-resolution scans from projection datasets with limited angular coverage (less than 180°) by developing effective reconstruction algorithms in conjunction with robust scan acquisition procedures. Internal features of inspected objects barely distinguishable in a 2D X-ray radiograph can be enhanced by additional projections that are reconstructed to a stack of slices, dramatically improving depth perception, a technique referred to as digital tomosynthesis. Building on the success of state-of-the-art medical tomosynthesis systems, this work sought to explore the feasibility of this technique for composite structures in aerospace applications. The challenge lies in the fact that the slices generated in medical tomosynthesis are too thick for relevant industrial applications. In order to adapt this concept to composite structures, reconstruction algorithms were expanded by implementation of optimized iterative stochastic methods (capable of reducing noise and refining scan quality) which resulted in better depth perception. The optimal scan acquisition procedure paired with the improved reconstruction algorithm facilitated higher in-plane and depth resolution compared to the clinical application. The developed limited angle tomography technique was demonstrated to be able to detect practically significant manufacturing defects (voids) and structural damage (delaminations) critical to structural integrity of composite parts. Keeping in mind the intended real-world aerospace applications where objects often have virtually unlimited in-plane dimensions, the developed technique of partial scanning could potentially extend the versatility of CT-based inspection and enable game changing NDI systems.

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.

High temperature x-ray micro-tomography

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

MacDowell, Alastair A., E-mail: aamacdowell@lbl.gov; Barnard, Harold; Parkinson, Dilworth Y.

2016-07-27

There is increasing demand for 3D micro-scale time-resolved imaging of samples in realistic - and in many cases extreme environments. The data is used to understand material response, validate and refine computational models which, in turn, can be used to reduce development time for new materials and processes. Here we present the results of high temperature experiments carried out at the x-ray micro-tomography beamline 8.3.2 at the Advanced Light Source. The themes involve material failure and processing at temperatures up to 1750°C. The experimental configurations required to achieve the requisite conditions for imaging are described, with examples of ceramic matrixmore » composites, spacecraft ablative heat shields and nuclear reactor core Gilsocarbon graphite.« less

Prospects for AGN Science using the ART-XC on the SRG Mission

NASA Technical Reports Server (NTRS)

Swartz, Douglas A.; Elsner, Ronald F.; Gubarev, Mikhail V.; O'Dell, Stephen L.; Ramsey, Brian D.; Bonamente, Massimiliano

2012-01-01

The enhanced hard X-ray sensitivity provided by the Astronomical Roentgen Telescope to the Spectrum Roentgen Gamma mission facilitates the detection of heavily obscured and other hard-spectrum cosmic X-ray sources. The SRG all-sky survey will obtain large, statistically-well-defined samples of active galactic nuclei (AGN) including a significant population of local heavily-obscured AGN. In anticipation of the SRG all-sky survey, we investigate the prospects for refining the bright end of the AGN luminosity function and determination of the local black hole mass function and comparing the spatial distribution of AGN with large-scale structure defined by galaxy clusters and groups. Particular emphasis is placed on studies of the deep survey Ecliptic Pole regions.

Electronic structure modifications and band gap narrowing in Zn0.95V0.05O

NASA Astrophysics Data System (ADS)

Ahad, Abdul; Majid, S. S.; Rahman, F.; Shukla, D. K.; Phase, D. M.

2018-04-01

We present here, structural, optical and electronic structure studies on Zn0.95V0.05O, synthesized using solid state method. Rietveld refinement of x-ray diffraction pattern indicates no considerable change in the lattice of doped ZnO. The band gap of doped sample, as calculated by Kubelka-Munk transformed reflectance spectra, has been found reduced compared to pure ZnO. Considerable changes in absorbance in UV-Vis range is observed in doped sample. V doping induced decrease in band gap is supported by x-ray absorption spectroscopy measurements. It is experimentally confirmed that conduction band edge in Zn0.95V0.05O has shifted towards Fermi level than in pure ZnO.

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

Measuring and modeling diffuse scattering in protein X-ray crystallography

PubMed Central

Van Benschoten, Andrew H.; Liu, Lin; Gonzalez, Ana; Brewster, Aaron S.; Sauter, Nicholas K.; Wall, Michael E.

2016-01-01

X-ray diffraction has the potential to provide rich information about the structural dynamics of macromolecules. To realize this potential, both Bragg scattering, which is currently used to derive macromolecular structures, and diffuse scattering, which reports on correlations in charge density variations, must be measured. Until now, measurement of diffuse scattering from protein crystals has been scarce because of the extra effort of collecting diffuse data. Here, we present 3D measurements of diffuse intensity collected from crystals of the enzymes cyclophilin A and trypsin. The measurements were obtained from the same X-ray diffraction images as the Bragg data, using best practices for standard data collection. To model the underlying dynamics in a practical way that could be used during structure refinement, we tested translation–libration–screw (TLS), liquid-like motions (LLM), and coarse-grained normal-modes (NM) models of protein motions. The LLM model provides a global picture of motions and was refined against the diffuse data, whereas the TLS and NM models provide more detailed and distinct descriptions of atom displacements, and only used information from the Bragg data. Whereas different TLS groupings yielded similar Bragg intensities, they yielded different diffuse intensities, none of which agreed well with the data. In contrast, both the LLM and NM models agreed substantially with the diffuse data. These results demonstrate a realistic path to increase the number of diffuse datasets available to the wider biosciences community and indicate that dynamics-inspired NM structural models can simultaneously agree with both Bragg and diffuse scattering. PMID:27035972

Measuring and modeling diffuse scattering in protein X-ray crystallography

DOE PAGES

Van Benschoten, Andrew H.; Liu, Lin; Gonzalez, Ana; ...

2016-03-28

X-ray diffraction has the potential to provide rich information about the structural dynamics of macromolecules. To realize this potential, both Bragg scattering, which is currently used to derive macromolecular structures, and diffuse scattering, which reports on correlations in charge density variations, must be measured. Until now, measurement of diffuse scattering from protein crystals has been scarce because of the extra effort of collecting diffuse data. Here, we present 3D measurements of diffuse intensity collected from crystals of the enzymes cyclophilin A and trypsin. The measurements were obtained from the same X-ray diffraction images as the Bragg data, using best practicesmore » for standard data collection. To model the underlying dynamics in a practical way that could be used during structure refinement, we tested translation–libration–screw (TLS), liquid-like motions (LLM), and coarse-grained normal-modes (NM) models of protein motions. The LLM model provides a global picture of motions and was refined against the diffuse data, whereas the TLS and NM models provide more detailed and distinct descriptions of atom displacements, and only used information from the Bragg data. Whereas different TLS groupings yielded similar Bragg intensities, they yielded different diffuse intensities, none of which agreed well with the data. In contrast, both the LLM and NM models agreed substantially with the diffuse data. In conclusion, these results demonstrate a realistic path to increase the number of diffuse datasets available to the wider biosciences community and indicate that dynamics-inspired NM structural models can simultaneously agree with both Bragg and diffuse scattering.« less

Developments in x-ray tomography I - IX

NASA Astrophysics Data System (ADS)

Stock, S. R.

2016-10-01

Nine Developments in X-ray Tomography conferences have been held previously, and this paper summarizes data from these conference proceedings. The Developments conference provides snapshots of the x-ray tomography field which spans clinical and biological applications, engineering and industrial studies and physical sciences.

Infrared Applications of Semiconductors II: Symposium Held in Boston, Massachusetts on December 1-4, 1997

DTIC Science & Technology

1997-12-01

James (Academic Press, San Diego, CA 1995) pp. 335-381. 2. J. R. Heffelfinger, D. L. Medlin, H. Yoon, H. Hermon and R. B. James, in Hard X - ray and...J. P. Cozzatti and J. P. Schomer, in Hard X - ray and Gamma-rav Detector Physics. Optics and Application, edited by R. B. Hoover and F. P. Doty (SPIE...resolution compared to the best previous instrumentation in hard x - ray and gamma ray astronomy. Previous work has shown the good imaging and

Indus-2 X-ray lithography beamline for X-ray optics and material science applications

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

Dhamgaye, V. P., E-mail: vishal@rrcat.gov.in; Lodha, G. S., E-mail: vishal@rrcat.gov.in

2014-04-24

X-ray lithography is an ideal technique by which high aspect ratio and high spatial resolution micro/nano structures are fabricated using X-rays from synchrotron radiation source. The technique has been used for fabricating optics (X-ray, visible and infrared), sensors and actuators, fluidics and photonics. A beamline for X-ray lithography is operational on Indus-2. The beamline offers wide lithographic window from 1-40keV photon energy and wide beam for producing microstructures in polymers upto size ∼100mm × 100mm. X-ray exposures are possible in air, vacuum and He gas environment. The air based exposures enables the X-ray irradiation of resist for lithography and alsomore » irradiation of biological and liquid samples.« less

A compact high-speed pnCCD camera for optical and x-ray applications

NASA Astrophysics Data System (ADS)

Ihle, Sebastian; Ordavo, Ivan; Bechteler, Alois; Hartmann, Robert; Holl, Peter; Liebel, Andreas; Meidinger, Norbert; Soltau, Heike; Strüder, Lothar; Weber, Udo

2012-07-01

We developed a camera with a 264 × 264 pixel pnCCD of 48 μm size (thickness 450 μm) for X-ray and optical applications. It has a high quantum efficiency and can be operated up to 400 / 1000 Hz (noise≍ 2:5 ° ENC / ≍4:0 ° ENC). High-speed astronomical observations can be performed with low light levels. Results of test measurements will be presented. The camera is well suitable for ground based preparation measurements for future X-ray missions. For X-ray single photons, the spatial position can be determined with significant sub-pixel resolution.

Experimental Investigation of Material Flows Within FSWs Using 3D Tomography

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

Charles R. Tolle; Timothy A. White; Karen S. Miller

2008-06-01

There exists significant prior work using tracers or pre-placed hardened markers within friction stir welding (FSWing) to experimentally explore material flow within the FSW process. Our experiments replaced markers with a thin sheet of copper foil placed between the 6061 aluminum lap and butt joints that were then welded. The absorption characteristics of x-rays for copper and aluminum are significantly different allowing for non-destructive evaluation (NDE) methods such as x-ray computed tomography (CT) to be used to demonstrate the material movement within the weldment on a much larger scale than previously shown. 3D CT reconstruction of the copper components ofmore » the weldment allows for a unique view into the final turbulent state of the welding process as process parameters are varied. The x-ray CT data of a section of the weld region was collected using a cone-beam x-ray imaging system developed at the INL. Six-hundred projections were collected over 360-degrees using a 160-kVp Bremsstrahlung x-ray generator (25-micrometer focal spot) and amorphoussilicon x-ray detector. The region of the object that was imaged was about 3cm tall and 1.5cm x 1cm in cross section, and was imaged at a magnification of about 3.6x. The data were reconstructed on a 0.5x0.5x0.5 mm3 voxel grid. After reconstruction, the aluminum and copper could be easily discriminated using a gray level threshold allowing visualization of the copper components. Fractal analysis of the tomographic reconstructed material topology is investigated as a means to quantify macro level material flow based on process parameters. The results of multi-pass FSWs show increased refinement of the copper trace material. Implications of these techniques for quantifying process flow are discussed.« less

Structure refinement for tantalum nitrides nanocrystals with various morphologies

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

Liu, Lianyun; School of Science, Beijing Jiaotong University, 3 Shang Yuan Cun, Haidian District, Beijing 100044; Huang, Kai

2012-07-15

Graphical abstract: Tantalum nitrides nanocrystals with various phases and morphologies for the first time have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. Highlights: ► The spherical TaN, cuboidal TaN{sub 0.83} and TaN{sub 0.5} nanocrystals have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. ► The crystal structures of different tantalum nitrides were determined by Rietveld refinement on the X-ray diffraction data and the examinations of electron microcopies. ► The specific surface area of the tantalum nitrides powders was around 10 m{supmore » 2} g{sup −1}. ► Tantalum nitrides powders could be suitable for capacitor with high specific capacitance. -- Abstract: Tantalum nitrides (TaN{sub x}) nanocrystals with different phase and morphology have been synthesized through homogenous sodium reduction under low temperature with the subsequent annealing process under high vacuum. The crystal structures of tantalum nitrides were determined by Rietveld refinement based on the X-ray diffraction data. The morphologies of various tantalum nitrides nanocrystals in high quality were analyzed through the electron microcopies examinations. The spherical TaN nanoparticles, cuboidal TaN{sub 0.83} and TaN{sub 0.5} nanocrystals have been selectively prepared at different annealing temperatures. In addition, the specific surface areas of the tantalum nitrides nanocrystals measured by BET method were around 9.87–11.64 m{sup 2} g{sup −1}, indicating that such nano-sized tantalum nitrides could be suitable for capacitor with high specific capacitance.« less

Application of Mythen detector: In-situ XRD study on the thermal expansion behavior of metal indium

NASA Astrophysics Data System (ADS)

Du, Rong; Chen, ZhongJun; Cai, Quan; Fu, JianLong; Gong, Yu; Wu, ZhongHua

2016-07-01

A Mythen detector has been equipped at the beamline 4B9A of Beijing Synchrotron Radiation Facility (BSRF), which is expected to enable BSRF to perform time-resolved measurement of X-ray diffraction (XRD) full-profiles. In this paper, the thermal expansion behavior of metal indium has been studied by using the in-situ XRD technique with the Mythen detector. The indium was heated from 303 to 433 K with a heating rate of 2 K/min. The in-situ XRD full-profiles were collected with a rate of one profile per 10 seconds. Rietveld refinement was used to extract the structural parameters. The results demonstrate that these collected quasi-real-time XRD profiles can be well used for structural analysis. The metal indium was found to have a nonlinear thermal expansion behavior from room temperature to the melting point (429.65 K). The a-axis of the tetragonal unit cell expands with a biquadratic dependency on temperature, while the c-axis contracts with a cubic dependency on temperature. By the time-resolved XRD measurements, it was observed that the [200] preferred orientation can maintain to about 403.15 K. While (110) is the last and detectable crystal plane just before melting of the polycrystalline indium foil. This study is not only beneficial to the application of metal indium, but also exhibits the capacity of in-situ time-resolved XRD measurements at the X-ray diffraction station of BSRF.

Grain refinement and Lattice Imperfections in Commercial Aluminum Alloy Processed by Severe Plastic Deformation

NASA Astrophysics Data System (ADS)

Charfeddine, Saifeddine; Zehani, Karim; Besais, Lotfi; Korchef, Atef

2014-08-01

In the present work, investigations on the microstructure of an aluminum alloy that had been subjected to severe plastic deformation (SPD) by equal channel angular pressing (ECAP), filing and ball milling, were carried out using X-ray diffraction and scanning electron microscopy. SPD leads to lattice distortions, increased dislocation density and an intensive refinement of the microstructure. The refinement and lattice imperfections of the material are greatly affected by the deformation modes and loading performance occurring during SPD. During the milling, the dislocation annihilation increases at higher strains thereby resulting in a smaller crystallite size. After ECAP, the material manifests a strong shear texture and anisotropy of the deformation behavior. Strain anisotropy is less pronounced in filed and ball milled powder particles.

Next Generation X-Ray Optics: High-Resolution, Light-Weight, and Low-Cost

NASA Technical Reports Server (NTRS)

Zhang, William W.

2012-01-01

X-ray telescopes are essential to the future of x-ray astronomy. In this talk I will describe a comprehensive program to advance the technology for x-ray telescopes well beyond the state of the art represented by the three currently operating missions: Chandra, XMM-Newton, and Suzaku. This program will address the three key issues in making an x-ray telescope: (1) angular resolution, (2) effective area per unit mass, and (3) cost per unit effective area. The objectives of this technology program are (1) in the near term, to enable Explorer-class x-ray missions and an IXO-type mission, and (2) in the long term, to enable a flagship x-ray mission with sub-arcsecond angular resolution and multi-square-meter effective area, at an affordable cost. We pursue two approaches concurrently, emphasizing the first approach in the near term (2-5 years) and the second in the long term (4-10 years). The first approach is precision slumping of borosilicate glass sheets. By design and choice at the outset, this technique makes lightweight and low-cost mirrors. The development program will continue to improve angular resolution, to enable the production of 5-arcsecond x-ray telescopes, to support Explorer-class missions and one or more missions to supersede the original IXO mission. The second approach is precision polishing and light-weighting of single-crystal silicon mirrors. This approach benefits from two recent commercial developments: (1) the inexpensive and abundant availability of large blocks of monocrystalline silicon, and (2) revolutionary advances in deterministic, precision polishing of mirrors. By design and choice at the outset, this technique is capable of producing lightweight mirrors with sub-arcsecond angular resolution. The development program will increase the efficiency and reduce the cost of the polishing and the light-weighting processes, to enable the production of lightweight sub-arcsecond x-ray telescopes. Concurrent with the fabrication of lightweight mirror segments is the continued development and perfection of alignment and integration techniques, for incorporating individual mirror segments into a precision mirror assembly. Recently, we have been developing a technique called edge-bonding, which has achieved an accuracy to enable 10-arcsecond x-ray telescopes. Currently, we are investigating and improving the long-term alignment stability of so-bonded mirrors. Next, we shall refine this process to enable 5-arsecond x-ray telescopes. This technology development program includes all elements to demonstrate progress toward TRL-6: metrology; x-ray performance tests; coupled structural, thermal, and optical performance analysis, and environmental testing.

Next Generation X-Ray Optics: High-Resolution, Light-Weight, and Low-Cost

NASA Technical Reports Server (NTRS)

Zhang, William W.

2011-01-01

X-ray telescopes are essential to the future of x-ray astronomy. This paper describes a comprehensive program to advance the technology for x-ray telescopes well beyond the state of the art represented by the three currently operating missions: Chandra, XMM-Newton , and Suzaku . This program will address the three key issues in making an x-ray telescope: (I) angular resolution, (2) effective area per unit mass, and (3) cost per unit effective area. The objectives of this technology program are (1) in the near term, to enable Explorer-class x-ray missions and an IXO type mission, and (2) in the long term, to enable a flagship x-ray mission with sub-arcsecond angular resolution and multi-square-meter effective area, at an affordable cost. We pursue two approaches concurrently, emphasizing the first approach in the near term (2-5 years) and the second in the long term (4-10 years). The first approach is precision slumping of borosilicate glass sheets. By design and choice at the outset, this technique makes lightweight and low-cost mirrors. The development program will continue to improve angular resolution, to enable the production of 5-arcsecond x-ray telescopes, to support Explorer-class missions and one or more missions to supersede the original IXO mission. The second approach is precision polishing and light-weighting of single-crystal silicon mirrors. This approach benefits from two recent commercial developments: (1) the inexpensive and abundant availability of large blocks of mono crystalline silicon, and (2) revolutionary advances in deterministic, precision polishing of mirrors. By design and choice at the outset, this technique is capable of producing lightweight mirrors with sub-arcsecond angular resolution. The development program will increase the efficiency and reduce the cost of the polishing and the lightweighting processes, to enable the production of lightweight sub-arcsecond x-ray telescopes. Concurrent with the fabrication of lightweight mirror segments is the continued development and perfection of alignment and integration techniques, for incorporating individual mirror segments into a precision mirror assembly. Recently, we have been developing a technique called edge-bonding, which has achieved an accuracy to enable 10- arcsecond x-ray telescopes. Currently, we are investigating and improving the long-term alignment stability of so-bonded mirrors. Next, we shall refine this process to enable 5-arsecond x-ray telescopes. This technology development program includes all elements to demonstrate progress toward TRL-6: metrology; x-ray performance tests; coupled structural, thermal, and optical performance analysis, and environmental testing.

Medical X-ray sources now and for the future

NASA Astrophysics Data System (ADS)

Behling, Rolf

2017-11-01

This paper focuses on the use of X-rays in their largest field of application: medical diagnostic imaging and image-guided therapy. For this purpose, vacuum electronics in the form of X-ray tubes as the source of bremsstrahlung (braking radiation) have been the number one choice for X-ray production in the range of photon energies between about 16 keV for mammography and 150 keV for general radiography. Soft tissue on one end and bony structures on the other are sufficiently transparent and the contrast delivered by difference of absorption is sufficiently high for this spectral range. The dominance of X-ray tubes holds even more than 120 years after Conrad Roentgen's discovery of the bremsstrahlung mechanism. What are the specifics of current X-ray tubes and their medical diagnostic applications? How may the next available technology at or beyond the horizon look like? Can we hope for substantial game changers? Will flat panel sources, less expensive X-ray "LED's", compact X-ray Lasers, compact synchrotrons or equivalent X-ray sources appear in medical diagnostic imaging soon? After discussing the various modalities of imaging systems and their sources of radiation, this overview will briefly touch on the physics of bremsstrahlung generation, key characteristics of X-ray tubes, and material boundary conditions, which restrict performance. It will discuss the deficits of the bremsstrahlung technology and try to sketch future alternatives and their prospects of implementation in medical diagnostics.

Ultrafast secondary emission X-ray imaging detectors: A possible application to TRD

NASA Astrophysics Data System (ADS)

Akkerman, A.; Breskin, A.; Chechik, R.; Elkind, V.; Gibrekhterman, A.; Majewski, S.

