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Sample records for electron microscopy x-ray

  1. X-ray and electron microscopy of actinide materials.

    PubMed

    Moore, Kevin T

    2010-06-01

    Actinide materials demonstrate a wide variety of interesting physical properties in both bulk and nanoscale form. To better understand these materials, a broad array of microscopy techniques have been employed, including transmission electron microscopy (TEM), electron energy-loss spectroscopy (EELS), energy dispersive X-ray spectroscopy (EDXS), high-angle annular dark-field imaging (HAADF), scanning electron microscopy (SEM), wavelength dispersive X-ray spectroscopy (WDXS), electron back scattered diffraction (EBSD), scanning tunneling microscopy (STM), atomic force microscopy (AFM), and scanning transmission X-ray microscopy (STXM). Here these techniques will be reviewed, highlighting advances made in the physics, materials science, chemistry, and biology of actinide materials through microscopy. Construction of a spin-polarized TEM will be discussed, considering its potential for examining the nanoscale magnetic structure of actinides as well as broader materials and devices, such as those for computational magnetic memory. Copyright 2009 Elsevier Ltd. All rights reserved.

  2. Soft X-ray contact microscopy and transmission electron microscopy: Comparative study of biological samples

    NASA Astrophysics Data System (ADS)

    Limongi, T.; Palladino, L.; Bernieri, E.; Tomassetti, G.; Reale, L.; Flora, F.; Cesare, P.; Ercole, C.; Aimola, P.; Ragnelli, A. M.

    2003-03-01

    Isolated cellular organelles (mitochondria, chloroplasts) and cultured bacteria were analysed both by soft X-ray contact microscopy (SXCM), and by transmission electron microscopy (TEM) after negative staining. For each sample, a comparison was performed between images obtained with either technique, with the aim of facilitating the interpretation of SXCM images. The validity and the limits of this comparative approach are discussed.

  3. Bulk sensitive hard x-ray photoemission electron microscopy

    SciTech Connect

    Patt, M. Wiemann, C.; Weber, N.; Escher, M.; Merkel, M.; Gloskovskii, A.; Drube, W.; Schneider, C. M.

    2014-11-15

    Hard x-ray photoelectron spectroscopy (HAXPES) has now matured into a well-established technique as a bulk sensitive probe of the electronic structure due to the larger escape depth of the highly energetic electrons. In order to enable HAXPES studies with high lateral resolution, we have set up a dedicated energy-filtered hard x-ray photoemission electron microscope (HAXPEEM) working with electron kinetic energies up to 10 keV. It is based on the NanoESCA design and also preserves the performance of the instrument in the low and medium energy range. In this way, spectromicroscopy can be performed from threshold to hard x-ray photoemission. The high potential of the HAXPEEM approach for the investigation of buried layers and structures has been shown already on a layered and structured SrTiO{sub 3} sample. Here, we present results of experiments with test structures to elaborate the imaging and spectroscopic performance of the instrument and show the capabilities of the method to image bulk properties. Additionally, we introduce a method to determine the effective attenuation length of photoelectrons in a direct photoemission experiment.

  4. Scanning electron microscopy and electron probe X-ray microanalysis (SEM-EPMA) of pink teeth

    SciTech Connect

    Ikeda, N.; Watanabe, G.; Harada, A.; Suzuki, T.

    1988-11-01

    Samples of postmortem pink teeth were investigated by scanning electron microscopy and electron probe X-ray microanalysis. Fracture surfaces of the dentin in pink teeth were noticeably rough and revealed many more smaller dentinal tubules than those of the control white teeth. Electron probe X-ray microanalysis showed that the pink teeth contained iron which seemed to be derived from blood hemoglobin. The present study confirms that under the same circumstance red coloration of teeth may occur more easily in the teeth in which the dentin is less compact and contains more dentinal tubules.

  5. X-ray absorption in pillar shaped transmission electron microscopy specimens.

    PubMed

    Bender, H; Seidel, F; Favia, P; Richard, O; Vandervorst, W

    2017-03-07

    The dependence of the X-ray absorption on the position in a pillar shaped transmission electron microscopy specimen is modeled for X-ray analysis with single and multiple detector configurations and for different pillar orientations relative to the detectors. Universal curves, applicable to any pillar diameter, are derived for the relative intensities between weak and medium or strongly absorbed X-ray emission. For the configuration as used in 360° X-ray tomography, the absorption correction for weak and medium absorbed X-rays is shown to be nearly constant along the pillar diameter. Absorption effects in pillars are about a factor 3 less important than in planar specimens with thickness equal to the pillar diameter. A practical approach for the absorption correction in pillar shaped samples is proposed and its limitations discussed. The modeled absorption dependences are verified experimentally for pillars with HfO2 and SiGe stacks.

  6. X-ray diffraction and scanning electron microscopy of galvannealed coatings on steel.

    PubMed

    Schmid, P; Uran, K; Macherey, F; Ebert, M; Ullrich, H-J; Sommer, D; Friedel, F

    2009-04-01

    The formation of Fe-Zn intermetallic compounds, as relevant in the commercial product galvannealed steel sheet, was investigated by scanning electron microscopy and different methods of X-ray diffraction. A scanning electron microscope with high resolution was applied to investigate the layers of the galvannealed coating and its topography. Grazing incidence X-ray diffraction (GID) was preferred over conventional Bragg-Brentano geometry for analysing thin crystalline layers because of its lower incidence angle alpha and its lower depth of information. Furthermore, in situ experiments at an environmental scanning electron microscope (ESEM) with an internal heating plate and at an X-ray diffractometer equipped with a high-temperature chamber were carried out. Thus, it was possible to investigate the phase evolution during heat treatment by X-ray diffraction and to display the growth of the zeta crystals in the ESEM.