1992-05-01

Fist high accuracy, X-ray imaging at high photon flux can be achieved when coupling thin solid convertors to gaseous electron multipliers, operating at low gas pressures. Secondary electrons emitted from the convertor foil are multiplied in several successive amplification elements. The obvious advantages of solid X-ray convertors, as compared to gaseous conversion, are the production of parallax-free images and the fast (subnanosecond) response. These X-ray detectors have many potential applications in basic and applied research. Of particular interest is the possibility of an efficient and ultrafast high resolution imaging of transition radiation (TR), with a reduced d E/d x background. We present experimental results on the operation of secondary emission X-ray (SEX) detectors, their detection efficiency, localization and time resolution. The experimental work is accompanied by mathematical modelling and computer simulation of transition radiation detectors (TRDs) based on CsI TR convertors.

New contrasts for x-ray imaging and synergy with optical imaging

NASA Astrophysics Data System (ADS)

Wang, Ge

2017-02-01

Due to its penetrating power, fine resolution, unique contrast, high-speed, and cost-effectiveness, x-ray imaging is one of the earliest and most popular imaging modalities in biomedical applications. Current x-ray radiographs and CT images are mostly on gray-scale, since they reflect overall energy attenuation. Recent advances in x-ray detection, contrast agent, and image reconstruction technologies have changed our perception and expectation of x-ray imaging capabilities, and generated an increasing interest in imaging biological soft tissues in terms of energy-sensitive material decomposition, phase-contrast, small angle scattering (also referred to as dark-field), x-ray fluorescence and luminescence properties. These are especially relevant to preclinical and mesoscopic studies, and potentially mendable for hybridization with optical molecular tomography. In this article, we review new x-ray imaging techniques as related to optical imaging, suggest some combined x-ray and optical imaging schemes, and discuss our ideas on micro-modulated x-ray luminescence tomography (MXLT) and x-ray modulated opto-genetics (X-Optogenetics).

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.

Towards shot-noise limited diffraction experiments with table-top femtosecond hard x-ray sources.

PubMed

Holtz, Marcel; Hauf, Christoph; Weisshaupt, Jannick; Salvador, Antonio-Andres Hernandez; Woerner, Michael; Elsaesser, Thomas

2017-09-01

Table-top laser-driven hard x-ray sources with kilohertz repetition rates are an attractive alternative to large-scale accelerator-based systems and have found widespread applications in x-ray studies of ultrafast structural dynamics. Hard x-ray pulses of 100 fs duration have been generated at the Cu K α wavelength with a photon flux of up to 10 9 photons per pulse into the full solid angle, perfectly synchronized to the sub-100-fs optical pulses from the driving laser system. Based on spontaneous x-ray emission, such sources display a particular noise behavior which impacts the sensitivity of x-ray diffraction experiments. We present a detailed analysis of the photon statistics and temporal fluctuations of the x-ray flux, together with experimental strategies to optimize the sensitivity of optical pump/x-ray probe experiments. We demonstrate measurements close to the shot-noise limit of the x-ray source.

Towards shot-noise limited diffraction experiments with table-top femtosecond hard x-ray sources

PubMed Central

Holtz, Marcel; Hauf, Christoph; Weisshaupt, Jannick; Salvador, Antonio-Andres Hernandez; Woerner, Michael; Elsaesser, Thomas

2017-01-01

Table-top laser-driven hard x-ray sources with kilohertz repetition rates are an attractive alternative to large-scale accelerator-based systems and have found widespread applications in x-ray studies of ultrafast structural dynamics. Hard x-ray pulses of 100 fs duration have been generated at the Cu Kα wavelength with a photon flux of up to 109 photons per pulse into the full solid angle, perfectly synchronized to the sub-100-fs optical pulses from the driving laser system. Based on spontaneous x-ray emission, such sources display a particular noise behavior which impacts the sensitivity of x-ray diffraction experiments. We present a detailed analysis of the photon statistics and temporal fluctuations of the x-ray flux, together with experimental strategies to optimize the sensitivity of optical pump/x-ray probe experiments. We demonstrate measurements close to the shot-noise limit of the x-ray source. PMID:28795079

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.

High-resolution x-ray imaging for microbiology at the Advanced Photon Source

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

Lai, B.; Kemner, K. M.; Maser, J.

1999-11-02

Exciting new applications of high-resolution x-ray imaging have emerged recently due to major advances in high-brilliance synchrotrons sources and high-performance zone plate optics. Imaging with submicron resolution is now routine with hard x-rays: the authors have demonstrated 150 run in the 6--10 keV range with x-ray microscopes at the Advanced Photon Source (APS), a third-generation synchrotrons radiation facility. This has fueled interest in using x-ray imaging in applications ranging from the biomedical, environmental, and materials science fields to the microelectronics industry. One important application they have pursued at the APS is a study of the microbiology of bacteria and theirmore » associated extracellular material (biofilms) using fluorescence microanalysis. No microscopy techniques were previously available with sufficient resolution to study live bacteria ({approx}1 {micro}m x 4 {micro}m in size) and biofilms in their natural hydrated state with better than part-per-million elemental sensitivity and the capability of determining g chemical speciation. In vivo x-ray imaging minimizes artifacts due to sample fixation, drying, and staining. This provides key insights into the transport of metal contaminants by bacteria in the environment and potential new designs for remediation and sequestration strategies.« less

The application of x-ray, computed tomography, and magnetic resonance imaging on 22 pediatric Langerhans cell histiocytosis patients with long bone involvement: A retrospective analysis.

PubMed

Zhang, Xiaojun; Zhou, Jing; Chai, Xuee; Chen, Guiling; Guo, Bin; Ni, Lei; Wu, Peng

2018-04-01

The studies focusing on x-ray, computed tomography (CT), and magnetic resonance imaging (MRI) in pediatric Langerhans cell histiocytosis (LCH) patients were still rare. Therefore, we aimed to evaluate the application of x-ray, CT, and MRI in pediatric LCH patients with long bone involvement.Total 22 pediatric LCH patients were included in this study. The diagnosis of LCH was confirmed by pathological examination. All patients were followed up for 3 years. X-ray, CT, or MRI was performed and the results were recorded for further analyses.Among 22 pediatric patients, x-ray (n = 20), CT (n = 18), or MRI (n = 12) were used to scan the lesion on long bones affected by LCH. Femurs (n = 13, 38.24%), tibia (n = 11, 32.35%), humerus (n = 5, 14.71%), and radius (n = 4, 11.76%) were the most frequently affected anatomic sites. Ovoid or round radiolucent lesions, aggressive periosteal reaction, and swelling of surrounding soft tissues were characteristic image of long bones on x-ray, CT, and MRI in pediatric LCH.Femurs, tibia, humerus, and radius were the most commonly affected long bones of pediatric LCH. The application of x-ray, CT, and MRI on long bones could help with the diagnosis of pediatric LCH.

Spectral correction algorithm for multispectral CdTe x-ray detectors

NASA Astrophysics Data System (ADS)

Christensen, Erik D.; Kehres, Jan; Gu, Yun; Feidenhans'l, Robert; Olsen, Ulrik L.

2017-09-01

Compared to the dual energy scintillator detectors widely used today, pixelated multispectral X-ray detectors show the potential to improve material identification in various radiography and tomography applications used for industrial and security purposes. However, detector effects, such as charge sharing and photon pileup, distort the measured spectra in high flux pixelated multispectral detectors. These effects significantly reduce the detectors' capabilities to be used for material identification, which requires accurate spectral measurements. We have developed a semi analytical computational algorithm for multispectral CdTe X-ray detectors which corrects the measured spectra for severe spectral distortions caused by the detector. The algorithm is developed for the Multix ME100 CdTe X-ray detector, but could potentially be adapted for any pixelated multispectral CdTe detector. The calibration of the algorithm is based on simple attenuation measurements of commercially available materials using standard laboratory sources, making the algorithm applicable in any X-ray setup. The validation of the algorithm has been done using experimental data acquired with both standard lab equipment and synchrotron radiation. The experiments show that the algorithm is fast, reliable even at X-ray flux up to 5 Mph/s/mm2, and greatly improves the accuracy of the measured X-ray spectra, making the algorithm very useful for both security and industrial applications where multispectral detectors are used.

Tomographic image via background subtraction using an x-ray projection image and a priori computed tomography

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

Zhang Jin; Yi Byongyong; Lasio, Giovanni

Kilovoltage x-ray projection images (kV images for brevity) are increasingly available in image guided radiotherapy (IGRT) for patient positioning. These images are two-dimensional (2D) projections of a three-dimensional (3D) object along the x-ray beam direction. Projecting a 3D object onto a plane may lead to ambiguities in the identification of anatomical structures and to poor contrast in kV images. Therefore, the use of kV images in IGRT is mainly limited to bony landmark alignments. This work proposes a novel subtraction technique that isolates a slice of interest (SOI) from a kV image with the assistance of a priori information frommore » a previous CT scan. The method separates structural information within a preselected SOI by suppressing contributions to the unprocessed projection from out-of-SOI-plane structures. Up to a five-fold increase in the contrast-to-noise ratios (CNRs) was observed in selected regions of the isolated SOI, when compared to the original unprocessed kV image. The tomographic image via background subtraction (TIBS) technique aims to provide a quick snapshot of the slice of interest with greatly enhanced image contrast over conventional kV x-ray projections for fast and accurate image guidance of radiation therapy. With further refinements, TIBS could, in principle, provide real-time tumor localization using gantry-mounted x-ray imaging systems without the need for implanted markers.« less

Development of microchannel plate x-ray optics

NASA Technical Reports Server (NTRS)

Kaaret, Philip

1995-01-01

The goal of this research program was to develop a novel technique for focusing x-rays based on the optical system of a lobster's eye. A lobster eye employs many closely packed reflecting surfaces arranged within a spherical or cylindrical shell. These optics have two unique properties: they have unlimited fields of view and can be manufactured via replication of identical structures. Because the angular resolution is given by the ratio of the size of the individual optical elements to the focal length, optical elements with size on the order of one hundred microns are required to achieve good angular resolution with a compact telescope. We employed anisotropic etching of single crystal silicon wafers for the fabrication of micron-scale optical elements. This technique, commonly referred to as silicon micromachining, is based on silicon fabrication techniques developed by the microelectronics industry. We have succeeded in producing silicon lenses with a geometry suitable for a 1-d focusing x-ray optics. These lenses have an aspect ratio (40:1) suitable for x-ray reflection and have very good optical surface alignment. We have developed a number of process refinements which improved the quality of the lens geometry and the repeatability of the etch process. In addition to the silicon fabrication, an x-ray beam line was constructed at Columbia for testing the optics. Most recently, we have done several experiments to find the fundamental limits that the anisotropic etch process placed on the etched surface roughness.

Overview of options for generating high-brightness attosecond x-ray pulses at free-electron lasers and applications at the European XFEL

NASA Astrophysics Data System (ADS)

Serkez, S.; Geloni, G.; Tomin, S.; Feng, G.; Gryzlova, E. V.; Grum-Grzhimailo, A. N.; Meyer, M.

2018-02-01

The generation of attosecond, highbrightness x-ray pulses is a matter of great interest given their applications in the study of ultra-fast processes. In recent years, the production of x-ray pulses of high brightness, both in the soft and in the hard x-ray range, has been enabled by x-ray free-electron lasers (XFELs). In contrast to conventional quantum lasers, XFELs are based on the use of an ultra-relativistic electron beam as gain medium. They often work in the self-amplified spontaneous emission (SASE) regime, which provides pulses of duration down to a few femtoseconds, composed of several longitudinal modes. In order to further decrease the duration of these pulses, special methods need to be implemented. In this paper we review available methods, with particular focus on the x-ray laser-enhanced attosecond pulse generation, which is one of the most promising techniques. We illustrate the method using the SASE3 soft x-ray undulator of the European XFEL facility as a case study, emphasizing the importance of high-repetition rate attosecond x-ray pulses. The expected attosecond-level radiation output is used for simulations of sequential ionization processes in atoms in the case of ionization in the soft x-ray regime, demonstrating the importance of this opportunity for the user community.

Magnesium Electrorefining in Non-Aqueous Electrolyte at Room Temperature

NASA Astrophysics Data System (ADS)

Kwon, Kyungjung; Park, Jesik; Kusumah, Priyandi; Dilasari, Bonita; Kim, Hansu; Lee, Churl Kyoung

Magnesium, of which application is often limited by its poor corrosion resistance, is more vulnerable to corrosion with existence of metal impurities such as Fe. Therefore, for the refining and recycling of magnesium, high temperature electrolysis using molten salts has been frequently adopted. In this report, the purification of magnesium scrap by electrolysis at room temperature is investigated with non-aqueous electrolytes. An aprotic solvent of tetrahydrofuran (THF) was used as a solvent of the electrolyte. Magnesium scrap was used as anode materials and ethyl magnesium bromide (EtMgBr) was dissolved in THF for magnesium source. The purified magnesium can be uniformly electrodeposited on copper electrode under potentiostatic conditions. The deposits were confirmed by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) analysis.

X-ray Echo Spectroscopy

NASA Astrophysics Data System (ADS)

Shvyd'ko, Yuri

2016-02-01

X-ray echo spectroscopy, a counterpart of neutron spin echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a pointlike x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-0.02 meV ultrahigh-resolution IXS applications (resolving power >108 ) with broadband ≃5 - 13 meV dispersing systems are introduced featuring more than 103 signal enhancement. The technique is general, applicable in different photon frequency domains.

Automatic SMT Inspection With -X-Ray Vision

NASA Astrophysics Data System (ADS)

Kuntz, Robert A.; Steinmetz, Peter D.

1988-02-01

X-ray is used in many different ways and in a broad variety of applications with today's world. One of the most obvious uses is in the medically related applications. Although less obvious, x-ray is used within industry as well. Inspection of metal castings, pipe-line welds, equipment structures and personal security are just a few. Historically, both medical and industrial x-ray have been dependent on film exposure, development and reading to capture and present the projected image. This process however is labor intensive, time consuming and costly. Correct exposure time and proper view orientation are in question until the film is developed and examined. In many cases, this trial and error causes retakes with the accompanying expense and delays. Recently, due to advances in x-ray tube technology, tubes with microfocus construction have become available. These tubes operate at high enough flux density such that when combined with x-ray to visible light converters, real-time imaging is possible.

Optics for coherent X-ray applications.

PubMed

Yabashi, Makina; Tono, Kensuke; Mimura, Hidekazu; Matsuyama, Satoshi; Yamauchi, Kazuto; Tanaka, Takashi; Tanaka, Hitoshi; Tamasaku, Kenji; Ohashi, Haruhiko; Goto, Shunji; Ishikawa, Tetsuya

2014-09-01

Developments of X-ray optics for full utilization of diffraction-limited storage rings (DLSRs) are presented. The expected performance of DLSRs is introduced using the design parameters of SPring-8 II. To develop optical elements applicable to manipulation of coherent X-rays, advanced technologies on precise processing and metrology were invented. With propagation-based coherent X-rays at the 1 km beamline of SPring-8, a beryllium window fabricated with the physical-vapour-deposition method was found to have ideal speckle-free properties. The elastic emission machining method was utilized for developing reflective mirrors without distortion of the wavefronts. The method was further applied to production of diffraction-limited focusing mirrors generating the smallest spot size in the sub-10 nm regime. To enable production of ultra-intense nanobeams at DLSRs, a low-vibration cooling system for a high-heat-load monochromator and advanced diagnostic systems to characterize X-ray beam properties precisely were developed. Finally, new experimental schemes for combinative nano-analysis and spectroscopy realised with novel X-ray optics are discussed.

Emerging trends in X-ray spectroscopic studies of plasma produced by intense laser beams

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

Arora, V., E-mail: arora@rrcat.gov.in; Chakera, J. A.; Naik, P. A.

2015-07-31

X-ray line emission from hot dense plasmas, produced by ultra-short high intensity laser systems, has been studied experimentally in recent years for applications in materials science as well as for back-lighter applications. By virtue of the CPA technology, several laser facilities delivering pulses with peak powers in excess of one petawatt (focused intensities > 10{sup 20} W-cm{sup −2}) have either been commissioned across the globe during the last few years or are presently under construction. On the other hand, hard x-ray sources on table top, generating ultra-short duration x-rays at a repetition rate up to 10 kHz, are routinely available formore » time resolved x-ray diffraction studies. In this paper, the recent experiments on x-ray spectroscopic studies of plasma produced by 45 fs, Ti:sapphire laser pulses (focused iintensity > 10{sup 18} W-cm{sup −2}) at RRCAT Indore will be presented.« less

Separation of Lead from Crude Antimony by Pyro-Refining Process with NaPO3 Addition

NASA Astrophysics Data System (ADS)

Ye, Longgang; Hu, Yuejie; Xia, Zhimei; Chen, Yongming

2016-06-01

The main purpose of this study was to separate lead from crude antimony through an oxidation pyro-refining process and by using sodium metaphosphate as a lead elimination reagent. The process parameters that will affect the refining results were optimized experimentally under controlled conditions, such as the sodium metaphosphate charging dosage, the refining temperature and duration, and the air flow rate, to determine their effect on the lead content in refined antimony and the lead removal rate. A minimum lead content of 0.0522 wt.% and a 98.6% lead removal rate were obtained under the following optimal conditions: W_{{{NaPO}_{{3}} }} = 15% W Sb (where W represents weight), a refining temperature of 800°C, a refining time of 30 min, and an air flow rate of 3 L/min. X-ray diffractometry and scanning electron microscopy showed that high-purity antimony was obtained. The smelting operation is free from smoke or ammonia pollution when using monobasic sodium phosphate or ammonium dihydrogen phosphate as the lead elimination reagent. However, this refining process can also remove a certain amount of sulfur, cobalt, and silicon simultaneously, and smelting results also suggest that sodium metaphosphate can be used as a potential lead elimination reagent for bismuth and copper refining.

Advanced Computational Methods for High-accuracy Refinement of Protein Low-quality Models

NASA Astrophysics Data System (ADS)

Zang, Tianwu

Predicting the 3-dimentional structure of protein has been a major interest in the modern computational biology. While lots of successful methods can generate models with 3˜5A root-mean-square deviation (RMSD) from the solution, the progress of refining these models is quite slow. It is therefore urgently needed to develop effective methods to bring low-quality models to higher-accuracy ranges (e.g., less than 2 A RMSD). In this thesis, I present several novel computational methods to address the high-accuracy refinement problem. First, an enhanced sampling method, named parallel continuous simulated tempering (PCST), is developed to accelerate the molecular dynamics (MD) simulation. Second, two energy biasing methods, Structure-Based Model (SBM) and Ensemble-Based Model (EBM), are introduced to perform targeted sampling around important conformations. Third, a three-step method is developed to blindly select high-quality models along the MD simulation. These methods work together to make significant refinement of low-quality models without any knowledge of the solution. The effectiveness of these methods is examined in different applications. Using the PCST-SBM method, models with higher global distance test scores (GDT_TS) are generated and selected in the MD simulation of 18 targets from the refinement category of the 10th Critical Assessment of Structure Prediction (CASP10). In addition, in the refinement test of two CASP10 targets using the PCST-EBM method, it is indicated that EBM may bring the initial model to even higher-quality levels. Furthermore, a multi-round refinement protocol of PCST-SBM improves the model quality of a protein to the level that is sufficient high for the molecular replacement in X-ray crystallography. Our results justify the crucial position of enhanced sampling in the protein structure prediction and demonstrate that a considerable improvement of low-accuracy structures is still achievable with current force fields.

Study of the Polarization Properties of the Crab Nebula and Pulsar with BATSE

NASA Technical Reports Server (NTRS)

Forrest, David J.; Vestrand, W. T.; McConnell, Mark

1997-01-01

Activities carried out under this proposal included: 1) development and refinements of Monte Carlo simulations of the atmospheric reflected albedo hard x-ray emissions, both unpolarized and polarized, 2) modeling and simulations of the off-axis response of the BATSE LAD detectors, and 3) comparison of our simulation results with numerous BATSE flare and cosmic burst data sets.

Study of the specific features of single-crystal boron microstructure

NASA Astrophysics Data System (ADS)

Blagov, A. E.; Vasil'ev, A. L.; Dmitriev, V. P.; Ivanova, A. G.; Kulikov, A. G.; Marchenkov, N. V.; Popov, P. A.; Presnyakov, M. Yu.; Prosekov, P. A.; Pisarevskii, Yu. V.; Targonskii, A. V.; Chernaya, T. S.; Chernyshov, D. Yu.

2017-09-01

A complex study of the structure of β-boron single crystal grown by the floating-zone method, with sizes significantly exceeding the analogs known in the literature, has been performed. The study includes X-ray diffraction analysis and X-ray diffractometry (measurement of pole figures and rocking curves), performed on both laboratory and synchrotron sources; atomic-resolution scanning transmission electron microscopy with spherical aberration correction; and energy-dispersive microanalysis. X-ray diffraction analysis using synchrotron radiation has been used to refine the β-boron structure and find impurity Si atoms. The relative variations in the unit-cell parameters a and c for the crystal bulk are found to be δ a/ a ≈ 0.4 and δ c/ c ≈ 0.1%. X-ray diffractometry has revealed that the single-crystal growth axis coincides with the [2\\bar 2013] crystallographic axis and makes an angle of 21.12° with the [0001] threefold axis. Electron microscopy data have confirmed that the sample under study is a β-boron crystal, which may contain 0.3-0.4 at % Si as an impurity. Planar defects (stacking faults and dislocations) are found. The results of additional measurements of the temperature dependence of the thermal conductivity of the crystal in the range of 50-300 K are indicative of its high structural quality.

Hydrodynamic study of plasma amplifiers for soft-x-ray lasers: a transition in hydrodynamic behavior for plasma columns with widths ranging from 20 μm to 2 mm.

PubMed

Oliva, Eduardo; Zeitoun, Philippe; Velarde, Pedro; Fajardo, Marta; Cassou, Kevin; Ros, David; Sebban, Stephan; Portillo, David; le Pape, Sebastien

2010-11-01

Plasma-based seeded soft-x-ray lasers have the potential to generate high energy and highly coherent short pulse beams. Due to their high density, plasmas created by the interaction of an intense laser with a solid target should store the highest amount of energy density among all plasma amplifiers. Our previous numerical work with a two-dimensional (2D) adaptive mesh refinement hydrodynamic code demonstrated that careful tailoring of plasma shapes leads to a dramatic enhancement of both soft-x-ray laser output energy and pumping efficiency. Benchmarking of our 2D hydrodynamic code in previous experiments demonstrated a high level of confidence, allowing us to perform a full study with the aim of the way for 10-100 μJ seeded soft-x-ray lasers. In this paper, we describe in detail the mechanisms that drive the hydrodynamics of plasma columns. We observed transitions between narrow plasmas, where very strong bidimensional flow prevents them from storing energy, to large plasmas that store a high amount of energy. Millimeter-sized plasmas are outstanding amplifiers, but they have the limitation of transverse lasing. In this paper, we provide a preliminary solution to this problem.

Applications of synchrotron-based spectroscopic techniques in studying nucleic acids and nucleic acid-functionalized nanomaterials

PubMed Central

Wu, Peiwen; Yu, Yang; McGhee, Claire E.; Tan, Li Huey

2014-01-01

In this review, we summarize recent progresses in the application of synchrotron-based spectroscopic techniques for nucleic acid research that takes advantage of high-flux and high-brilliance electromagnetic radiation from synchrotron sources. The first section of the review focuses on the characterization of the structure and folding processes of nucleic acids using different types of synchrotron-based spectroscopies, such as X-ray absorption spectroscopy, X-ray emission spectroscopy, X-ray photoelectron spectroscopy, synchrotron radiation circular dichroism, X-ray footprinting and small-angle X-ray scattering. In the second section, the characterization of nucleic acid-based nanostructures, nucleic acid-functionalized nanomaterials and nucleic acid-lipid interactions using these spectroscopic techniques is summarized. Insights gained from these studies are described and future directions of this field are also discussed. PMID:25205057

Applications of synchrotron-based spectroscopic techniques in studying nucleic acids and nucleic acid-functionalized nanomaterials

DOE PAGES

Wu, Peiwen; Yu, Yang; McGhee, Claire E.; ...

2014-09-10

In this paper, we summarize recent progress in the application of synchrotron-based spectroscopic techniques for nucleic acid research that takes advantage of high-flux and high-brilliance electromagnetic radiation from synchrotron sources. The first section of the review focuses on the characterization of the structure and folding processes of nucleic acids using different types of synchrotron-based spectroscopies, such as X-ray absorption spectroscopy, X-ray emission spectroscopy, X-ray photoelectron spectroscopy, synchrotron radiation circular dichroism, X-ray footprinting and small-angle X-ray scattering. In the second section, the characterization of nucleic acid-based nanostructures, nucleic acid-functionalized nanomaterials and nucleic acid-lipid interactions using these spectroscopic techniques is summarized. Insightsmore » gained from these studies are described and future directions of this field are also discussed.« less

Real-time synchrotron x-ray observations of equiaxed solidification of aluminium alloys and implications for modelling

NASA Astrophysics Data System (ADS)

Prasad, A.; Liotti, E.; McDonald, S. D.; Nogita, K.; Yasuda, H.; Grant, P. S.; StJohn, D. H.

2015-06-01

Recently, in-situ observations were carried out by synchrotron X-ray radiography to observe the nucleation and growth in Al alloys during solidification. The nucleation and grain formation of a range of Al-Si and Al-Cu binary alloys were studied. When grain refiner was added to the alloys, the location of the nucleation events was readily observed. Once nucleation began it continued to occur in a wave of events with the movement of the temperature gradient across the field of view due to cooling. Other features observed were the settling of the primary phase grains in the Al-Si alloys and floating in the Al-Cu alloys, the effects of convection with marked fluctuation of the growth rate of the solid-liquid interface in the Al-Si alloys, and an absence of fragmentation. The microstructures are typical of those produced in the equiaxed zone of actual castings. These observations are compared with predictions arising from the Interdependence model. The results from this comparison have implications for further refinement of the model and simulation and modelling approaches in general. These implications will be discussed.

Structure refinement of the δ1p phase in the Fe-Zn system by single-crystal X-ray diffraction combined with scanning transmission electron microscopy.

PubMed

Okamoto, Norihiko L; Tanaka, Katsushi; Yasuhara, Akira; Inui, Haruyuki

2014-04-01

The structure of the δ1p phase in the iron-zinc system has been refined by single-crystal synchrotron X-ray diffraction combined with scanning transmission electron microscopy. The large hexagonal unit cell of the δ1p phase with the space group of P63/mmc comprises more or less regular (normal) Zn12 icosahedra, disordered Zn12 icosahedra, Zn16 icosioctahedra and dangling Zn atoms that do not constitute any polyhedra. The unit cell contains 52 Fe and 504 Zn atoms so that the compound is expressed with the chemical formula of Fe13Zn126. All Fe atoms exclusively occupy the centre of normal and disordered icosahedra. Iron-centred normal icosahedra are linked to one another by face- and vertex-sharing forming two types of basal slabs, which are bridged with each other by face-sharing with icosioctahedra, whereas disordered icosahedra with positional disorder at their vertex sites are isolated from other polyhedra. The bonding features in the δ1p phase are discussed in comparison with those in the Γ and ζ phases in the iron-zinc system.

Prediction of Cavitation Depth in an Al-Cu Alloy Melt with Bubble Characteristics Based on Synchrotron X-ray Radiography

NASA Astrophysics Data System (ADS)

Huang, Haijun; Shu, Da; Fu, Yanan; Zhu, Guoliang; Wang, Donghong; Dong, Anping; Sun, Baode

2018-06-01

The size of cavitation region is a key parameter to estimate the metallurgical effect of ultrasonic melt treatment (UST) on preferential structure refinement. We present a simple numerical model to predict the characteristic length of the cavitation region, termed cavitation depth, in a metal melt. The model is based on wave propagation with acoustic attenuation caused by cavitation bubbles which are dependent on bubble characteristics and ultrasonic intensity. In situ synchrotron X-ray imaging of cavitation bubbles has been made to quantitatively measure the size of cavitation region and volume fraction and size distribution of cavitation bubbles in an Al-Cu melt. The results show that cavitation bubbles maintain a log-normal size distribution, and the volume fraction of cavitation bubbles obeys a tanh function with the applied ultrasonic intensity. Using the experimental values of bubble characteristics as input, the predicted cavitation depth agrees well with observations except for a slight deviation at higher acoustic intensities. Further analysis shows that the increase of bubble volume and bubble size both leads to higher attenuation by cavitation bubbles, and hence, smaller cavitation depth. The current model offers a guideline to implement UST, especially for structural refinement.

Ottensite, brizziite and mopungite from Pereta mine (Tuscany, Italy): new occurrences and crystal structure refinement of mopungite

NASA Astrophysics Data System (ADS)

Bittarello, Erica; Cámara, Fernando; Ciriotti, Marco E.; Marengo, Alessandra

2015-08-01

Ottensite, Na3 (Sb2O3)(SbS3)·3H2O, brizziite, NaSbO3, and mopungite, NaSb(OH)6, have been found on several specimens from the antimony mine of Pereta (Grosseto, Tuscany, Italy). Ottensite from Pereta mine occurs as brilliant reddish-brown spheroidal aggregates, with a diameter up to 0.2 mm, formed by radially oriented individuals. These aggregates are associated with well-shaped tabular and pseudocubic colourless crystals of mopungite and platy aggregates of brizziite. This is the second world occurrence of ottensite and brizziite. The mineral species were characterized by electron microprobe analysis, X-ray diffraction study and microRaman spectroscopy. Single-crystal X-ray diffraction data were collected on a twinned crystal of mopungite and the structure was for the first time refined on a natural sample in space group P42/ n [unit cell parameters a = 8.036(3) Å, c = 7.926(6) Å, V = 511.88(5) Å3, Z = 4] obtaining an R 1 -index of 5.17, wR 2 of 13.52 and GooF of 1.247.

Effect of laser welding parameters on the austenite and martensite phase fractions of NiTi

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

Oliveira, J.P., E-mail: jp.oliveira@campus.fct.unl

Although laser welding is probably the most used joining technique for NiTi shape memory alloys there is still a lack of understanding about the effects of laser welding parameters on the microstructural induced changes: in both the heat affected and fusion zones martensite may be present, while the base material is fully austenitic. Synchrotron X-ray diffraction was used for fine probing laser welded NiTi joints. Through Rietveld refinement the martensite and austenite phase fractions were determined and it was observed that the martensite content increases towards the weld centreline. This is related to a change of the local transformation temperaturesmore » on these regions, which occurs due to compositional variation in those regions. The martensite phase fraction in the thermally affected regions may have significant implications on functional properties on these joints. - Highlights: •Synchrotron X-ray diffraction was used for fine probing of the microstructure in laser welded NiTi joints. •Rietveld refinement allowed to determine the content of martensite along the heat affected and fusion zones. •The martensite content increases from the base material towards the weld centreline.« less

Prediction of Cavitation Depth in an Al-Cu Alloy Melt with Bubble Characteristics Based on Synchrotron X-ray Radiography

NASA Astrophysics Data System (ADS)

Huang, Haijun; Shu, Da; Fu, Yanan; Zhu, Guoliang; Wang, Donghong; Dong, Anping; Sun, Baode

2018-04-01

The size of cavitation region is a key parameter to estimate the metallurgical effect of ultrasonic melt treatment (UST) on preferential structure refinement. We present a simple numerical model to predict the characteristic length of the cavitation region, termed cavitation depth, in a metal melt. The model is based on wave propagation with acoustic attenuation caused by cavitation bubbles which are dependent on bubble characteristics and ultrasonic intensity. In situ synchrotron X-ray imaging of cavitation bubbles has been made to quantitatively measure the size of cavitation region and volume fraction and size distribution of cavitation bubbles in an Al-Cu melt. The results show that cavitation bubbles maintain a log-normal size distribution, and the volume fraction of cavitation bubbles obeys a tanh function with the applied ultrasonic intensity. Using the experimental values of bubble characteristics as input, the predicted cavitation depth agrees well with observations except for a slight deviation at higher acoustic intensities. Further analysis shows that the increase of bubble volume and bubble size both leads to higher attenuation by cavitation bubbles, and hence, smaller cavitation depth. The current model offers a guideline to implement UST, especially for structural refinement.

Underestimated Halogen Bonds Forming with Protein Backbone in Protein Data Bank.

PubMed

Zhang, Qian; Xu, Zhijian; Shi, Jiye; Zhu, Weiliang

2017-07-24

Halogen bonds (XBs) are attracting increasing attention in biological systems. Protein Data Bank (PDB) archives experimentally determined XBs in biological macromolecules. However, no software for structure refinement in X-ray crystallography takes into account XBs, which might result in the weakening or even vanishing of experimentally determined XBs in PDB. In our previous study, we showed that side-chain XBs forming with protein side chains are underestimated in PDB on the basis of the phenomenon that the proportion of side-chain XBs to overall XBs decreases as structural resolution becomes lower and lower. However, whether the dominant backbone XBs forming with protein backbone are overlooked is still a mystery. Here, with the help of the ratio (R F ) of the observed XBs' frequency of occurrence to their frequency expected at random, we demonstrated that backbone XBs are largely overlooked in PDB, too. Furthermore, three cases were discovered possessing backbone XBs in high resolution structures while losing the XBs in low resolution structures. In the last two cases, even at 1.80 Å resolution, the backbone XBs were lost, manifesting the urgent need to consider XBs in the refinement process during X-ray crystallography study.

Structural and microstructural description of the glacial state in triphenyl phosphite from powder synchrotron X-ray diffraction data and Raman scattering investigations

NASA Astrophysics Data System (ADS)

Derollez, P.; Hernandez, O.; Hédoux, A.; Guinet, Y.; Masson, O.; Lefebvre, J.; Descamps, M.

2004-06-01

The structure and microstructure (refinement of the isotropic size and microstrain parameters) of the glacial state in triphenyl phosphite (TPP, P(OC 6H 5) 3) transformed at 222K have been determined from powder synchrotron X-ray diffraction data through a Rietveld and a Le Bail refinement, respectively. It is shown that the glacial state is composed of crystallites of the stable crystal phase coexisting with non-transformed supercooled liquid, the apparent size of the crystallites—depending on the aging temperature at which the glacial state is isothermally formed, [Phys. Rev. B 60 (1999) 9390]—being equal to 329.2(2) Å at 222K. The molecular conformation is slightly less mirror-symmetric than the one in the crystal state, and correlatively only one of the two unusual weak intermolecular C-H⋯O hydrogen bonds already observed in the latter state is encountered in the glacial one. Additional Raman scattering investigations confirm the previous result and reveal in addition that no hydrogen bonding interaction is observed neither in the glass nor in the liquid states.

[Determination of LF-VD refining furnace slag by X ray fluorescence spectrometry].

PubMed

Kan, Bin; Cheng, Jian-ping; Song, Zu-feng

2004-10-01

Eight components, i.e. TFe, CaO, MgO, Al2O3, SiO2, TiO2, MnO and P2O5 in refining furnace slag were determined by X ray fluorescence spectrometer. Because the content of CaO was high, the authors selected 12 national and departmental grade slag standard samples and prepared a series of synthetic standard samples by adding spectrally pure reagents to them. The calibration curve is suitable to the sample analysis of CaO, MgO and SiO2 with widely varying range. Meanwhile, the points on the curve are even. The samples were prepared at high temperature by adding Li2B4O7 as flux. The experiments for the selection of the sample preparation conditions about strip reagents, melting temperature and dulition ratio were carried out. The matrix effects on absorption and enhancement were corrected by means of PH model and theoretical alpha coefficient. Moreover, the precision and accuracy experiments were performed. In comparison with chemical analysis method, the quantitative analytical results for each component are satisfactory. The method has proven rapid, precise and simple.

Structure, microstructure and infrared studies of Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3}-NaNbO{sub 3} ceramics

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

Roy, Sumit K., E-mail: sumit.sxc13@gmail.com; Singh, S. N., E-mail: snsphyru@gmail.com; Prasad, K., E-mail: k.prasad65@gmail.com

2016-05-06

Lead-free solid solutions (1-x)Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3}-xNaNbO{sub 3} (0 ≤ x ≤ 1.0) were prepared by conventional ceramic fabrication technique. X-ray diffraction and Rietveld refinement analyses of these ceramics were carried out using X’Pert HighScore Plus software to determine the crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that NaNbO{sub 3} with orthorhombic structure was completely diffused into Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3} lattice having the rhombohedral-tetragonal symmetry. EDS and SEM studies were carried out in order to evaluate the quality and purity of the compounds. SEM images showed a change in grain shapemore » with the increase of NaNbO{sub 3} content. FTIR spectra confirmed the formation of solid solution.« less

Rietveld refinement and dielectric properties of (Na{sub 0.5}Bi{sub 0.5}TiO{sub 3})-(Bi{sub 0.8}Ba{sub 0.2}FeO{sub 3}) ceramics

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

Kaswan, Kavita, E-mail: kaswan.kavita@gmail.com; Agarwal, Ashish; Sanghi, Sujata

2015-06-24

(1-x)(Na{sub 0.5}Bi{sub 0.5}TiO{sub 3})-x(Bi{sub 0.8}Ba{sub 0.2}FeO{sub 3}) lead free ceramics (NBT, NBT-BBFO; x = 0.0, 0.1 respectively) have been synthesized by conventional solid state reaction method. Crystalline phase of sintered ceramics was investigated at room temperature using X-ray diffraction. Rietveld refinement of XRD data performed by FullProf revealed that both the samples exhibited rhombohedral structure with R3c space group. Dielectric properties of these ceramics were studied at different temperatures in a wide frequency range using impedance analyzer. Dielectric constant and dielectric loss were found to be increase with increase of BBFO content. The prepared ceramics exhibit a broad maximum inmore » dielectric permittivity at 593K and dispersive permittivity at high temperatures. The NBT-BBFO sample shows a relaxor ferroelectric behavior at different frequencies.« less

Crystallographic perturbations to valence charge density and hydrogen-surface interactions

NASA Astrophysics Data System (ADS)

Ciston, James W.

The subject of surfaces has been the epicenter of numerous studies in recent years, particularly with respect to applications in catalysis, thin films, and self-assembly of nanostructures where the surface-to-volume ratio is large. Understanding how the atomic structure of materials differs at surfaces where the atoms are far less constrained can yield fundamental insight into these interesting nanoscale phenomena. Quantum surface crystallography takes this one step further in an attempt to experimentally measure the structure of the electrons themselves, which is of greater importance than atomic positions in determining material properties. We report a procedure for obtaining a much better initial parameterization of the charge density than what is possible from a neutral atom model. This procedure involves the parameterization of a bulk charge density model in terms of simple variables such as bond lengths, which can then be transferred to the problem of interest, for instance a surface. Parameterization is accomplished through the fitting of Density Functional Theory calculations of a variety of crystal distortions to a bond-centered pseudoatom (BCPA) model. This parameterized model can then be applied to surfaces or for other problems where an initial higher-order model is needed without the addition of any extra fitted parameters. Through the use of the BCPA model, we report a three-dimensional charge density refinement from x-ray diffraction intensities of the Si (001) 2x1H surface. By properly accounting for the covalent bonding effects in the silicon structure, we were able to stably refine the positions of hydrogen atoms at this surface in three dimensions, which had never before been accomplished for any surface. In addition, we found experimentally an increased, slightly localized bond density of approximately 0.31 electrons between each Si atom pair at the surface. Both the atomic positions and the charge density were found to be in remarkably good agreement with density functional theory (DFT) calculations. The BCPA model was also applied to an experimental refinement of the local charge density at the Si (111) 7x7 surface utilizing a combination of x-ray and high energy electron diffraction. By perturbing about the bond-centered pseudoatom model, we found experimentally that the adatoms were in an anti-bonding state with the atoms directly below. We were also able to experimentally refine a charge transfer of 0.26+/-0.04 e- from each adatom site to the underlying layers. This was the first statistically significant refinement of site-specific bonding information at any surface utilizing x-ray diffraction data. Precession electron diffraction (PED) is a technique which is gaining increasing interest due to its ease of use and reduction of the dynamical scattering problem in electron diffraction. To further investigate the usefulness of this technique, we performed a systematic study of the effect of precession angle on the mineral andalusite where the semiangle was varied from 6.5 to 32 mrad in five discrete steps. We have shown that the intensities of kinematically forbidden reflections decayed exponentially as the precession semiangle (ϕ) was increased. Additionally, we have determined that charge density effects were best observed at moderately low angles (6.5-13 mrad) even though PED patterns became more kinematical in nature as the precession angle was increased further. We have also shown that the amount of interpretable information provided by direct methods phase inversion of the diffraction data increases monotonically but non-systematically as ϕ increases. We report an experimental and theoretical analysis of the ✓3x✓3-R30° and 2x2 reconstructions on the MgO (111) surface combining transmission electron microscopy, x-ray photoelectron spectroscopy, and reasonably accurate density functional calculations using the meta-GGA functional TPSS. We have not only conclusively solved the atomic structures of these reconstructions, but have developed a kinetic model for an evolutionary pathway between structures driven entirely by exchange of water molecules between the surface and the environment that does not require the cations to move when the structure transforms. This is the first time an experimentally and theoretically supported kinetic model has described not only all of the structures in a series on a single oxide surface, but also describes why none of the structures pass through the thermodynamically most stable configuration. Lastly, we have investigated the observability of valence bonding effects in aberration-corrected high resolution electron microscopy (HREM) images along the [010] projection of the mineral Forsterite (Mg2SiO 4). Direct observability of bonding effects would be both faster and less ambiguous than the refinement of similar features against diffraction data. Through analysis of simulated high resolution electron microscopy images, we have determined that bonding effects should be observable at levels approaching 20% of the total contrast. Initial experimental results for this material system have also been presented.

JT9D performance deterioration results from a simulated aerodynamic load test

NASA Technical Reports Server (NTRS)

Stakolich, E. G.; Stromberg, W. J.

1981-01-01

The results of testing to identify the effects of simulated aerodynamic flight loads on JT9D engine performance are presented. The test results were also used to refine previous analytical studies on the impact of aerodynamic flight loads on performance losses. To accomplish these objectives, a JT9D-7AH engine was assembled with average production clearances and new seals as well as extensive instrumentation to monitor engine performance, case temperatures, and blade tip clearance changes. A special loading device was designed and constructed to permit application of known moments and shear forces to the engine by the use of cables placed around the flight inlet. The test was conducted in the Pratt & Whitney Aircraft X-Ray Test Facility to permit the use of X-ray techniques in conjunction with laser blade tip proximity probes to monitor important engine clearance changes. Upon completion of the test program, the test engine was disassembled, and the condition of gas path parts and final clearances were documented. The test results indicate that the engine lost 1.1 percent in thrust specific fuel consumption (TSFC), as measured under sea level static conditions, due to increased operating clearances caused by simulated flight loads. This compares with 0.9 percent predicted by the analytical model and previous study efforts.