  7. Correlative electron and X-ray microscopy: probing chemistry and bonding with high spatial resolution.

    PubMed

    Goode, Angela E; Porter, Alexandra E; Ryan, Mary P; McComb, David W

    2015-02-07

    Two powerful and complementary techniques for chemical characterisation of nanoscale systems are electron energy-loss spectroscopy in the scanning transmission electron microscope, and X-ray absorption spectroscopy in the scanning transmission X-ray microscope. A correlative approach to spectro-microscopy may not only bridge the gaps in spatial and spectral resolution which exist between the two instruments, but also offer unique opportunities for nanoscale characterisation. This review will discuss the similarities of the two spectroscopy techniques and the state of the art for each microscope. Case studies have been selected to illustrate the benefits and limitations of correlative electron and X-ray microscopy techniques. In situ techniques and radiation damage are also discussed.

  8. Structural states of myelin observed by x-ray diffraction and freeze- fracture electron microscopy

    PubMed Central

    1979-01-01

    Coordinated freeze-fracture electron microscopy and x-ray diffraction were used to visualize the morphological relation between compacted and native period membrane arrays in myelinated nerves treated with dimethylsulfoxide (DMSO). Comparison of x-ray diffraction at room temperature and at low temperature was used as a critical measure of the extent of structural preservation. Our x-ray diffraction patterns show that in the presence of cryoprotective agents, it is possible to preserve with only small changes the myelin structure which exists at room temperature. These changes include a slight increase in packing disorder of the membrane, a small, negative thermal expansion of the membrane unit, and some reorganization in the cytoplasmic half of the bilayer. The freeze-fracture electron microscopy clearly demonstrates continuity of compact and native period phases in DMSO-treated myelin. Finally, the use of freezing to trap the transient, intermediate structure during a structural transition in glycerol is demonstrated. PMID:479295

  9. Combining X-ray and electron-microscopy data to solve crystal structures

    SciTech Connect

    Navaza, Jorge

    2008-01-01

    Overview and examples of combined use of X-ray and electron-microscopy data. Low-resolution electron-microscopy reconstructions can be used as search models in molecular replacement or may be combined with existing monomeric structures in order to produce multimeric models suitable for molecular replacement. The technique is described in the case of viral and subviral particles as well as in the case of oligomeric proteins.

  10. Investigation of nanoparticulate silicon as printed layers using scanning electron microscopy, transmission electron microscopy, X-ray absorption spectroscopy and X-ray photoelectron spectroscopy

    DOE PAGES

    Unuigbe, David M.; Harting, Margit; Jonah, Emmanuel O.; ...

    2017-08-21

    The presence of native oxide on the surface of silicon nanoparticles is known to inhibit charge transport on the surfaces. Scanning electron microscopy (SEM) studies reveal that the particles in the printed silicon network have a wide range of sizes and shapes. High-resolution transmission electron microscopy reveals that the particle surfaces have mainly the (111)- and (100)-oriented planes which stabilizes against further oxidation of the particles. X-ray absorption spectroscopy (XANES) and X-ray photoelectron spectroscopy (XPS) measurements at the O 1s-edge have been utilized to study the oxidation and local atomic structure of printed layers of silicon nanoparticles which were milledmore » for different times. XANES results reveal the presence of the +4 (SiO2) oxidation state which tends towards the +2 (SiO) state for higher milling times. Si 2pXPS results indicate that the surfaces of the silicon nanoparticles in the printed layers are only partially oxidized and that all three sub-oxide, +1 (Si2O), +2 (SiO) and +3 (Si2O3), states are present. The analysis of the change in the sub-oxide peaks of the silicon nanoparticles shows the dominance of the +4 state only for lower milling times.« less

  11. X-ray structure determination using low-resolution electron microscopy maps for molecular replacement

    SciTech Connect

    Jackson, Ryan N.; McCoy, Airlie J.; Terwilliger, Thomas C.; Read, Randy J.; Wiedenheft, Blake

    2015-07-30

    Structures of multi-subunit macromolecular machines are primarily determined by either electron microscopy (EM) or X-ray crystallography. In many cases, a structure for a complex can be obtained at low resolution (at a coarse level of detail) with EM and at higher resolution (with finer detail) by X-ray crystallography. The integration of these two structural techniques is becoming increasingly important for generating atomic models of macromolecular complexes. A low-resolution EM image can be a powerful tool for obtaining the "phase" information that is missing from an X-ray crystallography experiment, however integration of EM and X-ray diffraction data has been technically challenging. Here we show a step-by-step protocol that explains how low-resolution EM maps can be placed in the crystallographic unit cell by molecular replacement, and how initial phases computed from the placed EM density are extended to high resolution by averaging maps over non-crystallographic symmetry. As the resolution gap between EM and Xray crystallography continues to narrow, the use of EM maps to help with X-ray crystal structure determination, as described in this protocol, will become increasingly effective.

  12. X-ray structure determination using low-resolution electron microscopy maps for molecular replacement

    DOE PAGES

    Jackson, Ryan N.; McCoy, Airlie J.; Terwilliger, Thomas C.; ...

    2015-07-30

    Structures of multi-subunit macromolecular machines are primarily determined by either electron microscopy (EM) or X-ray crystallography. In many cases, a structure for a complex can be obtained at low resolution (at a coarse level of detail) with EM and at higher resolution (with finer detail) by X-ray crystallography. The integration of these two structural techniques is becoming increasingly important for generating atomic models of macromolecular complexes. A low-resolution EM image can be a powerful tool for obtaining the "phase" information that is missing from an X-ray crystallography experiment, however integration of EM and X-ray diffraction data has been technically challenging.more » Here we show a step-by-step protocol that explains how low-resolution EM maps can be placed in the crystallographic unit cell by molecular replacement, and how initial phases computed from the placed EM density are extended to high resolution by averaging maps over non-crystallographic symmetry. As the resolution gap between EM and Xray crystallography continues to narrow, the use of EM maps to help with X-ray crystal structure determination, as described in this protocol, will become increasingly effective.« less

  13. Microscale reconstruction of biogeochemical substrates using multimode X-ray tomography and scanning electron microscopy

    NASA Astrophysics Data System (ADS)

    Miller, M.; Miller, E.; Liu, J.; Lund, R. M.; McKinley, J. P.

    2012-12-01

    X-ray computed tomography (CT), scanning electron microscopy (SEM), electron microprobe analysis (EMP), and computational image analysis are mature technologies used in many disciplines. Cross-discipline combination of these imaging and image-analysis technologies is the focus of this research, which uses laboratory and light-source resources in an iterative approach. The objective is to produce images across length scales, taking advantage of instrumentation that is optimized for each scale, and to unify them into a single compositional reconstruction. Initially, CT images will be collected using both x-ray absorption and differential phase contrast modes. The imaged sample will then be physically sectioned and the exposed surfaces imaged and characterized via SEM/EMP. The voxel slice corresponding to the physical sample surface will be isolated computationally, and the volumetric data will be combined with two-dimensional SEM images along CT image planes. This registration step will take advantage of the similarity between the X-ray absorption (CT) and backscattered electron (SEM) coefficients (both proportional to average atomic number in the interrogated volume) as well as the images' mutual information. Elemental and solid-phase distributions on the exposed surfaces, co-registered with SEM images, will be mapped using EMP. The solid-phase distribution will be propagated into three-dimensional space using computational methods relying on the estimation of compositional distributions derived from the CT data. If necessary, solid-phase and pore-space boundaries will be resolved using X-ray differential phase contrast tomography, x-ray fluorescence tomography, and absorption-edge microtomography at a light-source facility. Computational methods will be developed to register and model images collected over varying scales and data types. Image resolution, physically and dynamically, is qualitatively different for the electron microscopy and CT methodologies. Routine

  14. Microscale reconstruction of biogeochemical substrates using combined X-ray tomography and scanning electron microscopy

    NASA Astrophysics Data System (ADS)

    Miller, M.; McKinley, J. P.; Miller, E. A.; Liu, J.

    2011-12-01

    X-ray tomography (CT), scanning electron microscopy (SEM), electron microprobe analysis (EMP), and computational image analysis are mature technologies used in many disciplines. Cross-discipline combination of these imaging and image-analysis technologies is the focus of this research, which uses laboratory and light-source resources in an iterative approach. The objective is to produce images across length scales, taking advantage of instrumentation that is optimized for each scale, and to unify them into a single compositional reconstruction. Initially, a nominal CT image will be collected. The imaged sample will then be physically sectioned and the exposed surfaces imaged and characterized via SEM/EMP. The voxel slice corresponding to the physical sample surface will be isolated computationally, and the volumetric data will be combined with two-dimensional SEM images along CT image planes. This registration step will take advantage of the similarity between the X-ray absorption (CT) and backscattered electron (SEM) coefficients (both proportional to average atomic number in the interrogated volume). Elemental and solid-phase distributions on the exposed surfaces, pre-registered with SEM images, will be mapped using EMP. The solid-phase distribution will be propagated into three-dimensional space using computational methods relying on the estimation of compositional distributions derived from CT data. If necessary, solid-phase and pore-space boundaries will be resolved using X-ray phase-contrast imaging, x-ray fluorescence tomography, and absorption-edge microtomography at a light-source facility. Computational methods will be developed to register and model images collected over varying scales and data types. Image resolution, physically and dynamically, is qualitatively different for the electron microscopy and CT methodologies. Routine CT images are resolved at 10-20 μm, while SEM images are resolved at 10-20 nm; grayscale values vary according to collection

  15. Transmission electron microscopy and x-ray diffraction studies of the detonation soot of high explosives

    NASA Astrophysics Data System (ADS)

    Kashkarov, A. O.; Pruuel, E. R.; Ten, K. A.; Rubtsov, I. A.; Gerasimov, E. Yu; Zubkov, P. I.

    2016-11-01

    This paper presents the results of electron microscopy and x-ray diffraction studies of the recovered carbonaceous residue (soot) from the detonation of some high explosives: TNT, a mixture of TNT and RDX (50/50), benzotrifuroxane, and triaminotrinitrobenzene. The use of the same experimental setup allowed a qualitative and quantitative comparison of the detonation products formed under similar conditions. The results clearly show differences in the morphology of graphite-like and diamond inclusions and in the quantitative content of nanodiamonds for the explosives used in this study.