Surface modification induced by UV nanosecond Nd:YVO4 laser structuring on biometals

NASA Astrophysics Data System (ADS)

Fiorucci, M. Paula; López, Ana J.; Ramil, Alberto

2014-08-01

Laser surface texturing is a promising tool for improving metallic biomaterials performance in dental and orthopedic bone-replacing applications. Laser ablation modifies the topography of bulk material and might alter surface properties that govern the interactions with the surrounding tissue. This paper presents a preliminary evaluation of surface modifications in two biometals, stainless steel 316L and titanium alloy Ti6Al4V by UV nanosecond Nd:YVO4. Scanning electron microscopy of the surface textured by parallel micro-grooves reveals a thin layer of remelted material along the grooves topography. Furthermore, X-ray diffraction allowed us to appreciate a grain refinement of original crystal structure and consequently induced residual strain. Changes in the surface chemistry were determined by means of X-ray photoelectron spectroscopy; in this sense, generalized surface oxidation was observed and characterization of the oxides and other compounds such hydroxyl groups was reported. In case of titanium alloy, oxide layer mainly composed by TiO2 which is a highly biocompatible compound was identified. Furthermore, laser treatment produces an increase in oxide thickness that could improve the corrosion behavior of the metal. Otherwise, laser treatment led to the formation of secondary phases which might be detrimental to physical and biocompatibility properties of the material.

Unraveling the Hydrogenation of TiO 2 and Graphene Oxide/TiO 2 Composites in Real Time by in Situ Synchrotron X-ray Powder Diffraction and Pair Distribution Function Analysis

DOE PAGES

Nguyen-Phan, Thuy-Duong; Liu, Zongyuan; Luo, Si; ...

2016-02-18

The functionalization of graphene oxide (GO) and graphene by TiO 2 and other metal oxides has attracted considerable attention due to numerous promising applications in catalysis, energy conversion, and storage. We propose hydrogenation of this class of materials as a promising way to tune catalytic properties by altering the structural and chemical transformations that occur upon H incorporation. We also investigate the structural changes that occur during the hydrogenation process using in situ powder X-ray diffraction and pair distribution function analysis of GO–TiO 2 and TiO 2 under H 2 reduction. Sequential Rietveld refinement was employed to gain insight intomore » the evolution of crystal growth of TiO 2 nanoparticles in the presence of two-dimensional (2D) GO nanosheets. GO sheets not only significantly retarded the nucleation and growth of rutile impurities, stabilizing the anatase structure, but was also partially reduced to hydrogenated graphene by the introduction of atomic hydrogen into the honeycomb lattice. We discuss the hydrogenation processes and the resulting composite structure that occurs during the incorporation of atomic H and the dynamic structural transformations that leads to a highly active photocatalyst.« less

A Comparison of Two Methods for Estimating Black Hole Spin in Active Galactic Nuclei

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

Capellupo, Daniel M.; Haggard, Daryl; Wafflard-Fernandez, Gaylor, E-mail: danielc@physics.mcgill.ca

Angular momentum, or spin, is a fundamental property of black holes (BHs), yet it is much more difficult to estimate than mass or accretion rate (for actively accreting systems). In recent years, high-quality X-ray observations have allowed for detailed measurements of the Fe K α emission line, where relativistic line broadening allows constraints on the spin parameter (the X-ray reflection method). Another technique uses accretion disk models to fit the AGN continuum emission (the continuum-fitting, or CF, method). Although each technique has model-dependent uncertainties, these are the best empirical tools currently available and should be vetted in systems where bothmore » techniques can be applied. A detailed comparison of the two methods is also useful because neither method can be applied to all AGN. The X-ray reflection technique targets mostly local ( z ≲ 0.1) systems, while the CF method can be applied at higher redshift, up to and beyond the peak of AGN activity and growth. Here, we apply the CF method to two AGN with X-ray reflection measurements. For both the high-mass AGN, H1821+643, and the Seyfert 1, NGC 3783, we find a range in spin parameter consistent with the X-ray reflection measurements. However, the near-maximal spin favored by the reflection method for NGC 3783 is more probable if we add a disk wind to the model. Refinement of these techniques, together with improved X-ray measurements and tighter BH mass constraints, will permit this comparison in a larger sample of AGN and increase our confidence in these spin estimation techniques.« less

Constraints on Biogenic Emplacement of Crystalline Calcium Carbonate and Dolomite

NASA Astrophysics Data System (ADS)

Colas, B.; Clark, S. M.; Jacob, D. E.

2015-12-01

Amorphous calcium carbonate (ACC) is a biogenic precursor of calcium carbonates forming shells and skeletons of marine organisms, which are key components of the whole marine environment. Understanding carbonate formation is an essential prerequisite to quantify the effect climate change and pollution have on marine population. Water is a critical component of the structure of ACC and the key component controlling the stability of the amorphous state. Addition of small amounts of magnesium (1-5% of the calcium content) is known to promote the stability of ACC presumably through stabilization of the hydrogen bonding network. Understanding the hydrogen bonding network in ACC is fundamental to understand the stability of ACC. Our approach is to use Monte-Carlo simulations constrained by X-ray and neutron scattering data to determine hydrogen bonding networks in ACC as a function of magnesium doping. We have already successfully developed a synthesis protocol to make ACC, and have collected X-ray data, which is suitable for determining Ca, Mg and O correlations, and have collected neutron data, which gives information on the hydrogen/deuterium (as the interaction of X-rays with hydrogen is too low for us to be able to constrain hydrogen atom positions with only X-rays). The X-ray and neutron data are used to constrain reverse Monte-Carlo modelling of the ACC structure using the Empirical Potential Structure Refinement program, in order to yield a complete structural model for ACC including water molecule positions. We will present details of our sample synthesis and characterization methods, X-ray and neutron scattering data, and reverse Monte-Carlo simulations results, together with a discussion of the role of hydrogen bonding in ACC stability.

3XMM J181923.7-170616: An X-Ray Binary with a 408 s Pulsar

NASA Astrophysics Data System (ADS)

Qiu, Hao; Zhou, Ping; Yu, Wenfei; Li, Xiangdong; Xu, Xiaojie

2017-09-01

We carry out a dedicated study of 3XMM J181923.7-170616 with an approximate pulsation period of 400 s using the XMM-Newton and Swift observations spanning across nine years. We have refined the period of the source to 407.904(7) s (at epoch MJD 57142) and constrained the 1σ upper limit on the period derivative \\dot{P}≤slant 1.1× {10}-8 {{s}} {{{s}}}-1. The source radiates hard, persistent X-ray emission during the observation epochs, which is best described by an absorbed power-law model (Γ ˜ 0.2-0.8) plus faint Fe lines at 6.4 and 6.7 keV. The X-ray flux revealed a variation within a factor of 2, along with a spectral hardening as the flux increased. The pulse shape is sinusoid-like and the spectral properties of different phases do not present significant variation. The absorption {N}{{H}} (˜ 1.3× {10}22 {{cm}}-2) is similar to the total Galactic hydrogen column density along the direction, indicating that it is a distant source. A search for the counterpart in optical and near-infrared surveys reveals a low-mass K-type giant, while the existence of a Galactic OB supergiant is excluded. A symbiotic X-ray binary (SyXB) is the favored nature of 3XMM J181923.7-170616 and can essentially explain the low luminosity of 2.78× {10}34{d}102 {erg} {{{s}}}-1, slow pulsation, hard X-ray spectrum, and possible K3 III companion. An alternative explanation of the source is a persistent Be X-ray binary (BeXB) with a companion star no earlier than B3-type.

The Lixiscope: a Pocket-size X-ray Imaging System

NASA Technical Reports Server (NTRS)

Yin, L. I.; Seltzer, S. M.

1978-01-01

A Low Intensity X ray Imaging device with the acronym LIXISCOPE is described. The Lixiscope has a small format and is powered only by a 2.7V battery. The high inherent gain of the Lixiscope permits the use of radioactive sources in lieu of X-ray machines in some fluoroscopic applications. In this mode of operation the complete X ray imaging system is truly portable and pocket-sized.

X-ray lasers

NASA Astrophysics Data System (ADS)

Elton, Raymond C.

Theoretical and practical aspects of X-ray lasers are discussed in an introduction emphasizing recent advances. Chapters are devoted to the unique optical properties of the X-ray spectral region, the principles of short-wavelength lasers, pumping by exciting plasma ions, pumping by electron capture into excited ionic states, pumping by ionization of atoms and ions, and alternative approaches. The potential scientific, technical, biological, and medical applications of X-ray lasers are briefly characterized.

Design and image-quality performance of high resolution CMOS-based X-ray imaging detectors for digital mammography

NASA Astrophysics Data System (ADS)

Cha, B. K.; Kim, J. Y.; Kim, Y. J.; Yun, S.; Cho, G.; Kim, H. K.; Seo, C.-W.; Jeon, S.; Huh, Y.

2012-04-01

In digital X-ray imaging systems, X-ray imaging detectors based on scintillating screens with electronic devices such as charge-coupled devices (CCDs), thin-film transistors (TFT), complementary metal oxide semiconductor (CMOS) flat panel imagers have been introduced for general radiography, dental, mammography and non-destructive testing (NDT) applications. Recently, a large-area CMOS active-pixel sensor (APS) in combination with scintillation films has been widely used in a variety of digital X-ray imaging applications. We employed a scintillator-based CMOS APS image sensor for high-resolution mammography. In this work, both powder-type Gd2O2S:Tb and a columnar structured CsI:Tl scintillation screens with various thicknesses were fabricated and used as materials to convert X-ray into visible light. These scintillating screens were directly coupled to a CMOS flat panel imager with a 25 × 50 mm2 active area and a 48 μm pixel pitch for high spatial resolution acquisition. We used a W/Al mammographic X-ray source with a 30 kVp energy condition. The imaging characterization of the X-ray detector was measured and analyzed in terms of linearity in incident X-ray dose, modulation transfer function (MTF), noise-power spectrum (NPS) and detective quantum efficiency (DQE).

Geological applications of synchrotron radiation

NASA Astrophysics Data System (ADS)

Henderson, C. M. B.; Cressey, G.; Redfern, S. A. T.

1995-03-01

Synchrotron-based, Earth sciences research carried out over the last 5 years is reviewed with special attention being given to X-ray absorption studies; X-ray diffraction and X-ray fluorescence microprobe applications are considered more briefly. A comprehensive bibliography is included. The main part of the paper summarizes recent work carried out at the Daresbury SRS. K-edge XAS studies of glasses as models for silicate melts provide information on the local structural environments of Si, Fe 2+ and Fe 3+. By analogy with synthetic "leucites" which contain Fe 2+ and Fe 3+ in tetrahedral framework sites, it seems that many model glasses also contain both oxidation states of Fe in the network, rather than as network modifiers. The structural sites occupied by the minor elements Mn, Zn and Ti in staurolite have been identified using XAFS; Mn and Zn substitute for Fe 2+ in the tetrahedral T2 site, while Ti occupies the distorted M2 octahedral site. L-edge spectroscopy is used to identify the valencies and electronic structures of Mn and Fe in minerals and the Fe 2+:Fe 3+ ratio in a natural spinel is determined. The polarized nature of the synchrotron beam is exploited in determining the Fe X-ray absorption anisotropy in single crystal tourmaline and epidote. XRD powder studies include Rietveld-refinement structure determination and compressibility studies. Synthetic "leucites" having the stoichiometry K 2MgSi 5O 12 have distinctly different structures. The dry-synthesized form is cubic Ia3d with Si and Mg fully disordered on tetrahedral framework sites, while the hydrothermally-synthesized polymorph is monoclinic P2 1/c with Si and Mg fully disordered on, respectively, 10 and 2 tetrahedral sites. The reversible tetragonal to orthorhombic phase transition in gillespite (BaFeSi 4O 10) has been studied in a diamond anvil cell using ED detection and found to occur at 1.2 ± 0.1 GPa. The anomalous compressibility observed has been interpreted in terms of ferroelastic and coelastic phenomena and the related order parameters analysed using Landau theory. The compressibility of MgCO 3, determined up to 20 GPa, has been combined with thermochemical data to obtain an "equation to state" for magnesite and it is found that magnesite is likely to be the main host for carbon in the Earth's lower mantle.

Structure of the Archaeoglobus fulgidus orphan ORF AF1382 determined by sulfur SAD from a moderately diffracting crystal

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

Zhu, Jin-Yi; Fu, Zheng-Qing; Argonne National Laboratory, Argonne, Illinois

2012-09-01

The crystal structure of the 11.14 kDa orphan ORF 1382 from Archaeoglobus fulgidus (AF1382) has been determined by sulfur SAD phasing using data collected from a moderately diffracting crystal and 1.9 Å synchrotron X-rays. The crystal structure of the 11.14 kDa orphan ORF 1382 from Archaeoglobus fulgidus (AF1382) has been determined by sulfur SAD phasing using a moderately diffracting crystal and 1.9 Å wavelength synchrotron X-rays. AF1382 was selected as a structural genomics target by the Southeast Collaboratory for Structural Genomics (SECSG) since sequence analyses showed that it did not belong to the Pfam-A database and thus could represent amore » novel fold. The structure was determined by exploiting longer wavelength X-rays and data redundancy to increase the anomalous signal in the data. AF1382 is a 95-residue protein containing five S atoms associated with four methionine residues and a single cysteine residue that yields a calculated Bijvoet ratio (ΔF{sub anom}/F) of 1.39% for 1.9 Å wavelength X-rays. Coupled with an average Bijvoet redundancy of 25 (two 360° data sets), this produced an excellent electron-density map that allowed 69 of the 95 residues to be automatically fitted. The S-SAD model was then manually completed and refined (R = 23.2%, R{sub free} = 26.8%) to 2.3 Å resolution. High-resolution data were subsequently collected from a better diffracting crystal using 0.97 Å wavelength synchrotron X-rays and the S-SAD model was refined (R = 17.9%, R{sub free} = 21.4%) to 1.85 Å resolution. AF1382 has a winged-helix–turn–helix structure common to many DNA-binding proteins and most closely resembles the N-terminal domain (residues 1–82) of the Rio2 kinase from A. fulgidus, which has been shown to bind DNA, and a number of MarR-family transcriptional regulators, suggesting a similar DNA-binding function for AF1382. The analysis also points out the advantage gained from carrying out data reduction and structure determination on-site while the crystal is still available for further data collection.« less

Hard X-ray Optics Technology Development for Astronomy at the Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

Gubarev, Mikhail; Ramsey, Brian; Kilaru, Kiranmayee

2009-01-01

Grazing-incidence telescopes based on Wolter 1 geometry have delivered impressive advances in astrophysics at soft-x-ray wavelengths, while the hard xray region remains relatively unexplored at fine angular resolution and high sensitivities. The ability to perform ground-breaking science in the hard-x-ray energy range had been the motivation for technology developments aimed at fabricating low-cost, light-weight, high-quality x-ray mirrors. Grazing-incidence x-ray optics for high-energy astrophysical applications is being developed at MSFC using the electroform-nickel replication process.

The trickle before the torrent-diffraction data from X-ray lasers.

PubMed

Maia, Filipe R N C; Hajdu, Janos

2016-08-01

Today Scientific Data launched a collection of publications describing data from X-ray free-electron lasers under the theme 'Structural Biology Applications of X-ray Lasers'. The papers cover data on nanocrystals, single virus particles, isolated cell organelles, and living cells. All data are deposited with the Coherent X-ray Imaging Data Bank (CXIDB) and available to the scientific community to develop ideas, tools and procedures to meet challenges with the expected torrents of data from new X-ray lasers, capable of producing billion exposures per day.

Composite x-ray pinholes for time-resolved microphotography of laser compressed targets.

PubMed

Attwood, D T; Weinstein, B W; Wuerker, R F

1977-05-01

Composite x-ray pinholes having dichroic properties are presented. These pinholes permit both x-ray imaging and visible alignment with micron accuracy by presenting different apparent apertures in these widely disparate regions of the spectrum. Their use is mandatory in certain applications in which the x-ray detection consists of a limited number of resolvable elements whose use one wishes to maximize. Mating the pinhole camera with an x-ray streaking camera is described, along with experiments which spatially and temporally resolve the implosion of laser irradiated targets.

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

Computed radiography as a gamma ray detector—dose response and applications

NASA Astrophysics Data System (ADS)

O'Keeffe, D. S.; McLeod, R. W.

2004-08-01

Computed radiography (CR) can be used for imaging the spatial distribution of photon emissions from radionuclides. Its wide dynamic range and good response to medium energy gamma rays reduces the need for long exposure times. Measurements of small doses can be performed without having to pre-sensitize the computed radiography plates via an x-ray exposure, as required with screen-film systems. Cassette-based Agfa MD30 and Kodak GP25 CR plates were used in applications involving the detection of gamma ray emissions from technetium-99m and iodine-131. Cassette entrance doses as small as 1 µGy (140 keV gamma rays) produce noisy images, but the images are suitable for applications such as the detection of breaks in radiation protection barriers. A consequence of the gamma ray sensitivity of CR plates is the possibility that some nuclear medicine patients may fog their x-rays if the x-ray is taken soon after their radiopharmaceutical injection. The investigation showed that such fogging is likely to be diffuse.

Extended investigation of intermartensitic transitions in Ni-Mn-Ga magnetic shape memory alloys: A detailed phase diagram determination

NASA Astrophysics Data System (ADS)

Ćakιr, Aslι; Righi, Lara; Albertini, Franca; Acet, Mehmet; Farle, Michael; Aktürk, Selçuk

2013-11-01

Martensitic transitions in shape memory Ni-Mn-Ga Heusler alloys take place between a high temperature austenite and a low temperature martensite phase. However, intermartensitic transformations have also been encountered that occur from one martensite phase to another. To examine intermartensitic transitions in magnetic shape memory alloys in detail, we carried out temperature dependent magnetization, resistivity, and x-ray diffraction measurements to investigate the intermartensitic transition in Ni50Mn50-xGax in the composition range 12≤x≤25 at. %. Rietveld refined x-ray diffraction results are found to be consistent with magnetization and resistivity data. Depending on composition, we observe that intermartensitic transitions occur in the sequences 7M→L10, 5M →7M, and 5M→7M→L10 with decreasing temperature. The L10 non-modulated structure is most stable at low temperature.

Drastic effect of the Mn-substitution in the strongly correlated semiconductor FeSb2.

NASA Astrophysics Data System (ADS)

Kassem, Mohamed A.; Tabata, Yoshikazu; Waki, Takeshi; Nakamura, Hiroyuki

2017-06-01

We report the effects of Mn substitution, corresponding to hole doping, on the electronic properties of the narrow gap semiconductor, FeSb2, using single crystals of Fe1- x Mn x Sb2 grown by the Sb flux method. The orthorhombic Pnnm structure was confirmed by powder X-ray diffraction (XRD) for the pure and Mn-substituted samples. Their crystal structure parameters were refined using the Rietveld method. The chemical composition was investigated by wavelength-dispersive X-ray spectroscopy (WDX). The solubility limit of Mn in FeSb2 is x max ˜ 0.05 and the lattice constants change monotonically with increasing the actual Mn concentration. A drastic change from semiconducting to metallic electronic transports was found at very low Mn concentration at x ˜ 0.01. Our experimental results and analysis indicate that the substitution of a small amount of Mn changes drastically the electronic state in FeSb2 as well as the Co-substitution does: closing of the narrow gap and emergence of the density of states (DOS) at the Fermi level.

Simulating the x-ray image contrast to setup techniques with desired flaw detectability

NASA Astrophysics Data System (ADS)

Koshti, Ajay M.

2015-04-01

The paper provides simulation data of previous work by the author in developing a model for estimating detectability of crack-like flaws in radiography. The methodology is developed to help in implementation of NASA Special x-ray radiography qualification, but is generically applicable to radiography. The paper describes a method for characterizing the detector resolution. Applicability of ASTM E 2737 resolution requirements to the model are also discussed. The paper describes a model for simulating the detector resolution. A computer calculator application, discussed here, also performs predicted contrast and signal-to-noise ratio calculations. Results of various simulation runs in calculating x-ray flaw size parameter and image contrast for varying input parameters such as crack depth, crack width, part thickness, x-ray angle, part-to-detector distance, part-to-source distance, source sizes, and detector sensitivity and resolution are given as 3D surfaces. These results demonstrate effect of the input parameters on the flaw size parameter and the simulated image contrast of the crack. These simulations demonstrate utility of the flaw size parameter model in setting up x-ray techniques that provide desired flaw detectability in radiography. The method is applicable to film radiography, computed radiography, and digital radiography.

A CPU benchmark for protein crystallographic refinement.

PubMed

Bourne, P E; Hendrickson, W A

1990-01-01

The CPU time required to complete a cycle of restrained least-squares refinement of a protein structure from X-ray crystallographic data using the FORTRAN codes PROTIN and PROLSQ are reported for 48 different processors, ranging from single-user workstations to supercomputers. Sequential, vector, VLIW, multiprocessor, and RISC hardware architectures are compared using both a small and a large protein structure. Representative compile times for each hardware type are also given, and the improvement in run-time when coding for a specific hardware architecture considered. The benchmarks involve scalar integer and vector floating point arithmetic and are representative of the calculations performed in many scientific disciplines.

Crystal-Chemical Analysis of Soil at Rocknest, Gale Crater

NASA Technical Reports Server (NTRS)

Morrison, S. M.; Downs, R. T.; Blake, D. F.; Bish, D. L.; Ming, D. W.; Morris, R. V.; Yen, A. S.; Chipera, S. J.; Treiman, A. H.; Vaniman, D. T.;

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

Shin, Kyung -Wook; Karim, Karim S.