  16. Sialolith characterization by scanning electron microscopy and X-ray photoelectron spectroscopy.

    PubMed

    Giray, C Bahadir; Dogan, Meral; Akalin, Ayse; Baltrusaitis, Jonas; Chan, Daniel C N; Skinner, H Catherine W; Dogan, A Umran

    2007-01-01

    The objective of this study has been to characterize sialolith, a calcium phosphate deposit that develops in the human oral cavity, by high-resolution field emission scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The morphological and chemical data obtained helped in the determination of their formation mechanism in salivary glands. Sialoliths in the submandibular salivary glands may arise secondary to sialodenitis, but not via a luminal organic nidus. We believe this is the first study that characterizes a sialolith by XPS.

  17. Silica granuloma: scanning electron microscopy and energy dispersive X-ray microanalysis.

    PubMed

    Chun, S I; Cho, S W

    1991-02-01

    A 46-year-old woman had 1-month-old erythematous papules on the left elbow and both knees where acupuncture with gold needles had been performed twenty years earlier. She also had a 2-month-old pruritic scar lesion on the nape. Histopathologic findings showed sarcoidal granulomas. The presence of silica components in the granulomas was confirmed by scanning electron microscopy (SEM) of the lesion on the nape and energy dispersive X-ray microanalysis (EDXA) of the lesions on the nape and the left elbow. We suggest that acupuncture with gold needles may be one cause of silica granuloma.

  18. Adenovirus Structure as Revealed by X-Ray Crystallography, Electron Microscopy, and Difference Imaging

    NASA Astrophysics Data System (ADS)

    Stewart, Phoebe L.; Burnett, Roger M.

    1993-03-01

    The three-dimensional structure of human type 2 adenovirus was studied by combining X-ray crystallography and electron microscopy in a novel way. The 2.9 Å crystal structure of the major capsid protein, hexon, was positioned into a three-dimensional image reconstruction of the intact virus that was derived from cryo-electron micrographs. A three-dimensional difference map was generated by subtracting 240 copies of the crystallographic hexon from the density of the intact virus. This map revealed several minor structural proteins acting as “cement” to stabilize the assembly. The current state of structural knowledge concerning the location of the polypeptide components and the viral DNA is presented.

  19. Clinical applications of scanning electron microscopy and X-ray microanalysis in dermatology

    SciTech Connect

    Forslind, B.

    1984-01-01

    Scanning electron microscopy is frequently applied to dermatological problems, as is evident from a review of the recent literature. In this paper, preparation methods and new techniques allowing experimental studies on the integumentary system are emphasized. Quantitative analysis in the electron microscope by use of energy-dispersive X-ray microanalysis (EDX) has become an important accessory technique. EDX can, for instance, be used to study problems involving physiological changes induced in skin by agents causing contact reactions. Recently, it has been shown that treatment with DNCB, chromate and nickel causes changes in elemental distribution in guinea-pig skin. In addition, elemental uptake in the integumentary system and in pathological inclusions in skin can be analyzed.

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

    PubMed

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

    2005-12-01

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

  1. An x-ray diffraction and TEM (transmission electron microscopy) study of subsurface recovery during abrasion

    SciTech Connect

    Rao, C.M.; Kosel, T.H.

    1985-01-01

    The subsurface dislocation structures and the extent of dynamic recovery and recrystallization in pure metals subjected to low-stress abrasion have been examined. Pure copper and aluminum were chosen to provide a range of melting and therefore recrystallization temperatures. The materials were strain annealed before abrasion in order to produce extremely large initial grain sizes. Back-reflection x-ray pinhole photographs of the original specimens produced single crystal Laue patterns, whereas the abraded specimens produced Debye rings. In the case of aluminum the Debye rings contained distinct individual spots, whereas the copper produced smooth, continuous rings. Transmission electron microscopy (TEM) was used to examine subsurface sections parallel to the war tracks to provide more direct evidence of the subsurface microstructural changes. In all cases, at greater depths below the worn surface, the materials showed dislocation cells typical of a high degree of room temperature deformation, with the degree of deformation decreasing with depth. Closer to the surface, the copper exhibited a fine, high-misorientations subgrain structure which is believed to be responsible for the continuous Debye rings seen in the x-ray pattern. In the case of aluminum, there appeared to be a mixture of fine subgrains and larger dynamically recrystallized grains which are believed to have produced the spotty Debye rings. 29 refs., 14 figs.

  2. Scanning electron microscopy, X-ray microanalysis and immunohistochemistry on worn soft contact lenses

    SciTech Connect

    Versura, P.; Maltarello, M.C.; Roomans, G.M.; Caramazza, R.; Laschi, R.

    1988-03-01

    The deposits accumulated on the surfaces of soft contact lenses are a cause of problems for the wearer of these lenses, as the deposits are never completely removed by the available washing solutions. Therefore it appears of interest to investigate the composition of these deposits. In this paper we review the major findings in the literature and, in addition, present our personal experience. We have studied new, continuously and daily worn soft contact lenses by scanning electron microscopy (SEM), X-ray microanalysis and immunohistochemistry. We have carefully evaluated preparative methods, and we can conclude that SEM and X-ray microanalysis are best carried out on unfixed, air-dried lenses. The deposits present consist mainly of mucus, especially on the tarsal side of the lenses. Chloride and potassium, coming from the tear fluid, as well as sulfur, derived from proteins, were found. Calcium was very rarely detected. IgG, IgA, IgE and C3c complement fractions were found only on the outer surfaces and not within the lens. We believe that the best characterization of the deposits is achieved by means of correlative techniques on the same lens. In fact, this approach integrates morphology and composition.

  3. X-ray photoemission electron microscopy for the study of semiconductor materials

    SciTech Connect

    Anders, S.; Stammler, T.; Padmore, H.; Terminello, L.J.; Jankowski, A.F.; Stohr, J.; Diaz, J.; Cossy-Gantner, A.

    1998-03-01

    Photoemission Electron Microscopy (PEEM) using X-rays is a novel combination of two established materials analysis techniques--PEEM using UV light, and Near Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy. This combination allows the study of elemental composition and bonding structure of the sample by NEXAFS spectroscopy with a high spatial resolution given by the microscope. A simple, two lens, 10 kV operation voltage PEEM has been used at the Stanford Synchrotron Radiation Laboratory and at the Advanced Light Source (ALS) in Berkeley to study various problems including materials of interest for the semiconductor industry. In the present paper the authors give a short overview over the method and the instrument which was used, and describe in detail a number of applications. These applications include the study of the different phases of titanium disilicide, various phases of boron nitride, and the analysis of small particles. A brief outlook is given on possible new fields of application of the PEEM technique, and the development of new PEEM instruments.

  4. Biomedical and agricultural applications of energy dispersive X-ray spectroscopy in electron microscopy.

    PubMed

    Wyroba, Elżbieta; Suski, Szymon; Miller, Karolina; Bartosiewicz, Rafał

    2015-09-01

    Energy dispersive X-ray spectroscopy (EDS) in electron microscopy has been widely used in many research areas since it provides precise information on the chemical composition of subcellular structures that may be correlated with their high resolution images. In EDS the characteristic X-rays typical of each element are analyzed and the new detectors - an example of which we describe - allow for setting precisely the area of measurements and acquiring signals as a point analysis, as a linescan or in the image format of the desired area. Mapping of the elements requires stringent methods of sample preparation to prevent redistribution/loss of the elements as well as elimination of the risk of overlapping spectra. Both qualitative and quantitative analyses may be performed at a low probe current suitable for thin biological samples. Descriptions of preparation techniques, drawbacks and precautions necessary to obtain reliable results are provided, including data on standards, effects of specimen roughness and quantification. Data on EPMA application in different fields of biomedical and agricultural studies are reviewed. In this review we refer to recent EDS/EPMA applications in medical diagnostics, studies on air pollution and agrochemicals as well as on plant models used to monitor the environment.

  5. X-Ray Diffraction and Electron Microscopy Study of Cr/Sb Multilayered Films

    NASA Astrophysics Data System (ADS)

    Dohnomae, Hitoshi

    1994-03-01

    Structures of [Cr(2 Å)/Sb(50 Å)] n multilayered films have been investigated by X-ray diffraction and transmission electron microscopy (TEM) of cross sections. When the substrate temperature (T s) was 90° C, an epitaxial structure with a coherent stacking of Sb and compound (CrSb) layers was formed by the interfacial reaction. On the other hand, at T s=-50° C, a non-epitaxial structure composed of crystalline Sb layers and amorphous Cr metal layers was obtained. Interfaces of multilayers observed by TEM are very flat for both samples. The structures of very thin Cr layers depend on the reactivity of interfaces and greatly affect on the orientations of Sb layers.

  6. Applications of scanning electron microscopy and X-ray microanalysis in inner ear pathology

    SciTech Connect

    Anniko, M.; Lim, D.J.; Sobin, A.; Wroblewski, R.

    1985-01-01

    Surface pathology of inner ear structures so far described in detail concern cochlear and vestibular hair cells and the stria vascularis. In man, surgical intervention into the inner ear is very uncommon and when performed is in general with the primary objective of destroying the diseased peripheral end organs. The vast majority of inner ear tissue available for use with scanning electron microscopy (SEM) is therefore obtained from animals. The present paper reviews the progression of surface pathology caused by aminoglycoside antibiotics, acoustic overstimulation and in a guinea pig strain with genetic inner ear disease. The primary site of onset of surface pathology differs, depending on the underlying cause. Advanced surface pathology shows a similar type of morphological degeneration independent of cause. The combination of SEM and energy dispersive X-ray microanalysis (XRMA) of inner ear pathology has as yet been reported in only three studies, all concerning inner ear fluids or otoconia.

  7. Small angle x-ray scattering and electron microscopy of nanoparticles formed in an electrical arc

    NASA Astrophysics Data System (ADS)

    Carvou, E.; Garrec, J. L. Le; Pérez, J.; Praquin, J.; Djeddi, M.; Mitchell, J. B. A.

    2013-03-01

    Small Angle X-ray Scattering has been used to characterize nanoparticles generated by electrical arcing between metallic (AgSnO2) electrodes. The particles are found to have diameters between 30 and 40 nm and display smooth surfaces suggesting that they are either in liquid form or have solidified from the liquid state. Particles collected around the electrodes were analyzed by Transmission Electron Microscopy and were seen to be much larger than those seen in the SAXS measurement, to be spherical in form and composed of silver metal with irregular tin oxide particles deposited on their surface. Mixed metal nanoparticles can have important practical applications and the use of mixed sintered electrodes may be a direct method for their production.

  8. Scanning electron microscopy, x-ray diffraction, and electron microprobe analysis of calcific deposits on intrauterine contraceptive devices

    SciTech Connect

    Khan, S.R.; Wilkinson, E.J.