Direct conversion crystalline silicon X-ray imagers are used for low-energy X-ray photon (4-20 keV) detection in scientific research applications such as protein crystallography. In this paper, we demonstrate a novel pixel architecture that integrates a crystalline silicon X-ray detector with a thin-film transistor amorphous silicon pixel readout circuit. We describe a simplified two-mask process to fabricate a complete imaging array and present preliminary results that show the fabricated pixel to be sensitive to 5.89-keV photons from a low activity Fe-55 gamma source. Furthermore, this paper presented can expedite the development of high spatial resolution, low cost, direct conversion imagers formore » X-ray diffraction and crystallography applications.« less

Development of speckle-free channel-cut crystal optics using plasma chemical vaporization machining for coherent x-ray applications.

PubMed

Hirano, Takashi; Osaka, Taito; Sano, Yasuhisa; Inubushi, Yuichi; Matsuyama, Satoshi; Tono, Kensuke; Ishikawa, Tetsuya; Yabashi, Makina; Yamauchi, Kazuto

2016-06-01

We have developed a method of fabricating speckle-free channel-cut crystal optics with plasma chemical vaporization machining, an etching method using atmospheric-pressure plasma, for coherent X-ray applications. We investigated the etching characteristics to silicon crystals and achieved a small surface roughness of less than 1 nm rms at a removal depth of >10 μm, which satisfies the requirements for eliminating subsurface damage while suppressing diffuse scattering from rough surfaces. We applied this method for fabricating channel-cut Si(220) crystals for a hard X-ray split-and-delay optical system and confirmed that the crystals provided speckle-free reflection profiles under coherent X-ray illumination.

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography.

PubMed

Gicquel, Yannig; Schubert, Robin; Kapis, Svetlana; Bourenkov, Gleb; Schneider, Thomas; Perbandt, Markus; Betzel, Christian; Chapman, Henry N; Heymann, Michael

2018-04-24

This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The devices are patterned from epoxy glue using soft lithography and are suitable for in situ X-ray diffraction experiments at room temperature. The sample wells are lidded on both sides with polymeric polyimide foil windows that allow diffraction data collection with low X-ray background. This fabrication method is undemanding and inexpensive. After the sourcing of a SU-8 master wafer, all fabrication can be completed outside of a cleanroom in a typical research lab environment. The chip design and fabrication protocol utilize capillary valving to microfluidically split an aqueous reaction into defined nanoliter sized droplets. This loading mechanism avoids the sample loss from channel dead-volume and can easily be performed manually without using pumps or other equipment for fluid actuation. We describe how isolated nanoliter sized drops of protein solution can be monitored in situ by dynamic light scattering to control protein crystal nucleation and growth. After suitable crystals are grown, complete X-ray diffraction datasets can be collected using goniometer based in situ fixed target serial X-ray crystallography at room temperature. The protocol provides custom scripts to process diffraction datasets using a suite of software tools to solve and refine the protein crystal structure. This approach avoids the artefacts possibly induced during cryo-preservation or manual crystal handling in conventional crystallography experiments. We present and compare three protein structures that were solved using small crystals with dimensions of approximately 10-20 µm grown in chip. By crystallizing and diffracting in situ, handling and hence mechanical disturbances of fragile crystals is minimized. The protocol details how to fabricate a custom X-ray transparent microfluidic chip suitable for in situ serial crystallography. As almost every crystal can be used for diffraction data collection, these microfluidic chips are a very efficient crystal delivery method.

X-ray intravital microscopy for functional imaging in rat hearts using synchrotron radiation coronary microangiography

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

Umetani, K.; Fukushima, K.

2013-03-15

An X-ray intravital microscopy technique was developed to enable in vivo visualization of the coronary, cerebral, and pulmonary arteries in rats without exposure of organs and with spatial resolution in the micrometer range and temporal resolution in the millisecond range. We have refined the system continually in terms of the spatial resolution and exposure time. X-rays transmitted through an object are detected by an X-ray direct-conversion type detector, which incorporates an X-ray SATICON pickup tube. The spatial resolution has been improved to 6 {mu}m, yielding sharp images of small arteries. The exposure time has been shortened to around 2 msmore » using a new rotating-disk X-ray shutter, enabling imaging of beating rat hearts. Quantitative evaluations of the X-ray intravital microscopy technique were extracted from measurements of the smallest-detectable vessel size and detection of the vessel function. The smallest-diameter vessel viewed for measurements is determined primarily by the concentration of iodinated contrast material. The iodine concentration depends on the injection technique. We used ex vivo rat hearts under Langendorff perfusion for accurate evaluation. After the contrast agent is injected into the origin of the aorta in an isolated perfused rat heart, the contrast agent is delivered directly into the coronary arteries with minimum dilution. The vascular internal diameter response of coronary arterial circulation is analyzed to evaluate the vessel function. Small blood vessels of more than about 50 {mu}m diameters were visualized clearly at heart rates of around 300 beats/min. Vasodilation compared to the control was observed quantitatively using drug manipulation. Furthermore, the apparent increase in the number of small vessels with diameters of less than about 50 {mu}m was observed after the vasoactive agents increased the diameters of invisible small blood vessels to visible sizes. This technique is expected to offer the potential for direct investigation of mechanisms of vascular dysfunctions.« less

Spatially resolved X-ray emission measurements of the residual velocity during the stagnation phase of inertial confinement fusion implosion experiments

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

Ruby, J. J.; Pak, A., E-mail: pak5@llnl.gov; Field, J. E.

2016-07-15

A technique for measuring residual motion during the stagnation phase of an indirectly driven inertial confinement experiment has been implemented. This method infers a velocity from spatially and temporally resolved images of the X-ray emission from two orthogonal lines of sight. This work investigates the accuracy of recovering spatially resolved velocities from the X-ray emission data. A detailed analytical and numerical modeling of the X-ray emission measurement shows that the accuracy of this method increases as the displacement that results from a residual velocity increase. For the typical experimental configuration, signal-to-noise ratios, and duration of X-ray emission, it is estimatedmore » that the fractional error in the inferred velocity rises above 50% as the velocity of emission falls below 24 μm/ns. By inputting measured parameters into this model, error estimates of the residual velocity as inferred from the X-ray emission measurements are now able to be generated for experimental data. Details of this analysis are presented for an implosion experiment conducted with an unintentional radiation flux asymmetry. The analysis shows a bright localized region of emission that moves through the larger emitting volume at a relatively higher velocity towards the location of the imposed flux deficit. This technique allows for the possibility of spatially resolving velocity flows within the so-called central hot spot of an implosion. This information would help to refine our interpretation of the thermal temperature inferred from the neutron time of flight detectors and the effect of localized hydrodynamic instabilities during the stagnation phase. Across several experiments, along a single line of sight, the average difference in magnitude and direction of the measured residual velocity as inferred from the X-ray and neutron time of flight detectors was found to be ∼13 μm/ns and ∼14°, respectively.« less

Spatially resolved X-ray emission measurements of the residual velocity during the stagnation phase of inertial confinement fusion implosion experiments

DOE PAGES

Ruby, J. J.; Pak, A.; Field, J. E.; ...

2016-07-01

A technique for measuring residual motion during the stagnation phase of an indirectly driven inertial confinement experiment has been implemented. Our method infers a velocity from spatially and temporally resolved images of the X-ray emission from two orthogonal lines of sight. This work investigates the accuracy of recovering spatially resolved velocities from the X-ray emission data. A detailed analytical and numerical modeling of the X-ray emission measurement shows that the accuracy of this method increases as the displacement that results from a residual velocity increase. For the typical experimental configuration, signal-to-noise ratios, and duration of X-ray emission, it is estimatedmore » that the fractional error in the inferred velocity rises above 50% as the velocity of emission falls below 24 μm/ns. Furthermore, by inputting measured parameters into this model, error estimates of the residual velocity as inferred from the X-ray emission measurements are now able to be generated for experimental data. Details of this analysis are presented for an implosion experiment conducted with an unintentional radiation flux asymmetry. The analysis shows a bright localized region of emission that moves through the larger emitting volume at a relatively higher velocity towards the location of the imposed flux deficit. Our technique allows for the possibility of spatially resolving velocity flows within the so-called central hot spot of an implosion. This information would help to refine our interpretation of the thermal temperature inferred from the neutron time of flight detectors and the effect of localized hydrodynamic instabilities during the stagnation phase. Across several experiments, along a single line of sight, the average difference in magnitude and direction of the measured residual velocity as inferred from the X-ray and neutron time of flight detectors was found to be ~13 μm/ns and ~14°, respectively.« less

Seeing Red and Shooting Blanks: Study of Red Quasars and Blank X-Ray Sources

NASA Technical Reports Server (NTRS)

Oliversen, Ronald (Technical Monitor); Elvis, Martin

2005-01-01

A major paper describing the technique and providing a list of 'blanks' was published in the Astrophysical Journal (abstract below). The results revealed a fascinating trove of novel X-ray sources: high redshift clusters of galaxies found efficiently; X-ray absorbed, optically clean AGN, which may be the bright prototypes of Chandra Deep Survey sources; and several with a still unknown nature. Recent XMM-Newton results confirm the existence of this class of X-ray source with much refined positions. During the first year of this project we have made a major discovery. The second 'blanks' X-ray source observed with Chandra was found to be extended. Using Chandra data and ground-based R and K band imaging we estimated this to be a high redshift cluster of galaxies with z approx. 0.85. Spectroscopy agrees with this estimate (z=0.89). This success shows that our method of hunting down 'blank' field X-ray sources is a highly efficient method of finding the otherwise elusive high redshift clusters. With extensive follow-up we should be able to use 'blanks' to make cosmological tests. The paper is now in press in the Astrophysical Journal (abstract below.) The other Chandra source is point-like, showing that there are a variety of 'blank' source types. Other follow-up observations with XMM-Newton, and (newly approved in cycle 2) with Chandra are eagerly awaited. A follow-up paper uses a large amount of supporting data for the remaining blanks. A combination of ROSAT, Chandra and ground based data convincingly identified one of the blanks as a Ultra-luminous X-ray source (ULX) in a spiral galaxy (abstract below). This program resulted in 3 refereed papers in major journals, 4 conference proceedings and a significant fraction of the PhD thesis of Dr. Ilaria Cagnoni. Details of the publications are given.

Protein crystal structure from non-oriented, single-axis sparse X-ray data

DOE PAGES

Wierman, Jennifer L.; Lan, Ti-Yen; Tate, Mark W.; ...

2016-01-01

X-ray free-electron lasers (XFELs) have inspired the development of serial femtosecond crystallography (SFX) as a method to solve the structure of proteins. SFX datasets are collected from a sequence of protein microcrystals injected across ultrashort X-ray pulses. The idea behind SFX is that diffraction from the intense, ultrashort X-ray pulses leaves the crystal before the crystal is obliterated by the effects of the X-ray pulse. The success of SFX at XFELs has catalyzed interest in analogous experiments at synchrotron-radiation (SR) sources, where data are collected from many small crystals and the ultrashort pulses are replaced by exposure times that aremore » kept short enough to avoid significant crystal damage. The diffraction signal from each short exposure is so `sparse' in recorded photons that the process of recording the crystal intensity is itself a reconstruction problem. Using theEMCalgorithm, a successful reconstruction is demonstrated here in a sparsity regime where there are no Bragg peaks that conventionally would serve to determine the orientation of the crystal in each exposure. In this proof-of-principle experiment, a hen egg-white lysozyme (HEWL) crystal rotating about a single axis was illuminated by an X-ray beam from an X-ray generator to simulate the diffraction patterns of microcrystals from synchrotron radiation. Millions of these sparse frames, typically containing only ~200 photons per frame, were recorded using a fast-framing detector. It is shown that reconstruction of three-dimensional diffraction intensity is possible using theEMCalgorithm, even with these extremely sparse frames and without knowledge of the rotation angle. Further, the reconstructed intensity can be phased and refined to solve the protein structure using traditional crystallographic software. In conclusion, this suggests that synchrotron-based serial crystallography of micrometre-sized crystals can be practical with the aid of theEMCalgorithm even in cases where the data are sparse.« less

Protein crystal structure from non-oriented, single-axis sparse X-ray data

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

Wierman, Jennifer L.; Lan, Ti-Yen; Tate, Mark W.

X-ray free-electron lasers (XFELs) have inspired the development of serial femtosecond crystallography (SFX) as a method to solve the structure of proteins. SFX datasets are collected from a sequence of protein microcrystals injected across ultrashort X-ray pulses. The idea behind SFX is that diffraction from the intense, ultrashort X-ray pulses leaves the crystal before the crystal is obliterated by the effects of the X-ray pulse. The success of SFX at XFELs has catalyzed interest in analogous experiments at synchrotron-radiation (SR) sources, where data are collected from many small crystals and the ultrashort pulses are replaced by exposure times that aremore » kept short enough to avoid significant crystal damage. The diffraction signal from each short exposure is so `sparse' in recorded photons that the process of recording the crystal intensity is itself a reconstruction problem. Using theEMCalgorithm, a successful reconstruction is demonstrated here in a sparsity regime where there are no Bragg peaks that conventionally would serve to determine the orientation of the crystal in each exposure. In this proof-of-principle experiment, a hen egg-white lysozyme (HEWL) crystal rotating about a single axis was illuminated by an X-ray beam from an X-ray generator to simulate the diffraction patterns of microcrystals from synchrotron radiation. Millions of these sparse frames, typically containing only ~200 photons per frame, were recorded using a fast-framing detector. It is shown that reconstruction of three-dimensional diffraction intensity is possible using theEMCalgorithm, even with these extremely sparse frames and without knowledge of the rotation angle. Further, the reconstructed intensity can be phased and refined to solve the protein structure using traditional crystallographic software. In conclusion, this suggests that synchrotron-based serial crystallography of micrometre-sized crystals can be practical with the aid of theEMCalgorithm even in cases where the data are sparse.« less

Advances in photographic X-ray imaging for solar astronomy

NASA Technical Reports Server (NTRS)

Moses, J. Daniel; Schueller, R.; Waljeski, K.; Davis, John M.

1989-01-01

The technique of obtaining quantitative data from high resolution soft X-ray photographic images produced by grazing incidence optics was successfully developed to a high degree during the Solar Research Sounding Rocket Program and the S-054 X-Ray Spectrographic Telescope Experiment Program on Skylab. Continued use of soft X-ray photographic imaging in sounding rocket flights of the High Resolution Solar Soft X-Ray Imaging Payload has provided opportunities to further develop these techniques. The developments discussed include: (1) The calibration and use of an inexpensive, commercially available microprocessor controlled drum type film processor for photometric film development; (2) The use of Kodak Technical Pan 2415 film and Kodak SO-253 High Speed Holographic film for improved resolution; and (3) The application of a technique described by Cook, Ewing, and Sutton for determining the film characteristics curves from density histograms of the flight film. Although the superior sensitivity, noise level, and linearity of microchannel plate and CCD detectors attracts the development efforts of many groups working in soft X-ray imaging, the high spatial resolution and dynamic range as well as the reliability and ease of application of photographic media assures the continued use of these techniques in solar X-ray astronomy observations.

Electronic structure and soft-X-ray-induced photoreduction studies of iron-based magnetic polyoxometalates of type {(M)M5}12Fe(III)30 (M = Mo(VI), W(VI)).

PubMed

Kuepper, Karsten; Derks, Christine; Taubitz, Christian; Prinz, Manuel; Joly, Loïc; Kappler, Jean-Paul; Postnikov, Andrei; Yang, Wanli; Kuznetsova, Tatyana V; Wiedwald, Ulf; Ziemann, Paul; Neumann, Manfred

2013-06-14

Giant Keplerate-type molecules with a {Mo72Fe30} core show a number of very interesting properties, making them particularly promising for various applications. So far, only limited data on the electronic structure of these molecules from X-ray spectra and electronic structure calculations have been available. Here we present a combined electronic and magnetic structure study of three Keplerate-type nanospheres--two with a {Mo72Fe30} core and one with a {W72Fe30} core by means of X-ray absorption spectroscopy, X-ray magnetic circular dichroism (XMCD), SQUID magnetometry, and complementary theoretical approaches. Furthermore, we present detailed studies of the Fe(3+)-to-Fe(2+) photoreduction process, which is induced under soft X-ray radiation in these molecules. We observe that the photoreduction rate greatly depends on the ligand structure surrounding the Fe ions, with negatively charged ligands leading to a dramatically reduced photoreduction rate. This opens the possibility of tailoring such polyoxometalates by X-ray spectroscopic studies and also for potential applications in the field of X-ray induced photochemistry.

Reconstitution of SNARE proteins into solid-supported lipid bilayer stacks and X-ray structure analysis.

PubMed

Xu, Yihui; Kuhlmann, Jan; Brennich, Martha; Komorowski, Karlo; Jahn, Reinhard; Steinem, Claudia; Salditt, Tim

2018-02-01

SNAREs are known as an important family of proteins mediating vesicle fusion. For various biophysical studies, they have been reconstituted into supported single bilayers via proteoliposome adsorption and rupture. In this study we extended this method to the reconstitution of SNAREs into supported multilamellar lipid membranes, i.e. oriented multibilayer stacks, as an ideal model system for X-ray structure analysis (X-ray reflectivity and diffraction). The reconstitution was implemented through a pathway of proteomicelle, proteoliposome and multibilayer. To monitor the structural evolution in each step, we used small-angle X-ray scattering for the proteomicelles and proteoliposomes, followed by X-ray reflectivity and grazing-incidence small-angle scattering for the multibilayers. Results show that SNAREs can be successfully reconstituted into supported multibilayers, with high enough orientational alignment for the application of surface sensitive X-ray characterizations. Based on this protocol, we then investigated the effect of SNAREs on the structure and phase diagram of the lipid membranes. Beyond this application, this reconstitution protocol could also be useful for X-ray analysis of many further membrane proteins. Copyright © 2017 Elsevier B.V. All rights reserved.

Microfabrication: LIGA-X and applications

NASA Astrophysics Data System (ADS)

Kupka, R. K.; Bouamrane, F.; Cremers, C.; Megtert, S.

2000-09-01

X-ray LIGA (Lithography, Electrogrowth, Moulding) is one of today's key technologies in microfabrication and upcoming modern (meso)-(nano) fabrication, already used and anticipated for micromechanics (micromotors, microsensors, spinnerets, etc.), micro-optics, micro-hydrodynamics (fluidic devices), microbiology, in medicine, in biology, and in chemistry for microchemical reactors. It compares to micro-electromechanical systems (MEMS) technology, offering a larger, non-silicon choice of materials and better inherent precision. X-ray LIGA relies on synchrotron radiation to obtain necessary X-ray fluxes and uses X-ray proximity printing. Inherent advantages are its extreme precision, depth of field and very low intrinsic surface roughness. However, the quality of fabricated structures often depends on secondary effects during exposure and effects like resist adhesion. UV-LIGA, relying on thick UV resists is an alternative for projects requiring less precision. Modulating the spectral properties of synchrotron radiation, different regimes of X-ray lithography lead to (a) the mass-fabrication of classical nanostructures, (b) the fabrication of high aspect ratio nanostructures (HARNST), (c) the fabrication of high aspect ratio microstructures (HARMST), and (d) the fabrication of high aspect ratio centimeter structures (HARCST). Reviewing very recent activities around X-ray LIGA, we show the versatility of the method, obviously finding its region of application there, where it is best and other competing microtechnologies are less advantageous. An example of surface-based X-ray and particle lenses (orthogonal reflection optics (ORO)) made by X-ray LIGA is given.

The Role of X-Rays in Future Space Navigation and Communication

NASA Technical Reports Server (NTRS)

Winternitz, Luke M. B.; Gendreau, Keith C.; Hasouneh, Monther A.; Mitchell, Jason W.; Fong, Wai H.; Lee, Wing-Tsz; Gavriil, Fotis; Arzoumanian, Zaven

2013-01-01

In the near future, applications using X-rays will enable autonomous navigation and time distribution throughout the solar system, high capacity and low-power space data links, highly accurate attitude sensing, and extremely high-precision formation flying capabilities. Each of these applications alone has the potential to revolutionize mission capabilities, particularly beyond Earth orbit. This paper will outline the NASA Goddard Space Flight Center vision and efforts toward realizing the full potential of X-ray navigation and communications.

Application of X-ray imaging techniques to auroral monitoring

NASA Technical Reports Server (NTRS)

Rust, D. M.; Burstein, P.

1981-01-01

The precipitation of energetic particles into the ionosphere produces bremsstrahlung X-rays and K-alpha line emission from excited oxygen and nitrogen. If viewed from a spacecraft in a highly elliptical polar orbit, this soft (0.3 - 3.0 keV) X-radiation will provide an almost uninterrupted record of dayside and nightside auroras. A grazing incidence X-ray telescope especially designed for such auroral monitoring is described. High photon collection efficiency will permit exposure times of approximately 100 seconds during substorms. Spectrophotometry will allow users to derive the energy spectrum of the precipitating particles. If placed in a 15 earth-radius orbit, the telescope can produce auroral X-ray images with 30 km resolution. Absolute position of X-ray auroras can be established with a small optical telescope co-aligned with the X-ray telescope. Comparison of X-ray and optical images will establish the height and global distribution of X-ray aurorae, relative to well-known optical auroras, thus melding the new X-ray results with knowledge of optical auroras.

Extended investigation of intermartensitic transitions in Ni-Mn-Ga magnetic shape memory alloys: A detailed phase diagram determination

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

Çakir, Asli; Aktürk, Selçuk; Righi, Lara

2013-11-14

Martensitic transitions in shape memory Ni-Mn-Ga Heusler alloys take place between a high temperature austenite and a low temperature martensite phase. However, intermartensitic transformations have also been encountered that occur from one martensite phase to another. To examine intermartensitic transitions in magnetic shape memory alloys in detail, we carried out temperature dependent magnetization, resistivity, and x-ray diffraction measurements to investigate the intermartensitic transition in Ni{sub 50}Mn{sub 50–x}Ga{sub x} in the composition range 12≤x≤25 at. %. Rietveld refined x-ray diffraction results are found to be consistent with magnetization and resistivity data. Depending on composition, we observe that intermartensitic transitions occur inmore » the sequences 7M→L1{sub 0}, 5M→7M, and 5M→7M→L1{sub 0} with decreasing temperature. The L1{sub 0} non-modulated structure is most stable at low temperature.« less

Insights into the effect of iron and cobalt doping on the structure of nanosized ZnO.

PubMed

Giuli, Gabriele; Trapananti, Angela; Mueller, Franziska; Bresser, Dominic; d'Acapito, Francesco; Passerini, Stefano

2015-10-05

Here we report an in-depth structural characterization of transition metal-doped zinc oxide nanoparticles that have recently been used as anode materials for Li-ion batteries. Structural refinement of powder X-ray diffraction (XRD) data allowed the determination of small though reproducible changes in the unit cell dimensions of four ZnO samples (wurtzite structure) prepared with different dopants or different synthesis conditions. Moreover, large variations of the full width at half-maximum of the XRD reflections indicate that the crystallinity of the samples decreases in the order ZnO, Zn0.9Co0.1O, Zn0.9Fe0.1O/C, and Zn0.9Fe0.1O (the crystallite sizes as determined by Williamson-Hall plots are 42, 29, 15, and 13 nm, respectively). X-ray absorption spectroscopy data indicate that Co is divalent, whereas Fe is purely trivalent in Zn0.9Fe0.1O and 95% trivalent (Fe(3+)/(Fe(3+) + Fe(2+)) ratio = 0.95) in Zn0.9Fe0.1O/C. The aliovalent substitution of Fe(3+) for Zn(2+) implies the formation of local defects around Fe(3+) such as cationic vacancies or interstitial oxygen for charge balance. The EXAFS (extended X-ray absorption fine structure) data, besides providing local Fe-O and Co-O bond distances, are consistent with a large amount of charge-compensating defects. The Co-doped sample displays similar EXAFS features to those of pure ZnO, suggesting the absence of a large concentration of defects as found in the Fe-doped samples. These results are of substantial importance for understanding and elucidating the modified electrochemical lithiation mechanism by introducing transition metal dopants into the ZnO structure for the application as lithium-ion anode material.

Application of the gas-discharge surge arresters in X-ray devices and low voltage instrumentation

NASA Astrophysics Data System (ADS)

Simon, V. A.; Gerasimov, V. A.; Kostrin, D. K.; Lisenkov, A. A.; Selivanov, L. M.; Uhov, A. A.

2018-02-01

Usage of the gas discharge in science and engineering is discussed. Application examples of the compact gas-discharge tubes in the X-ray devices and low voltage instrumentation appliances for the surge protection are presented.

Crystalline structure of Cu4SSe

NASA Astrophysics Data System (ADS)

Amiraslanov, I. R.; Alieva, N. A.; Guseinov, G. G.

2016-12-01

Ternary compound Cu4SSe has been first synthesized by alloying the Cu, S, and Se elements taken in stoichiometric ratios. An X-ray diffraction study of polycrystalline samples has revealed the synthesized material to be crystallized into the trigonal system with unit-cell parameters a = 4.021(1) Å, c = 6.838(1) Å, and V = 95.75(4) Å3; sp. gr. P bar 3 m1; Z = 1; D x = 6.333(3) g/cm3. The crystal structure has been solved and refined to the reliability factor R Bragg = 0.40%.

Recent development of radiation measurement instrument for industrial and medical applications

NASA Astrophysics Data System (ADS)

Baba, Sueki; Ohmori, Koichi; Mito, Yoshio; Tanoue, Toshiya; Yano, Shigeki; Tokumori, Kenji; Toyofuku, Fukai; Kanda, Shigenobu

2001-02-01

Recently, computer imaging technology has developed very high-quality image and fast processing time. X-rays have been used for many purposes such as medical diagnosis and analyzing the structure of industrial materials. However, as X-rays are hazardous to the human body, it is desirable to reduce its exposed dose to a minimum. For this purpose, it is necessary to use a semiconductor radiation detector with a high efficiency for X-rays. We have developed photon-counting CdTe array detector system for medical and industrial use. The bone densitometer for Dual Energy X-ray Absorptometry (DEXA) has been developed to make diagnosis of osteoporosis, and it is developed to analyze a material element for industrial use. Recently, we have developed a monochromatic X-ray CT using a 256 ch CdTe array detector. We found that the array detector systems are very useful for medical and industrial applications.

X-ray phase-contrast imaging

NASA Astrophysics Data System (ADS)

Endrizzi, Marco

2018-01-01

X-ray imaging is a standard tool for the non-destructive inspection of the internal structure of samples. It finds application in a vast diversity of fields: medicine, biology, many engineering disciplines, palaeontology and earth sciences are just few examples. The fundamental principle underpinning the image formation have remained the same for over a century: the X-rays traversing the sample are subjected to different amount of absorption in different parts of the sample. By means of phase-sensitive techniques it is possible to generate contrast also in relation to the phase shifts imparted by the sample and to extend the capabilities of X-ray imaging to those details that lack enough absorption contrast to be visualised in conventional radiography. A general overview of X-ray phase contrast imaging techniques is presented in this review, along with more recent advances in this fast evolving field and some examples of applications.

[The application of X-ray imaging in forensic medicine].

PubMed

Kučerová, Stěpánka; Safr, Miroslav; Ublová, Michaela; Urbanová, Petra; Hejna, Petr

2014-07-01

X-ray is the most common, basic and essential imaging method used in forensic medicine. It serves to display and localize the foreign objects in the body and helps to detect various traumatic and pathological changes. X-ray imaging is valuable in anthropological assessment of an individual. X-ray allows non-invasive evaluation of important findings before the autopsy and thus selection of the optimal strategy for dissection. Basic indications for postmortem X-ray imaging in forensic medicine include gunshot and explosive fatalities (identification and localization of projectiles or other components of ammunition, visualization of secondary missiles), sharp force injuries (air embolism, identification of the weapon) and motor vehicle related deaths. The method is also helpful for complex injury evaluation in abused victims or in persons where abuse is suspected. Finally, X-ray imaging still remains the gold standard method for identification of unknown deceased. With time modern imaging methods, especially computed tomography and magnetic resonance imaging, are more and more applied in forensic medicine. Their application extends possibilities of the visualization the bony structures toward a more detailed imaging of soft tissues and internal organs. The application of modern imaging methods in postmortem body investigation is known as digital or virtual autopsy. At present digital postmortem imaging is considered as a bloodless alternative to the conventional autopsy.

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.

Observation and theory of X-ray mirages

PubMed Central

Magnitskiy, Sergey; Nagorskiy, Nikolay; Faenov, Anatoly; Pikuz, Tatiana; Tanaka, Mamoko; Ishino, Masahiko; Nishikino, Masaharu; Fukuda, Yuji; Kando, Masaki; Kawachi, Tetsuya; Kato, Yoshiaki

2013-01-01

The advent of X-ray lasers allowed the realization of compact coherent soft X-ray sources, thus opening the way to a wide range of applications. Here we report the observation of unexpected concentric rings in the far-field beam profile at the output of a two-stage plasma-based X-ray laser, which can be considered as the first manifestation of a mirage phenomenon in X-rays. We have developed a method of solving the Maxwell–Bloch equations for this problem, and find that the experimentally observed phenomenon is due to the emergence of X-ray mirages in the plasma amplifier, appearing as phase-matched coherent virtual point sources. The obtained results bring a new insight into the physical nature of amplification of X-ray radiation in laser-induced plasma amplifiers and open additional opportunities for X-ray plasma diagnostics and extreme ultraviolet lithography. PMID:23733009

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

Sun, Cheng-Jun, E-mail: cjsun@aps.anl.gov; Brewe, Dale L.; Heald, Steve M.

X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorptionmore » near edge structure for Pr{sub 0.67}Sr{sub 0.33}MnO{sub 3} film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam.« less

High energy X-ray phase and dark-field imaging using a random absorption mask.

PubMed

Wang, Hongchang; Kashyap, Yogesh; Cai, Biao; Sawhney, Kawal

2016-07-28

High energy X-ray imaging has unique advantage over conventional X-ray imaging, since it enables higher penetration into materials with significantly reduced radiation damage. However, the absorption contrast in high energy region is considerably low due to the reduced X-ray absorption cross section for most materials. Even though the X-ray phase and dark-field imaging techniques can provide substantially increased contrast and complementary information, fabricating dedicated optics for high energies still remain a challenge. To address this issue, we present an alternative X-ray imaging approach to produce transmission, phase and scattering signals at high X-ray energies by using a random absorption mask. Importantly, in addition to the synchrotron radiation source, this approach has been demonstrated for practical imaging application with a laboratory-based microfocus X-ray source. This new imaging method could be potentially useful for studying thick samples or heavy materials for advanced research in materials science.

Observation and theory of X-ray mirages.

PubMed

Magnitskiy, Sergey; Nagorskiy, Nikolay; Faenov, Anatoly; Pikuz, Tatiana; Tanaka, Mamoko; Ishino, Masahiko; Nishikino, Masaharu; Fukuda, Yuji; Kando, Masaki; Kawachi, Tetsuya; Kato, Yoshiaki

2013-01-01

The advent of X-ray lasers allowed the realization of compact coherent soft X-ray sources, thus opening the way to a wide range of applications. Here we report the observation of unexpected concentric rings in the far-field beam profile at the output of a two-stage plasma-based X-ray laser, which can be considered as the first manifestation of a mirage phenomenon in X-rays. We have developed a method of solving the Maxwell-Bloch equations for this problem, and find that the experimentally observed phenomenon is due to the emergence of X-ray mirages in the plasma amplifier, appearing as phase-matched coherent virtual point sources. The obtained results bring a new insight into the physical nature of amplification of X-ray radiation in laser-induced plasma amplifiers and open additional opportunities for X-ray plasma diagnostics and extreme ultraviolet lithography.

X-ray detectors in medical imaging

NASA Astrophysics Data System (ADS)

Spahn, Martin

2013-12-01

Healthcare systems are subject to continuous adaptation, following trends such as the change of demographic structures, the rise of life-style related and chronic diseases, and the need for efficient and outcome-oriented procedures. This also influences the design of new imaging systems as well as their components. The applications of X-ray imaging in the medical field are manifold and have led to dedicated modalities supporting specific imaging requirements, for example in computed tomography (CT), radiography, angiography, surgery or mammography, delivering projection or volumetric imaging data. Depending on the clinical needs, some X-ray systems enable diagnostic imaging while others support interventional procedures. X-ray detector design requirements for the different medical applications can vary strongly with respect to size and shape, spatial resolution, frame rates and X-ray flux, among others. Today, integrating X-ray detectors are in common use. They are predominantly based on scintillators (e.g. CsI or Gd2O2S) and arrays of photodiodes made from crystalline silicon (Si) or amorphous silicon (a-Si) or they employ semiconductors (e.g. Se) with active a-Si readout matrices. Ongoing and future developments of X-ray detectors will include optimization of current state-of-the-art integrating detectors in terms of performance and cost, will enable the usage of large size CMOS-based detectors, and may facilitate photon counting techniques with the potential to further enhance performance characteristics and foster the prospect of new clinical applications.

X-Ray Absorption Microspectroscopy with Electrostatic Force Microscopy and its Application to Chemical States Mapping

NASA Astrophysics Data System (ADS)

Ishii, M.; Rigopoulos, N.; Poolton, N. R. J.; Hamilton, B.

2007-02-01

A new technique named X-EFM that measures the x-ray absorption fine structure (XAFS) of nanometer objects was developed. In X-EFM, electrostatic force microscopy (EFM) is used as an x-ray absorption detector, and photoionization induced by x-ray absorption of surface electron trapping sites is detected by EFM. An EFM signal with respect to x-ray photon energy provides the XAFS spectra of the trapping sites. We adopted X-EFM to observe Si oxide thin films. An edge jump shift intrinsic to the X-EFM spectrum was found, and it was explained with a model where an electric field between the trapping site and probe deepens the energy level of the inner-shell. A scanning probe under x-rays with fixed photon energy provided the chemical state mapping on the surface.

Structural Significance of Lipid Diversity as Studied by Small Angle Neutron and X-ray Scattering

DOE PAGES

Kučerka, Norbert; Heberle, Frederick A.; Pan, Jianjun; ...

2015-09-21

In this paper, we review recent developments in the rapidly growing field of membrane biophysics, with a focus on the structural properties of single lipid bilayers determined by different scattering techniques, namely neutron and X-ray scattering. The need for accurate lipid structural properties is emphasized by the sometimes conflicting results found in the literature, even in the case of the most studied lipid bilayers. Increasingly, accurate and detailed structural models require more experimental data, such as those from contrast varied neutron scattering and X-ray scattering experiments that are jointly refined with molecular dynamics simulations. This experimental and computational approach producesmore » robust bilayer structural parameters that enable insights, for example, into the interplay between collective membrane properties and its components (e.g., hydrocarbon chain length and unsaturation, and lipid headgroup composition). Finally, from model studies such as these, one is better able to appreciate how a real biological membrane can be tuned by balancing the contributions from the lipid’s different moieties (e.g., acyl chains, headgroups, backbones, etc.).« less

Accessing protein conformational ensembles using room-temperature X-ray crystallography

PubMed Central

Fraser, James S.; van den Bedem, Henry; Samelson, Avi J.; Lang, P. Therese; Holton, James M.; Echols, Nathaniel; Alber, Tom

2011-01-01

Modern protein crystal structures are based nearly exclusively on X-ray data collected at cryogenic temperatures (generally 100 K). The cooling process is thought to introduce little bias in the functional interpretation of structural results, because cryogenic temperatures minimally perturb the overall protein backbone fold. In contrast, here we show that flash cooling biases previously hidden structural ensembles in protein crystals. By analyzing available data for 30 different proteins using new computational tools for electron-density sampling, model refinement, and molecular packing analysis, we found that crystal cryocooling remodels the conformational distributions of more than 35% of side chains and eliminates packing defects necessary for functional motions. In the signaling switch protein, H-Ras, an allosteric network consistent with fluctuations detected in solution by NMR was uncovered in the room-temperature, but not the cryogenic, electron-density maps. These results expose a bias in structural databases toward smaller, overpacked, and unrealistically unique models. Monitoring room-temperature conformational ensembles by X-ray crystallography can reveal motions crucial for catalysis, ligand binding, and allosteric regulation. PMID:21918110

Small Angle X-Ray Scattering from Lipid-Bound Myelin Basic Protein in Solution

PubMed Central

Haas, H.; Oliveira, C. L. P.; Torriani, I. L.; Polverini, E.; Fasano, A.; Carlone, G.; Cavatorta, P.; Riccio, P.

2004-01-01

The structure of myelin basic protein (MBP), purified from the myelin sheath in both lipid-free (LF-MBP) and lipid-bound (LB-MBP) forms, was investigated in solution by small angle x-ray scattering. The water-soluble LF-MBP, extracted at pH < 3.0 from defatted brain, is the classical preparation of MBP, commonly regarded as an intrinsically unfolded protein. LB-MBP is a lipoprotein-detergent complex extracted from myelin with its native lipidic environment at pH > 7.0. Under all conditions, the scattering from the two protein forms was different, indicating different molecular shapes. For the LB-MBP, well-defined scattering curves were obtained, suggesting that the protein had a unique, compact (but not globular) structure. Furthermore, these data were compatible with earlier results from molecular modeling calculations on the MBP structure which have been refined by us. In contrast, the LF-MBP data were in accordance with the expected open-coil conformation. The results represent the first direct structural information from x-ray scattering measurements on MBP in its native lipidic environment in solution. PMID:14695288

Facile one-pot synthesis of hexagons of NaSrB5O9:Tb3+ phosphor for solid-state lighting

NASA Astrophysics Data System (ADS)

Ramesh, B.; Dillip, G. R.; Deva Prasad Raju, B.; Somasundaram, K.; Prasad Peddi, Siva; de Carvalho dos Anjos, Virgilio; Joo, S. W.

2017-04-01

NaSrB5O9:Tb3+ hexagons were synthesized by a facile solid-state reaction method. The synthesized powders were structurally examined by x-ray diffraction analysis (XRD), and Rietveld refinement was performed using the XRD data and Fullprof software. Hexagon-like morphology was observed using field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The elemental composition of the phosphors was investigated qualitatively by energy dispersive x-ray analysis (EDS) and quantitatively by x-ray photoelectron spectroscopy (XPS). The phosphor has a strong green emission at 545 nm under excitation of 379 nm, which is due to the 5{{\\text{D}}4}{{\\to}7}{{\\text{F}}5} transition of the Tb3+ ion. A lifetime of 3.48 ms was obtained for the phosphor. The important parameters of the light source were determined, such as the thermal quenching, critical distance, the nature of the dopant ion interaction, color coordinates, and quantum yield values. Other reported properties include the site occupancy of the dopant, surface properties, morphological properties, and optical properties.

Neutron and high-resolution room-temperature X-ray data collection from crystallized lytic polysaccharide monooxygenase

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

Bacik, John -Paul; Mekasha, Sophanit; Forsberg, Zarah

Bacteria and fungi express lytic polysaccharide monooxgyenase (LPMO) enzymes that act in conjunction with canonical hydrolytic sugar-processing enzymes to rapidly convert polysaccharides such as chitin, cellulose and starch to single monosaccharide products. In order to gain a better understanding of the structure and oxidative mechanism of these enzymes, large crystals (1–3 mm 3) of a chitin-processing LPMO from the Gram-positive soil bacterium Jonesia denitrificans were grown and screened for their ability to diffract neutrons. In addition to the collection of neutron diffraction data, which were processed to 2.1 Å resolution, a high-resolution room-temperature X-ray diffraction data set was collected andmore » processed to 1.1 Å resolution in space group P2 12 12 1. To our knowledge, this work marks the first successful neutron crystallographic experiment on an LPMO. As a result, joint X-ray/neutron refinement of the resulting data will reveal new details of the structure and mechanism of this recently discovered class of enzymes.« less

Neutron and high-resolution room-temperature X-ray data collection from crystallized lytic polysaccharide monooxygenase

DOE PAGES

Bacik, John -Paul; Mekasha, Sophanit; Forsberg, Zarah; ...

2015-01-01

Bacteria and fungi express lytic polysaccharide monooxgyenase (LPMO) enzymes that act in conjunction with canonical hydrolytic sugar-processing enzymes to rapidly convert polysaccharides such as chitin, cellulose and starch to single monosaccharide products. In order to gain a better understanding of the structure and oxidative mechanism of these enzymes, large crystals (1–3 mm 3) of a chitin-processing LPMO from the Gram-positive soil bacterium Jonesia denitrificans were grown and screened for their ability to diffract neutrons. In addition to the collection of neutron diffraction data, which were processed to 2.1 Å resolution, a high-resolution room-temperature X-ray diffraction data set was collected andmore » processed to 1.1 Å resolution in space group P2 12 12 1. To our knowledge, this work marks the first successful neutron crystallographic experiment on an LPMO. As a result, joint X-ray/neutron refinement of the resulting data will reveal new details of the structure and mechanism of this recently discovered class of enzymes.« less

Quantification of 2D elemental distribution maps of intermediate-thick biological sections by low energy synchrotron μ-X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Kump, P.; Vogel-Mikuš, K.

2018-05-01

Two fundamental-parameter (FP) based models for quantification of 2D elemental distribution maps of intermediate-thick biological samples by synchrotron low energy μ-X-ray fluorescence spectrometry (SR-μ-XRF) are presented and applied to the elemental analysis in experiments with monochromatic focused photon beam excitation at two low energy X-ray fluorescence beamlines—TwinMic, Elettra Sincrotrone Trieste, Italy, and ID21, ESRF, Grenoble, France. The models assume intermediate-thick biological samples composed of measured elements, the sources of the measurable spectral lines, and by the residual matrix, which affects the measured intensities through absorption. In the first model a fixed residual matrix of the sample is assumed, while in the second model the residual matrix is obtained by the iteration refinement of elemental concentrations and an adjusted residual matrix. The absorption of the incident focused beam in the biological sample at each scanned pixel position, determined from the output of a photodiode or a CCD camera, is applied as a control in the iteration procedure of quantification.

The effects of rigid motions on elastic network model force constants.

PubMed

Lezon, Timothy R

2012-04-01

Elastic network models provide an efficient way to quickly calculate protein global dynamics from experimentally determined structures. The model's single parameter, its force constant, determines the physical extent of equilibrium fluctuations. The values of force constants can be calculated by fitting to experimental data, but the results depend on the type of experimental data used. Here, we investigate the differences between calculated values of force constants and data from NMR and X-ray structures. We find that X-ray B factors carry the signature of rigid-body motions, to the extent that B factors can be almost entirely accounted for by rigid motions alone. When fitting to more refined anisotropic temperature factors, the contributions of rigid motions are significantly reduced, indicating that the large contribution of rigid motions to B factors is a result of over-fitting. No correlation is found between force constants fit to NMR data and those fit to X-ray data, possibly due to the inability of NMR data to accurately capture protein dynamics. Copyright © 2011 Wiley Periodicals, Inc.

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.