    1985-07-01

    Deposits found on intrauterine contraceptive devices (IUDs) were studied by scanning electron microscopy, x-ray diffraction, and energy dispersive x-ray microanalysis. All seven devices, including five plastic and two copper IUDs, were coated with a crust containing cellular, acellular, and fibrillar material. The cellular material was composed of erythrocytes, leukocytes, cells of epithelial origin, sperm, and bacteria. Some of the bacteria were filamentous, with acute-angle branching. The fibrillar material appeared to be fibrin. Most of the acellular material was amorphous; calcite was identified by x-ray diffraction, and x-ray microanalysis showed only calcium. Some of the acellular material, particularly that on the IUD side of the crust, was organized in spherulitic crystals and was identified as calcium phosphate by x-ray microanalysis. The crust was joined to the IUD surface by a layer of fibrillar and amorphous material. It is suggested that the initial event in the formation of calcific deposits on IUD surfaces is the deposition of an amorphous and fibrillar layer. Various types of cells present in the endometrial environment adhere to this layer and then calcify. Thus, the deposition of calcific material on the IUDs is a calcification phenomenon, not unlike the formation of plaque on teeth.

  9. X-ray absorption spectroscopy by full-field X-ray microscopy of a thin graphite flake: Imaging and electronic structure via the carbon K-edge

    PubMed Central

    Hitchock, Adam P; Ke, Xiaoxing; Van Tendeloo, Gustaaf; Ewels, Chris P; Guttmann, Peter

    2012-01-01

    Summary We demonstrate that near-edge X-ray-absorption fine-structure spectra combined with full-field transmission X-ray microscopy can be used to study the electronic structure of graphite flakes consisting of a few graphene layers. The flake was produced by exfoliation using sodium cholate and then isolated by means of density-gradient ultracentrifugation. An image sequence around the carbon K-edge, analyzed by using reference spectra for the in-plane and out-of-plane regions of the sample, is used to map and spectrally characterize the flat and folded regions of the flake. Additional spectral features in both π and σ regions are observed, which may be related to the presence of topological defects. Doping by metal impurities that were present in the original exfoliated graphite is indicated by the presence of a pre-edge signal at 284.2 eV. PMID:23016137

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

    PubMed

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

    2015-10-01

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

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

    PubMed

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

    2014-09-01

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

  12. Comparison of SOFC Cathode Microstructure Quantified using X-ray Nanotomography and Focused Ion Beam - Scanning Electron Microscopy

    SciTech Connect

    Nelson, George J.; Harris, William H.; Lombardo, Jeffrey J.; Izzo, Jr., John R.; Chiu, W. K. S.; Tanasini, Pietro; Cantoni, Marco; Van herle, Jan; Comninellis, Christos; Andrews, Joy C.; Liu, Yijin; Pianetta, Piero; Chu, Yong

    2011-03-24

    X-ray nanotomography and focused ion beam scanning electron microscopy (FIB-SEM) have been applied to investigate the complex 3D microstructure of solid oxide fuel cell (SOFC) electrodes at spatial resolutions of 45 nm and below. The application of near edge differential absorption for x-ray nanotomography and energy selected backscatter detection for FIB–SEM enable elemental mapping within the microstructure. Using these methods, non-destructive 3D x-ray imaging and FIB–SEM serial sectioning have been applied to compare three-dimensional elemental mapping of the LSM, YSZ, and pore phases in the SOFC cathode microstructure. The microstructural characterization of an SOFC cathode is reported based on these measurements. The results presented demonstrate the viability of x-ray nanotomography as a quantitative characterization technique and provide key insights into the SOFC cathode microstructure.

  13. Comparison of SOFC Cathode Microstructure Quantified using X-ray Nanotomography and Focused Ioni Beam-scanning Electron Microscopy

    SciTech Connect

    G Nelson; W Harris; J Lombardo; J Izzo Jr.; W Chiu; P Tanasini; M Cantoni; J Van herle; C Comninellis; et al.

    2011-12-31

    X-ray nanotomography and focused ion beam scanning electron microscopy (FIB-SEM) have been applied to investigate the complex 3D microstructure of solid oxide fuel cell (SOFC) electrodes at spatial resolutions of 45 nm and below. The application of near edge differential absorption for x-ray nanotomography and energy selected backscatter detection for FIB-SEM enable elemental mapping within the microstructure. Using these methods, non-destructive 3D x-ray imaging and FIB-SEM serial sectioning have been applied to compare three-dimensional elemental mapping of the LSM, YSZ, and pore phases in the SOFC cathode microstructure. The microstructural characterization of an SOFC cathode is reported based on these measurements. The results presented demonstrate the viability of x-ray nanotomography as a quantitative characterization technique and provide key insights into the SOFC cathode microstructure.

  14. Surface characterization of ginger powder examined by X-ray photoelectron spectroscopy and scanning electron microscopy.

    PubMed

    Zhao, Xiaoyan; Ao, Qiang; Du, Fangling; Zhu, Junqing; Liu, Jie

    2010-09-01

    The surface composition of five types of ginger powders with the particle sizes of 300, 149, 74, 37 and 8.34 microm was investigated by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and various types of physical-chemical characteristics regarding material particle size distributions, discoloration and chemical composition. The results show that the color differences are greater for superfine ground ginger than for conventional comminuted ones; the values of crude fibre, neutral detergent fiber (NDF) and acid detergent fiber (ADF) decrease with decreasing ginger particle size. However, no relationship with the surface fat, crude protein, ash and total solids exists. With superfine grinding the XPS O/C ratios of the five ginger powders were similar since the surfaces were not oxidized. Correlations were observed between the XPS N/C ratios and the high resolution XPS N 1s spectra. SEM observations revealed that the surface of ginger powder with a particle size of 300 microm is rougher, while superfine ground powders with particle sizes of 149, 74, 37 and 8.34 microm are similar to each other. This roughness difference between these surfaces correlates with the differences in their O/C ratios and the surface morphology of five ginger powders. Copyright 2010 Elsevier B.V. All rights reserved.