Structural investigations of Pu{sup III} phosphate by X-ray diffraction, MAS-NMR and XANES spectroscopy

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

Popa, Karin; Raison, Philippe E., E-mail: philippe.raison@ec.europa.eu; Martel, Laura

2015-10-15

PuPO{sub 4} was prepared by a solid state reaction method and its crystal structure at room temperature was solved by powder X-ray diffraction combined with Rietveld refinement. High resolution XANES measurements confirm the +III valence state of plutonium, in agreement with valence bond derivation. The presence of the americium (as β{sup −} decay product of plutonium) in the +III oxidation state was determined based on XANES spectroscopy. High resolution solid state {sup 31}P NMR agrees with the XANES results and the presence of a solid-solution. - Graphical abstract: A full structural analysis of PuPO{sub 4} based on Rietveld analysis ofmore » room temperature X-ray diffraction data, XANES and MAS NMR measurements was performed. - Highlights: • The crystal structure of PuPO{sub 4} monazite is solved. • In PuPO{sub 4} plutonium is strictly trivalent. • The presence of a minute amount of Am{sup III} is highlighted. • We propose PuPO{sub 4} as a potential reference material for spectroscopic and microscopic studies.« less

A highly sensitive x-ray imaging modality for hepatocellular carcinoma detection in vitro

NASA Astrophysics Data System (ADS)

Rand, Danielle; Walsh, Edward G.; Derdak, Zoltan; Wands, Jack R.; Rose-Petruck, Christoph

2015-01-01

Innovations that improve sensitivity and reduce cost are of paramount importance in diagnostic imaging. The novel x-ray imaging modality called spatial frequency heterodyne imaging (SFHI) is based on a linear arrangement of x-ray source, tissue, and x-ray detector, much like that of a conventional x-ray imaging apparatus. However, SFHI rests on a complete paradigm reversal compared to conventional x-ray absorption-based radiology: while scattered x-rays are carefully rejected in absorption-based x-ray radiology to enhance the image contrast, SFHI forms images exclusively from x-rays scattered by the tissue. In this study we use numerical processing to produce x-ray scatter images of hepatocellular carcinoma labeled with a nanoparticle contrast agent. We subsequently compare the sensitivity of SFHI in this application to that of both conventional x-ray imaging and magnetic resonance imaging (MRI). Although SFHI is still in the early stages of its development, our results show that the sensitivity of SFHI is an order of magnitude greater than that of absorption-based x-ray imaging and approximately equal to that of MRI. As x-ray imaging modalities typically have lower installation and service costs compared to MRI, SFHI could become a cost effective alternative to MRI, particularly in areas of the world with inadequate availability of MRI facilities.

Laser power meters as an X-ray power diagnostic for LCLS-II

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

Heimann, Philip; Moeller, Stefan; Carbajo, Sergio

For the LCLS-II X-ray instruments, laser power meters are being developed as compact X-ray power diagnostics to operate at soft and tender X-ray photon energies. These diagnostics can be installed at various locations along an X-ray free-electron laser (FEL) beamline in order to monitor the transmission of X-ray optics along the beam path. In addition, the power meters will be used to determine the absolute X-ray power at the endstations. Here, thermopile power meters, which measure average power, and have been chosen primarily for their compatibility with the high repetition rates at LCLS-II, are evaluated. Here, a number of characteristicsmore » in the soft X-ray range are presented including linearity, calibrations conducted with a photodiode and a gas monitor detector as well as ultra-high-vacuum compatibility tests using residual gas analysis. The application of these power meters for LCLS-II and other X-ray FEL sources is discussed.« less

Evaluation of the sensitivity and fading characteristics of an image plate system for x-ray diagnostics

NASA Astrophysics Data System (ADS)

Meadowcroft, A. L.; Bentley, C. D.; Stott, E. N.

2008-11-01

Image plates (IPs) are a reusable recording media capable of detecting ionizing radiation, used to diagnose x-ray emission from laser-plasma experiments. Due to their superior performance characteristics in x-ray applications [C. C. Bradford, W. W. Peppler, and J. T. Dobbins III, Med. Phys. 26, 27 (1999) and J. Digit. Imaging. 12, 54 (1999)], the Fuji Biological Analysis System (BAS) IPs are fielded on x-ray diagnostics for the HELEN laser by the Plasma Physics Department at AWE. The sensitivities of the Fuji BAS IPs have been absolutely calibrated for absolute measurements of x-ray intensity in the energy range of 0-100 keV. In addition, the Fuji BAS IP fading as a function of time was investigated. We report on the characterization of three Fuji BAS IP responses to x-rays using a radioactive source, and discrete x-ray line energies generated by the Excalibur soft x-ray facility and the Defense Radiological Standards Centre filter-fluorescer hard x-ray system at AWE.

Laser power meters as an X-ray power diagnostic for LCLS-II.

PubMed

Heimann, Philip; Moeller, Stefan; Carbajo, Sergio; Song, Sanghoon; Dakovski, Georgi; Nordlund, Dennis; Fritz, David

2018-01-01

For the LCLS-II X-ray instruments, laser power meters are being developed as compact X-ray power diagnostics to operate at soft and tender X-ray photon energies. These diagnostics can be installed at various locations along an X-ray free-electron laser (FEL) beamline in order to monitor the transmission of X-ray optics along the beam path. In addition, the power meters will be used to determine the absolute X-ray power at the endstations. Here, thermopile power meters, which measure average power, and have been chosen primarily for their compatibility with the high repetition rates at LCLS-II, are evaluated. A number of characteristics in the soft X-ray range are presented including linearity, calibrations conducted with a photodiode and a gas monitor detector as well as ultra-high-vacuum compatibility tests using residual gas analysis. The application of these power meters for LCLS-II and other X-ray FEL sources is discussed.

Laser power meters as an X-ray power diagnostic for LCLS-II

DOE PAGES

Heimann, Philip; Moeller, Stefan; Carbajo, Sergio; ...

2018-01-01

For the LCLS-II X-ray instruments, laser power meters are being developed as compact X-ray power diagnostics to operate at soft and tender X-ray photon energies. These diagnostics can be installed at various locations along an X-ray free-electron laser (FEL) beamline in order to monitor the transmission of X-ray optics along the beam path. In addition, the power meters will be used to determine the absolute X-ray power at the endstations. Here, thermopile power meters, which measure average power, and have been chosen primarily for their compatibility with the high repetition rates at LCLS-II, are evaluated. Here, a number of characteristicsmore » in the soft X-ray range are presented including linearity, calibrations conducted with a photodiode and a gas monitor detector as well as ultra-high-vacuum compatibility tests using residual gas analysis. The application of these power meters for LCLS-II and other X-ray FEL sources is discussed.« less

Influence of nanogold additives on phase formation, microstructure and dielectric properties of perovskite BaTiO3 ceramics

NASA Astrophysics Data System (ADS)

Nonkumwong, Jeeranan; Ananta, Supon; Srisombat, Laongnuan

2015-06-01

The formation of perovskite phase, microstructure and dielectric properties of nanogold-modified barium titanate (BaTiO3) ceramics was examined as a function of gold nanoparticle contents by employing a combination of X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray, Archimedes principle and dielectric measurement techniques. These ceramics were fabricated from a simple mixed-oxide method. The amount of gold nanoparticles was found to be one of the key factors controlling densification, grain growth and dielectric response in BaTiO3 ceramics. It was found that under suitable amount of nanogold addition (4 mol%), highly dense perovskite BaTiO3 ceramics with homogeneous microstructures of refined grains (~0.5-3.1 μm) and excellence dielectric properties can be produced.

Covalent Incorporation of Selenium into Oligonucleotides for X-ray Crystal Structure Determination via MAD: Proof of Principle

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

Teplova, M.; Wilds, C.J.; Wawrzak, Z.

2010-03-08

Selenium was incorporated into an oligodeoxynucleotide in the form of 2'-methylseleno-uridine (U{sub Se}). The X-ray crystal structure of the duplex d(GCGTA)U{sub Se}d(ACGC){sub 2} was determined by the multiwavelength anomalous dispersion (MAD) technique and refined to a resolution of 1.3 {angstrom}, demonstrating that selenium can selectively substitute oxygen in DNA and that the resulting compounds are chemically stable. Since derivatization at the 2'-{alpha}-position with selenium does not affect the preference of the sugar for the C3'-endo conformation, this strategy is suitable for incorporating selenium into RNA. The availability of selenium-containing nucleic acids for crystallographic phasing offers an attractive alternative to themore » commonly used halogenated pyrimidines.« less

X-ray and dielectric characterization of Co doped tetragonal BaTiO3 ceramics

NASA Astrophysics Data System (ADS)

Bujakiewicz-Koronska, R.; Vasylechko, L.; Markiewicz, E.; Nalecz, D. M.; Kalvane, A.

2017-01-01

The crystal structure modifications of BaTiO3 induced by cobalt doping were studied. The polycrystalline (1 - x)BaTiO3 + xCo2O3 samples, with x ≤ 10 wt.%, were prepared by high temperature sintering conventional method. According to X-ray phase and structural characterization, performed by full-profile Rietveld refinement technique, all synthesized samples showed tetragonal symmetry perovskite structure with minor amount of parasitic phases. Pure single-phase composition has been detected only in the low level of doping BaTiO3. It was indicated that substitution of Co for the Ti sites in the (1 - x)BaTiO3 + xCo2O3 series led to decrease of tetragonality (c/a) of the BaTiO3 perovskite structure. This effect almost vanished in the (1 - x)BaTiO3 + xCo2O3 samples with nominal Co content higher than ∼1 wt.%, in which precipitation of parasitic Co-containing phases CoO and Co2TiO4 has been observed. Based on the results, the solubility limit of Co in Ti sub-lattice in the (1 - x)BaTiO3 + xCo2O3 series is estimated as x = 0.75 wt.%.

High resolution imaging and lithography with hard x rays using parabolic compound refractive lenses

NASA Astrophysics Data System (ADS)

Schroer, C. G.; Benner, B.; Günzler, T. F.; Kuhlmann, M.; Zimprich, C.; Lengeler, B.; Rau, C.; Weitkamp, T.; Snigirev, A.; Snigireva, I.; Appenzeller, J.

2002-03-01

Parabolic compound refractive lenses are high quality optical components for hard x rays. They are particularly suited for full field imaging, with applications in microscopy and x-ray lithography. Taking advantage of the large penetration depth of hard x rays, the interior of opaque samples can be imaged with submicrometer resolution. To obtain the three-dimensional structure of a sample, microscopy is combined with tomographic techniques. In a first hard x-ray lithography experiment, parabolic compound refractive lenses have been used to project the reduced image of a lithography mask onto a resist. Future developments are discussed.

A Magnetron Sputter Deposition System for the Development of Multilayer X-Ray Optics

NASA Technical Reports Server (NTRS)

Broadway, David; Ramsey, Brian; Gubarev, Mikhail

2014-01-01

The proposal objective is to establish the capability to deposit multilayer structures for x-ray, neutron, and EUV optic applications through the development of a magnetron sputtering deposition system. A specific goal of this endeavor is to combine multilayer deposition technology with the replication process in order to enhance the MSFC's position as a world leader in the design of innovative X-ray instrumentation through the development of full shell replicated multilayer optics. The development of multilayer structures is absolutely necessary in order to advance the field of X-ray astronomy by pushing the limit for observing the universe to ever increasing photon energies (i. e. up to 200 keV or higher); well beyond Chandra (approx. 10 keV) and NuStar's (approx. 75 keV) capability. The addition of multilayer technology would significantly enhance the X-ray optics capability at MSFC and allow NASA to maintain its world leadership position in the development, fabrication and design of innovative X-ray instrumentation which would be the first of its kind by combining multilayer technology with the mirror replication process. This marriage of these technologies would allow astronomers to see the universe in a new light by pushing to higher energies that are out of reach with today's instruments.To this aim, a magnetron vacum sputter deposition system for the deposition of novel multilayer thin film X-ray optics is proposed. A significant secondary use of the vacuum deposition system includes the capability to fabricate multilayers for applications in the field of EUV optics for solar physics, neutron optics, and X-ray optics for a broad range of applications including medical imaging.

A Magnetron Sputter Deposition System for the Development of X-Ray Multilayer Optics

NASA Technical Reports Server (NTRS)

Broadway, David

2015-01-01

The project objective is to establish the capability to deposit multilayer structures for x-ray, neutron, and extreme ultraviolet (EUV) optic applications through the development of a magnetron sputtering deposition system. A specific goal of this endeavor is to combine multilayer deposition technology with the replication process in order to enhance NASA Marshall Space Flight Center's (MSFC's) position as a world leader in the design of innovative x-ray instrumentation through the development of full shell replicated multilayer optics. The development of multilayer structures are absolutely necessary in order to advance the field of x-ray astronomy by pushing the limit for observing the universe to ever-increasing photon energies (i.e., up to 200 keV or higher), well beyond Chandra's (approx.10 keV) and NuStar's (approx.75 keV) capability. The addition of multilayer technology would significantly enhance the x-ray optics capability at MSFC and allow NASA to maintain its world leadership position in the development, fabrication, and design of innovative x-ray instrumentation, which would be the first of its kind by combining multilayer technology with the mirror replication process. This marriage of these technologies would allow astronomers to see the universe in a new light by pushing to higher energies that are out of reach with today's instruments. To this aim, a magnetron vacuum sputter deposition system for the deposition of novel multilayer thin film x-ray optics is proposed. A significant secondary use of the vacuum deposition system includes the capability to fabricate multilayers for applications in the field of EUV optics for solar physics, neutron optics, and x-ray optics for a broad range of applications including medical imaging.

Structure-phase state and mechanical properties of surface layers in titanium nikelide single crystals after shock mechanical treatment

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

Surikova, N., E-mail: surikova@ispms.tsc.ru; Panin, V., E-mail: paninve@ispms.tsc.ru; Vlasov, I.

2015-10-27

The influence of ultrasonic shock surface treatment (USST) on refine structure and mechanical characteristics of surface layers and deformation behaviour of volume samples of TiNi(Fe, Mo) shape memory effect alloy single crystals is studied using optical and transmission electron microscope, X-ray diffraction, nanoindentation, mechanical attrition testing and experiments on uniaxial tension.

Structure-phase state and mechanical properties of surface layers in titanium nikelide single crystals after shock mechanical treatment

NASA Astrophysics Data System (ADS)

Surikova, N.; Panin, V.; Vlasov, I.; Narkevich, N.; Surikov, N.; Tolmachev, A.

2015-10-01

The influence of ultrasonic shock surface treatment (USST) on refine structure and mechanical characteristics of surface layers and deformation behaviour of volume samples of TiNi(Fe, Mo) shape memory effect alloy single crystals is studied using optical and transmission electron microscope, X-ray diffraction, nanoindentation, mechanical attrition testing and experiments on uniaxial tension.

Microanalysis of iron oxidation state in iron oxides using X Ray Absorption Near Edge Structure (XANES)

NASA Technical Reports Server (NTRS)

Sutton, S. R.; Delaney, J.; Bajt, S.; Rivers, M. L.; Smith, J. V.

1993-01-01

An exploratory application of x ray absorption near edge structure (XANES) analysis using the synchrotron x ray microprobe was undertaken to obtain Fe XANES spectra on individual sub-millimeter grains in conventional polished sections. The experiments concentrated on determinations of Fe valence in a suite of iron oxide minerals for which independent estimates of the iron speciation could be made by electron microprobe analysis and x ray diffraction.

Course Manual for X-Ray Applications.

ERIC Educational Resources Information Center

Food and Drug Administration (DHEW), Rockville, MD. Bureau of Radiological Health.

This publication is the third of three sequential course manuals for instructors in x-ray science and engineering. This course manual has been tested by introducing it into the Oregon State University curriculum. The publication is prepared for the purpose of improving the qualifications of x-ray users and to reduce the ionizing radiation exposure…

Evaluation of size, morphology, concentration, and surface effect of gold nanoparticles on X-ray attenuation in computed tomography.

PubMed

Khademi, Sara; Sarkar, Saeed; Kharrazi, Sharmin; Amini, Seyed Mohammad; Shakeri-Zadeh, Ali; Ay, Mohammad Reza; Ghadiri, Hossein

2018-01-01

Increasing attention has been focused on the use of nanostructures as contrast enhancement agents in medical imaging, especially in computed tomography (CT). To date, gold nanoparticles (GNPs) have been demonstrated to have great potential as contrast agents for CT imaging. This study was designed to evaluate any effect on X-ray attenuation that might result from employing GNPs with a variety of shapes, sizes, surface chemistries, and concentrations. Gold nanorods (GNRs) and spherical GNPs were synthesized for this application. X-ray attenuation was quantified by Hounsfield unit (HU) in CT. Our findings indicated that smaller spherical GNPs (13 nm) had higher X-ray attenuation than larger ones (60 nm) and GNRs with larger aspect ratio exhibited great effect on X-ray attenuation. Moreover, poly ethylene glycol (PEG) coating on GNRs declined X-ray attenuation as a result of limiting the aggregation of GNRs. We observed X-ray attenuation increased when mass concentration of GNPs was elevated. Overall, smaller spherical GNPs can be suggested as a better alternative to Omnipaque, a good contrast agent for CT imaging. This data can be also considered for the application of gold nanostructures in radiation dose enhancement where nanoparticles with high X-ray attenuation are applied. Copyright © 2017 Associazione Italiana di Fisica Medica. Published by Elsevier Ltd. All rights reserved.

X-ray echo spectroscopy (Conference Presentation)

NASA Astrophysics Data System (ADS)

Shvyd'ko, Yuri V.

2016-09-01

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

Optics for coherent X-ray applications

PubMed Central

Yabashi, Makina; Tono, Kensuke; Mimura, Hidekazu; Matsuyama, Satoshi; Yamauchi, Kazuto; Tanaka, Takashi; Tanaka, Hitoshi; Tamasaku, Kenji; Ohashi, Haruhiko; Goto, Shunji; Ishikawa, Tetsuya

2014-01-01

Developments of X-ray optics for full utilization of diffraction-limited storage rings (DLSRs) are presented. The expected performance of DLSRs is introduced using the design parameters of SPring-8 II. To develop optical elements applicable to manipulation of coherent X-rays, advanced technologies on precise processing and metrology were invented. With propagation-based coherent X-rays at the 1 km beamline of SPring-8, a beryllium window fabricated with the physical-vapour-deposition method was found to have ideal speckle-free properties. The elastic emission machining method was utilized for developing reflective mirrors without distortion of the wavefronts. The method was further applied to production of diffraction-limited focusing mirrors generating the smallest spot size in the sub-10 nm regime. To enable production of ultra-intense nanobeams at DLSRs, a low-vibration cooling system for a high-heat-load monochromator and advanced diagnostic systems to characterize X-ray beam properties precisely were developed. Finally, new experimental schemes for combinative nano-analysis and spectroscopy realised with novel X-ray optics are discussed. PMID:25177986

MICROANALYSIS OF MATERIALS USING SYNCHROTRON RADIATION.

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

JONES,K.W.; FENG,H.

2000-12-01

High intensity synchrotron radiation produces photons with wavelengths that extend from the infrared to hard x rays with energies of hundreds of keV with uniquely high photon intensities that can be used to determine the composition and properties of materials using a variety of techniques. Most of these techniques represent extensions of earlier work performed with ordinary tube-type x-ray sources. The properties of the synchrotron source such as the continuous range of energy, high degree of photon polarization, pulsed beams, and photon flux many orders of magnitude higher than from x-ray tubes have made possible major advances in the possiblemore » chemical applications. We describe here ways that materials analyses can be made using the high intensity beams for measurements with small beam sizes and/or high detection sensitivity. The relevant characteristics of synchrotron x-ray sources are briefly summarized to give an idea of the x-ray parameters to be exploited. The experimental techniques considered include x-ray fluorescence, absorption, and diffraction. Examples of typical experimental apparatus used in these experiments are considered together with descriptions of actual applications.« less

High spatial resolution soft-x-ray microscopy

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

Meyer-Ilse, W.; Medecki, H.; Brown, J.T.

1997-04-01

A new soft x-ray microscope (XM-1) with high spatial resolution has been constructed by the Center for X-ray Optics. It uses bending magnet radiation from beamline 6.1 at the Advanced Light Source, and is used in a variety of projects and applications in the life and physical sciences. Most of these projects are ongoing. The instrument uses zone plate lenses and achieves a resolution of 43 nm, measured over 10% to 90% intensity with a knife edge test sample. X-ray microscopy permits the imaging of relatively thick samples, up to 10 {mu}m thick, in water. XM-1 has an easy tomore » use interface, that utilizes visible light microscopy to precisely position and focus the specimen. The authors describe applications of this device in the biological sciences, as well as in studying industrial applications including structured polymer samples.« less

Replicated x-ray optics for space applications

NASA Astrophysics Data System (ADS)

Hudec, René; Pína, Ladislav; Inneman, Adolf

2017-11-01

We report on the program of design and development of X-ray optics for space applications in the Czech Republic. Having more than 30 years background in X-ray optics development for space applications (for use in astronomical X-ray telescopes onboard spacecrafts, before 1989 mostly for Soviet and East European INTERKOSMOS program), we focus nowadays on novel technologies and approaches, thin shell replicated mirrors, as well as studies of light-weight mirrors based on innovative materials such as ceramics. The collaboration includes teams from the Academy of Sciences, Universities, and industry. We will describe and discuss both the history of the development of Xray optics in the Czech Republic and the developed technologies and approaches (with focus on replication technology) as well as recent activities and developments including our participation on the ESA XEUS mirror technology development based on the Agreement between ESA and Czech Government.