  15. Barriers to Quantitative Electron Probe X-Ray Microanalysis for Low Voltage Scanning Electron Microscopy.

    PubMed

    Newbury, Dale E

    2002-01-01

    Low voltage x-ray microanalysis, defined as being performed with an incident beam energy ≤5 keV, can achieve spatial resolution, laterally and in depth, of 100 nm or less, depending on the exact selection of beam energy and the composition of the target. The shallow depth of beam penetration, with the consequent short path length for x-ray absorption, and the low overvoltage, the ratio of beam energy to the critical ionization energy, both contribute to minimizing the matrix effects in quantitative x-ray microanalysis when the unknown is compared to pure element standards. The low beam energy restricts the energy of the atomic shells that can be excited, forcing the analyst to choose unfamiliar shells/characteristic peaks. The low photon energy shells are subject to low fluorescence yield, so that the peak-to-continuum background is reduced, severely limiting detectability. The limited resolution of semiconductor energy dispersive spectrometry results in frequent peak interference situations and further exacerbates detection limits. Future improvements to the x-ray spectrometry limitations are possible with x-ray optics-augmented wavelength dispersive spectrometry and microcalorimeter energy dispersive spectrometry.

  16. Cadmium toxicity to the cornea of pregnant rats: Electron microscopy and x-ray microanalysis

    SciTech Connect

    Yoshizuka, M.; McCarthy, K.J.; Kaye, G.I.; Fujimoto, S. )

    1990-05-01

    Cadmium toxicity to the cornea of pregnant rats was studied using the electron microscope and x-ray microanalyzer. In in-vivo experiments, severe corneal edema occurred in pregnant dams that received intraperitoneal injections of cadmium sulphate for 4 days during gestation, but not in nonpregnant rats. Prominent swelling of mitochondria and the occurrence of intra- and intercellular vacuoles in the corneal endothelium were observed only in pregnant dams. In in-vitro experiments, electron-dense deposits consisting of cadmium-oxine complexes were preferentially found in swollen mitochondria of the endothelial cells. Cadmium peaks were obtained from these deposits with x-ray microanalysis. These data suggest that the corneal edema observed after administration of cadmium may imply the disturbance of pump function and barrier function of the corneal endothelium due to the primary toxic effects of this metal on mitochondria.

  17. SCANNING ELECTRON MICROSCOPY AND X-RAY DIFFRACTION ANALYSIS OF TANK 18 SAMPLES

    SciTech Connect

    Hay, M.; O'Rourke, P.; Ajo, H.

    2012-03-08

    The F-Area Tank Farm (FTF) Performance Assessment (PA) utilizes waste speciation in the waste release model used in the FTF fate and transport modeling. The waste release modeling associated with the residual plutonium in Tank 18 has been identified as a primary contributor to the Tank 18 dose uncertainty. In order to reduce the uncertainty related to plutonium in Tank 18, a better understanding of the plutonium speciation in the Tank 18 waste (including the oxidation state and stoichiometry) is desired. Savannah River National Laboratory (SRNL) utilized Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD) to analyze Tank 18 samples to provide information on the speciation of plutonium in the waste material. XRD analysis of the Tank 18 samples did not identify any plutonium mineral phases in the samples. These indicates the crystalline mineral phases of plutonium are below the detection limits of the XRD method or that the plutonium phase(s) lack long range order and are present as amorphous or microcrystalline solids. SEM analysis of the Tank 18 samples did locate particles containing plutonium. The plutonium was found as small particles, usually <1 {micro}m but ranging up to several micrometers in diameter, associated with particles of an iron matrix and at low concentration in other elemental matrices. This suggests the plutonium has an affinity for the iron matrix. Qualitatively, the particles of plutonium found in the SEM analysis do not appear to account for all of the plutonium in the sample based on concentrations determined from the chemical analysis of the Tank 18 samples. This suggests that plutonium is also distributed throughout the solids in low concentrations.

  18. Nanopaleomagnetism of meteoritic Fe-Ni studied using X-ray photoemission electron microscopy

    NASA Astrophysics Data System (ADS)

    Bryson, James F. J.; Herrero-Albillos, Julia; Kronast, Florian; Ghidini, Massimo; Redfern, Simon A. T.; van der Laan, Gerrit; Harrison, Richard J.

    2014-06-01

    X-ray photoemission electron microscopy (XPEEM) enables natural remanent magnetisation to be imaged with ˜30 nm resolution across a field of view of 5-20 μm. The method is applied to structural features typical of the Widmanstätten microstructure (kamacite - tetrataenite rim - cloudy zone - plessite) in the Tazewell IIICD iron meteorite. Kamacite lamellae and the tetrataenite rim are multidomain, whereas plessite consists of laths of different phases displaying a range of stable magnetisation directions. The cloudy zone (CZ) displays a complex interlocking domain pattern resulting from nanoscale islands of tetrataenite with easy axes distributed along three possible crystallographic directions. Quantitative analysis of the coarse and intermediate CZ was achieved using a combination of image simulations and histogram profile matching. Remanence information was extracted from individual regions of interest ˜400 nm wide, demonstrating for the first time the capability of XPEEM to perform quantitative paleomagnetic analysis at sub-micron length scales. The three tetrataenite easy axis orientations occur with equal probability in the coarse and intermediate CZ, suggesting that spinodal decomposition in these regions was not strongly influenced by internal interaction fields, and that they are suitable candidates for future paleomagnetic studies. The fine CZ shows a strong dominance of one easy axis. This effect is attributed to island-island exchange interactions that render the fine CZ unsuitable for paleomagnetic study. Variations in the relative strength (proportion of dominant easy axis) and direction (direction of dominant easy axis) of a paleomagnetic field can be resolved from different regions of the CZ using XPEEM, raising the prospect of obtaining a time-resolved measurement of the active dynamo period in meteorites originating from the upper unmelted regions of differentiated asteroids (e.g. chondrites, pallasites, mesosiderites).