Soft X-ray radiation damage in EM-CCDs used for Resonant Inelastic X-ray Scattering

NASA Astrophysics Data System (ADS)

Gopinath, D.; Soman, M.; Holland, A.; Keelan, J.; Hall, D.; Holland, K.; Colebrook, D.

2018-02-01

Advancement in synchrotron and free electron laser facilities means that X-ray beams with higher intensity than ever before are being created. The high brilliance of the X-ray beam, as well as the ability to use a range of X-ray energies, means that they can be used in a wide range of applications. One such application is Resonant Inelastic X-ray Scattering (RIXS). RIXS uses the intense and tuneable X-ray beams in order to investigate the electronic structure of materials. The photons are focused onto a sample material and the scattered X-ray beam is diffracted off a high resolution grating to disperse the X-ray energies onto a position sensitive detector. Whilst several factors affect the total system energy resolution, the performance of RIXS experiments can be limited by the spatial resolution of the detector used. Electron-Multiplying CCDs (EM-CCDs) at high gain in combination with centroiding of the photon charge cloud across several detector pixels can lead to sub-pixel spatial resolution of 2-3 μm. X-ray radiation can cause damage to CCDs through ionisation damage resulting in increases in dark current and/or a shift in flat band voltage. Understanding the effect of radiation damage on EM-CCDs is important in order to predict lifetime as well as the change in performance over time. Two CCD-97s were taken to PTB at BESSY II and irradiated with large doses of soft X-rays in order to probe the front and back surfaces of the device. The dark current was shown to decay over time with two different exponential components to it. This paper will discuss the use of EM-CCDs for readout of RIXS spectrometers, and limitations on spatial resolution, together with any limitations on instrument use which may arise from X-ray-induced radiation damage.

Two-dimensional ultrahigh-density X-ray optical memory.

PubMed

Bezirganyan, Hakob P; Bezirganyan, Siranush E; Bezirganyan, Hayk H; Bezirganyan, Petros H

2007-01-01

Most important aspect of nanotechnology applications in the information ultrahigh storage is the miniaturization of data carrier elements of the storage media with emphasis on the long-term stability. Proposed two-dimensional ultrahigh-density X-ray optical memory, named X-ROM, with long-term stability is an information carrier basically destined for digital data archiving. X-ROM is a semiconductor wafer, in which the high-reflectivity nanosized X-ray mirrors are embedded. Data are encoded due to certain positions of the mirrors. Ultrahigh-density data recording procedure can e.g., be performed via mask-less zone-plate-array lithography (ZPAL), spatial-phase-locked electron-beam lithography (SPLEBL), or focused ion-beam lithography (FIB). X-ROM manufactured by nanolithography technique is a write-once memory useful for terabit-scale memory applications, if the surface area of the smallest recording pits is less than 100 nm2. In this case the X-ROM surface-storage capacity of a square centimetre becomes by two orders of magnitude higher than the volumetric data density really achieved for three-dimensional optical data storage medium. Digital data read-out procedure from proposed X-ROM can e.g., be performed via glancing-angle incident X-ray micro beam (GIX) using the well-developed X-ray reflectometry technique. In presented theoretical paper the crystal-analyser operating like an image magnifier is added to the set-up of X-ROM data handling system for the purpose analogous to case of application the higher numerical aperture objective in optical data read-out system. We also propose the set-up of the X-ROM readout system based on more the one incident X-ray micro beam. Presented scheme of two-beam data handling system, which operates on two mutually perpendicular well-collimated monochromatic incident X-ray micro beams, essentially increases the reliability of the digital information read-out procedure. According the graphs of characteristic functions presented in paper, one may choose optimally the incident radiation wavelength, as well as the angle of incidence of X-ray micro beams, appropriate for proposed digital data read-out procedure.

Design of a normal incidence multilayer imaging x-ray microscope.

PubMed

Shealy, D L; Gabardi, D R; Hoover, R B; Walker, A B; Lindblom, J F; Barbee, T W

1989-01-01

Normal incidence multilayer Cassegrain x-ray telescopes were flown on the Stanford/MSFC Rocket X-Ray Spectroheliograph. These instruments produced high spatial resolution images of the Sun and conclusively demonstrated that doubly reflecting multilayer x-ray optical systems are feasible. The images indicated that aplanatic imaging soft x-ray /EUV microscopes should be achievable using multilayer optics technology. We have designed a doubly reflecting normal incidence multilayer imaging x-ray microscope based on the Schwarzschild configuration. The Schwarzschild microscope utilizes two spherical mirrors with concentric radii of curvature which are chosen such that the third-order spherical aberration and coma are minimized. We discuss the design of the microscope and the results of the optical system ray trace analysis which indicates that diffraction-limited performance with 600 Å spatial resolution should be obtainable over a 1 mm field of view at a wavelength of 100 Å. Fabrication of several imaging soft x-ray microscopes based upon these designs, for use in conjunction with x-ray telescopes and laser fusion research, is now in progress. High resolution aplanatic imaging x-ray microscopes using normal incidence multilayer x-ray mirrors should have many important applications in advanced x-ray astronomical instrumentation, x-ray lithography, biological, biomedical, metallurgical, and laser fusion research.

SU-E-T-25: Real Time Simulator for Designing Electron Dual Scattering Foil Systems.

PubMed

Carver, R; Hogstrom, K; Price, M; Leblanc, J; Harris, G

2012-06-01

To create a user friendly, accurate, real time computer simulator to facilitate the design of dual foil scattering systems for electron beams on radiotherapy accelerators. The simulator should allow for a relatively quick, initial design that can be refined and verified with subsequent Monte Carlo (MC) calculations and measurements. The simulator consists of an analytical algorithm for calculating electron fluence and a graphical user interface (GUI) C++ program. The algorithm predicts electron fluence using Fermi-Eyges multiple Coulomb scattering theory with a refined Moliere formalism for scattering powers. The simulator also estimates central-axis x-ray dose contamination from the dual foil system. Once the geometry of the beamline is specified, the simulator allows the user to continuously vary primary scattering foil material and thickness, secondary scattering foil material and Gaussian shape (thickness and sigma), and beam energy. The beam profile and x-ray contamination are displayed in real time. The simulator was tuned by comparison of off-axis electron fluence profiles with those calculated using EGSnrc MC. Over the energy range 7-20 MeV and using present foils on the Elekta radiotherapy accelerator, the simulator profiles agreed to within 2% of MC profiles from within 20 cm of the central axis. The x-ray contamination predictions matched measured data to within 0.6%. The calculation time was approximately 100 ms using a single processor, which allows for real-time variation of foil parameters using sliding bars. A real time dual scattering foil system simulator has been developed. The tool has been useful in a project to redesign an electron dual scattering foil system for one of our radiotherapy accelerators. The simulator has also been useful as an instructional tool for our medical physics graduate students. © 2012 American Association of Physicists in Medicine.

The Use of In Situ X-ray Imaging Methods in the Research and Development of Magnesium-Based Grain-Refined and Nanocomposite Materials

NASA Astrophysics Data System (ADS)

Sillekens, W. H.; Casari, D.; Mirihanage, W. U.; Terzi, S.; Mathiesen, R. H.; Salvo, L.; Daudin, R.; Lhuissier, P.; Guo, E.; Lee, P. D.

2016-12-01

Metallurgists have an ever-increasing suite of analytical techniques at their disposition. Among these techniques are the in situ methods, being those approaches that are designed to actually study events that occur in the material during for instance solidification, (thermo)-mechanical working or heat treatment. As such they are a powerful tool in unraveling the mechanisms behind these processes, supplementary to ex situ methods that instead analyze the materials before and after their processing. In this paper, case studies are presented of how in situ imaging methods—and more specifically micro-focus x-ray radiography and synchrotron x-ray tomography—are used in the research and development of magnesium-based grain-refined and nanocomposite materials. These results are drawn from the EC collaborative research project ExoMet (www.exomet-project.eu). The first example concerns the solidification of a Mg-Nd-Gd alloy with Zr addition to assess the role of zirconium content and cooling rate in crystal nucleation and growth. The second example concerns the solidification of a Mg-Zn-Al alloy and its SiC-containing nanocomposite material to reveal the influence of particle addition on microstructural development. The third example concerns the (partial) melting-solidification of Elektron21/AlN and Elektron21/Y2O3 nanocomposite materials to study such effects as particle pushing/engulfment and agglomeration during repeated processing. Such studies firstly visualize and by that confirm what is known or assumed. Secondly, they advance science by monitoring and quantifying phenomena as they evolve during processing and by that contribute toward a better understanding of the physics at play.

Structural, vibrational and dielectric studies of (0.95)Pb(Zr{sub x}Ti{sub 1−x})O{sub 3}-(0.05)BiFeO{sub 3} nanoceramics

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

Sharma, Subhash, E-mail: rk.dwivedi@jiit.ac.in; Singh, Vikash, E-mail: rk.dwivedi@jiit.ac.in; Dwivedi, R. K., E-mail: rk.dwivedi@jiit.ac.in

2014-04-24

(0.95)Pb(Zr{sub x}Ti{sub 1−x})O{sub 3}-(0.05)BiFeO{sub 3} nanoceramics with x=0.51, 0.53 and 0.55 were synthesized by sol-gel route. Rietveld refined X-ray powder diffraction pattern of the samples confirm the single phase formation of compounds with tetragonal structure (P4mm). FT-IR studies revealed that slight shift of phonon modes towards the lower wave number and increase in the bond length with increasing Zr{sup 4+} concentration. Room temperature dielectric properties of system revealed that relaxor characteristics of these samples. Ferroelectric hysteresis curve shows the decrease in polarization values with Zr concentration.

Structure and magnetic properties of flux grown single crystals of Co3-xFexSn2S2 shandites

NASA Astrophysics Data System (ADS)

Kassem, Mohamed A.; Tabata, Yoshikazu; Waki, Takeshi; Nakamura, Hiroyuki

2016-01-01

We report a successful single crystal growth of the shandite-type half-metallic ferromagnet Co3Sn2S2, and its Fe-substituted compounds, Co3-xFexSn2S2, by employing the flux method. Although Fe3Sn2S2 is unstable phase, we found that using the self Sn flux enables us to obtain single phase crystals up to x=0.53. The chemical composition of the grown plate-shaped single crystals was examined using wavelength-dispersive X-ray spectroscopy. The shandite structure with R 3 ̅m symmetry was confirmed by powder X-ray diffraction and the crystal structure parameters were refined using the Rietveld method. Magnetization measurements show suppression of the ferromagnetic order upon Fe-substitution , as well as in other substituted systems such as In- and Ni-substituted Co3Sn2S2. The almost identical magnetic phase diagrams of the Fe- and In-substituted compounds indicate that the electron number is dominantly significant to the magnetism in the Co-based shandite.

Structure and atomic correlations in molecular systems probed by XAS reverse Monte Carlo refinement

NASA Astrophysics Data System (ADS)

Di Cicco, Andrea; Iesari, Fabio; Trapananti, Angela; D'Angelo, Paola; Filipponi, Adriano

2018-03-01

The Reverse Monte Carlo (RMC) algorithm for structure refinement has been applied to x-ray absorption spectroscopy (XAS) multiple-edge data sets for six gas phase molecular systems (SnI2, CdI2, BBr3, GaI3, GeBr4, GeI4). Sets of thousands of molecular replicas were involved in the refinement process, driven by the XAS data and constrained by available electron diffraction results. The equilibrated configurations were analysed to determine the average tridimensional structure and obtain reliable bond and bond-angle distributions. Detectable deviations from Gaussian models were found in some cases. This work shows that a RMC refinement of XAS data is able to provide geometrical models for molecular structures compatible with present experimental evidence. The validation of this approach on simple molecular systems is particularly important in view of its possible simple extension to more complex and extended systems including metal-organic complexes, biomolecules, or nanocrystalline systems.

Formation and mechanism of nanocrystalline AZ91 powders during HDDR processing

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

Liu, Yafen; Fan, Jianfeng, E-mail: fanjianfeng@tyu

2017-03-15

Grain sizes of AZ91 alloy powders were markedly refined to about 15 nm from 100 to 160 μm by an optimized hydrogenation-disproportionation-desorption-recombination (HDDR) process. The effect of temperature, hydrogen pressure and processing time on phase and microstructure evolution of AZ91 alloy powders during HDDR process was investigated systematically by X-ray diffraction, optical microscopy, scanning electron microscopy and transmission electron microscopy, respectively. The optimal HDDR process for preparing nanocrystalline Mg alloy powders is hydriding at temperature of 350 °C under 4 MPa hydrogen pressure for 12 h and dehydriding at 350 °C for 3 h in vacuum. A modified unreacted coremore » model was introduced to describe the mechanism of grain refinement of during HDDR process. - Highlights: • Grain size of the AZ91 alloy powders was significantly refined from 100 μm to 15 nm. • The optimal HDDR technology for nano Mg alloy powders is obtained. • A modified unreacted core model of grain refinement mechanism was proposed.« less

Integrated description of protein dynamics from room-temperature X-ray crystallography and NMR

PubMed Central

Fenwick, R. Bryn; van den Bedem, Henry; Fraser, James S.; Wright, Peter E.

2014-01-01

Detailed descriptions of atomic coordinates and motions are required for an understanding of protein dynamics and their relation to molecular recognition, catalytic function, and allostery. Historically, NMR relaxation measurements have played a dominant role in the determination of the amplitudes and timescales (picosecond–nanosecond) of bond vector fluctuations, whereas high-resolution X-ray diffraction experiments can reveal the presence of and provide atomic coordinates for multiple, weakly populated substates in the protein conformational ensemble. Here we report a hybrid NMR and X-ray crystallography analysis that provides a more complete dynamic picture and a more quantitative description of the timescale and amplitude of fluctuations in atomic coordinates than is obtainable from the individual methods alone. Order parameters (S2) were calculated from single-conformer and multiconformer models fitted to room temperature and cryogenic X-ray diffraction data for dihydrofolate reductase. Backbone and side-chain order parameters derived from NMR relaxation experiments are in excellent agreement with those calculated from the room-temperature single-conformer and multiconformer models, showing that the picosecond timescale motions observed in solution occur also in the crystalline state. These motions are quenched in the crystal at cryogenic temperatures. The combination of NMR and X-ray crystallography in iterative refinement promises to provide an atomic resolution description of the alternate conformational substates that are sampled through picosecond to nanosecond timescale fluctuations of the protein structure. The method also provides insights into the structural heterogeneity of nonmethyl side chains, aromatic residues, and ligands, which are less commonly analyzed by NMR relaxation measurements. PMID:24474795

High-resolution proxies for wood density variations in Terminalia superba

PubMed Central

De Ridder, Maaike; Van den Bulcke, Jan; Vansteenkiste, Dries; Van Loo, Denis; Dierick, Manuel; Masschaele, Bert; De Witte, Yoni; Mannes, David; Lehmann, Eberhard; Beeckman, Hans; Van Hoorebeke, Luc; Van Acker, Joris

2011-01-01

Background and Aims Density is a crucial variable in forest and wood science and is evaluated by a multitude of methods. Direct gravimetric methods are mostly destructive and time-consuming. Therefore, faster and semi- to non-destructive indirect methods have been developed. Methods Profiles of wood density variations with a resolution of approx. 50 µm were derived from one-dimensional resistance drillings, two-dimensional neutron scans, and three-dimensional neutron and X-ray scans. All methods were applied on Terminalia superba Engl. & Diels, an African pioneer species which sometimes exhibits a brown heart (limba noir). Key Results The use of X-ray tomography combined with a reference material permitted direct estimates of wood density. These X-ray-derived densities overestimated gravimetrically determined densities non-significantly and showed high correlation (linear regression, R2 = 0·995). When comparing X-ray densities with the attenuation coefficients of neutron scans and the amplitude of drilling resistance, a significant linear relation was found with the neutron attenuation coefficient (R2 = 0·986) yet a weak relation with drilling resistance (R2 = 0·243). When density patterns are compared, all three methods are capable of revealing the same trends. Differences are mainly due to the orientation of tree rings and the different characteristics of the indirect methods. Conclusions High-resolution X-ray computed tomography is a promising technique for research on wood cores and will be explored further on other temperate and tropical species. Further study on limba noir is necessary to reveal the causes of density variations and to determine how resistance drillings can be further refined. PMID:21131386

Synthesis, crystal structure, vibrational spectroscopy and photoluminescence of new hybrid compound containing chlorate anions of stanate (II)

NASA Astrophysics Data System (ADS)

Lassoued, Mohamed Saber; Abdelbaky, Mohammed S. M.; Lassoued, Abdelmajid; Meroño, Rafael Mendoza; Gadri, Abdellatif; Ammar, Salah; Ben Salah, Abdelhamid; García-Granda, Santiago

2017-08-01

The present work aimed at studying a new organic-inorganic bis (4-amino quinolinium) hexachloro stanate (II) dihydrate compound. It was prepared and characterized by single crystal X-ray diffraction, X-ray powder, Hirshfeld surface, Spectroscopy measurement, thermal study and photoluminescence properties. It was found to crystallize in the monoclinic system (P21/c space group) with the following lattice parameters: a = 7.2558(6) Å, b = 13.4876(5) Å, c = 17.2107(13) Å, β = 102.028 (12)°. Its crystal structure was determined and refined down to an R value of 0.06 and a wR value of 0.087. The structure consisted of two different alternating organic-inorganic layers. The crystal packing was stabilized by Nsbnd H⋯Cl and Osbnd H⋯Cl hydrogen bonds and π-π interactions. Hirshfeld surface analysis was used to investigate intermolecular interactions, as well 2D finger plots were conducted to reveal the contribution of these interactions in the crystal structure quantitatively. The X-ray powder is in agreement with the X-ray structure. Scanning electronic microscopy (SEM) was carried out. Furthermore, the room temperature Infra Red (IR) spectrum of the title compound was analyzed on the basis of data found in the literature. Solid state 13C NMR spectrum shows ten signals, confirming the solid state structure determined by X-ray diffraction. Thermal analysis shows two anomalies at 380 and 610 °C. The optical properties of the crystal were studied using optical absorption UV-visible and photoluminescence (PL) spectroscopy, which were investigated at room temperature.

Miniature x-ray source

DOEpatents

Trebes, James E.; Stone, Gary F.; Bell, Perry M.; Robinson, Ronald B.; Chornenky, Victor I.

2002-01-01

A miniature x-ray source capable of producing broad spectrum x-ray emission over a wide range of x-ray energies. The miniature x-ray source comprises a compact vacuum tube assembly containing a cathode, an anode, a high voltage feedthru for delivering high voltage to the anode, a getter for maintaining high vacuum, a connection for an initial vacuum pump down and crimp-off, and a high voltage connection for attaching a compact high voltage cable to the high voltage feedthru. At least a portion of the vacuum tube wall is highly x-ray transparent and made, for example, from boron nitride. The compact size and potential for remote operation allows the x-ray source, for example, to be placed adjacent to a material sample undergoing analysis or in proximity to the region to be treated for medical applications.

Thin-film-based scintillators for hard x-ray microimaging detectors: the ScinTAX Project

NASA Astrophysics Data System (ADS)

Rack, A.; Cecilia, A.; Douissard, P.-A.; Dupré, K.; Wesemann, V.; Baumbach, T.; Couchaud, M.; Rochet, X.; Riesemeier, H.; Radtke, M.; Martin, T.

2014-09-01

The project ScinTAX developed novel thin scintillating films for the application in high performance X-ray imaging and subsequent introduced new X-ray detectors to the market. To achieve this aim lutetium orthosilicate (LSO) scintillators doped with different activators were grown successfully by liquid phase epitaxy. The high density of LSO (7.4 g/cm3), the effective atomic number (65.2) and the high light yield make this scintillator highly applicable for indirect X-ray detection in which the ionizing radiation is converted into visible light and then registered by a digital detector. A modular indirect detection system has been developed to fully exploit the potential of this thin film scintillator for radiographic and tomographic imaging. The system is compatible for high-resolution imaging with moderate dose as well as adaptable to intense high-dose applications where radiation hard microimaging detectors are required. This proceedings article shall review the achieved performances and technical details on this high-resolution detector system which is now available. A selected example application demonstrates the great potential of the optimized detector system for hard X-ray microimaging, i.e. either to improve image contrast due to the availability of efficient thin crystal films or to reduce the dose to the sample.

Novel Applications of Rapid Prototyping in Gamma-ray and X-ray Imaging

PubMed Central

Miller, Brian W.; Moore, Jared W.; Gehm, Michael E.; Furenlid, Lars R.; Barrett, Harrison H.

2010-01-01

Advances in 3D rapid-prototyping printers, 3D modeling software, and casting techniques allow for the fabrication of cost-effective, custom components in gamma-ray and x-ray imaging systems. Applications extend to new fabrication methods for custom collimators, pinholes, calibration and resolution phantoms, mounting and shielding components, and imaging apertures. Details of the fabrication process for these components are presented, specifically the 3D printing process, cold casting with a tungsten epoxy, and lost-wax casting in platinum. PMID:22984341

An X-ray fluorescence spectrometer and its applications in materials studies

NASA Technical Reports Server (NTRS)

Singh, J. J.; Han, K. S.

1977-01-01

An X-ray fluorescence system based on a Co(57) gamma-ray source has been developed. The system was used to calculate the atomic percentages of iron implanted in titanium targets. Measured intensities of Fe (k-alpha + k-beta) and Ti (k-alpha + k-beta) X-rays from the Fe-Ti targets are in good agreement with the calculated values based on photoelectric cross sections of Ti and Fe for the Co(57) gamma rays.