  19. Investigation of foreign substances in food using scanning electron microscopy-x-ray microanalysis.

    PubMed

    Charbonneau, J E

    1998-06-01

    Scanning electron microscopy (SEM) and x-ray microanalysis (EDS) were used to conduct forensic investigations on metal and glass foreign objects. SEM-EDS is an excellent method for identifying metal foreign objects in food, such as wire, dental fillings, bone, and metal packaging, based on their element composition. From a determination of the extent of corrosion of a metal foreign object using SEM-EDS, it is sometimes possible to determine whether the material has been processed with the food product. Case histories of processed aluminum, unprocessed nickel-coated steel, and corrosion resistant stainless steel foreign objects are discussed. A potential product-tampering problem involving a hole defect in a paperboard package was resolved using SEM-EDS. Blue fibers found in the hole were found to contain brass particles from a ball point pen rather than a syringe needle. SEM-EDS has been used to determine the elemental composition of glass foreign objects and is able to distinguish between many types of glass including container, electrical, and bakeware. A case history is presented to show that although container glasses cannot, in general, be distinguished from one another using SEM-EDS, they can be distinguished by trace element semiquantitative spectrograghic analysis. SEM-EDS can be used to distinguish glass-like foreign objects from glass. Case histories of struvite crystals found in salmon and cream of tartar crystals found in grape juice are discussed. Fourier transform infrared (FTIR) identified the cream of tartar crystal as calcium tartrate, and this complemented the calcium, carbon, and oxygen components of the compound found using SEM-EDS.

  20. Contrast enhancement of biological nanoporous materials with zinc oxide infiltration for electron and X-ray nanoscale microscopy.

    PubMed

    Ocola, L E; Sampathkumar, V; Kasthuri, N; Winarski, R P

    2017-07-19

    We show that using infiltration of ZnO metal oxide can be useful for high resolution imaging of biological samples in electron and X-ray microscopy. The method is compatible with standard fixation techniques that leave the sample dry, such as finishing with super critical CO2 drying, or simple vacuum drying up to 95 °C. We demonstrate this technique can be applied on tooth and brain tissue samples. We also show that high resolution X-ray tomography can be performed on biological systems using Zn K edge (1s) absorption to enhance internal structures, and obtained the first nanoscale 10 KeV X-ray absorption images of the interior regions of a tooth.

  1. Contrast enhancement of biological nanoporous materials with zinc oxide infiltration for electron and X-ray nanoscale microscopy

    DOE PAGES

    Ocola, L. E.; Sampathkumar, V.; Kasthuri, N.; ...

    2017-07-19

    Here, we show that using infiltration of ZnO metal oxide can be useful for high resolution imaging of biological samples in electron and X-ray microscopy. This method is compatible with standard fixation techniques that leave the sample dry, such as finishing with super critical CO2 drying, or simple vacuum drying at 95°C. We demonstrate this technique can be applied on tooth and brain tissue samples. We also show that high resolution X-ray tomography can be performed on biological systems using Zn K edge (1s) absorption to enhance internal structures, and obtained the first nanoscale 10 KeV X-ray absorption images ofmore » the interior regions of a tooth.« less

  2. Small angle X-ray scattering and transmission electron microscopy study of the Lactobacillus brevis S-layer protein

    NASA Astrophysics Data System (ADS)

    Jääskeläinen, Pentti; Engelhardt, Peter; Hynönen, Ulla; Torkkeli, Mika; Palva, Airi; Serimaa, Ritva

    2010-10-01

    The structure of self-assembly domain containing recombinant truncation mutants of Lactobacillus brevis surface layer protein SlpA in aqueous solution was studied using small-angle X-ray scattering and transmission electron microscopy. The proteins were found out to interact with each other forming stable globular oligomers of about 10 monomers. The maximum diameter of the oligomers varied between 75 Å and 435 Å.

  3. Genetically targeted 3D visualisation of Drosophila neurons under Electron Microscopy and X-Ray Microscopy using miniSOG

    PubMed Central

    Ng, Julian; Browning, Alyssa; Lechner, Lorenz; Terada, Masako; Howard, Gillian; Jefferis, Gregory S. X. E.

    2016-01-01

    Large dimension, high-resolution imaging is important for neural circuit visualisation as neurons have both long- and short-range patterns: from axons and dendrites to the numerous synapses at terminal endings. Electron Microscopy (EM) is the favoured approach for synaptic resolution imaging but how such structures can be segmented from high-density images within large volume datasets remains challenging. Fluorescent probes are widely used to localise synapses, identify cell-types and in tracing studies. The equivalent EM approach would benefit visualising such labelled structures from within sub-cellular, cellular, tissue and neuroanatomical contexts. Here we developed genetically-encoded, electron-dense markers using miniSOG. We demonstrate their ability in 1) labelling cellular sub-compartments of genetically-targeted neurons, 2) generating contrast under different EM modalities, and 3) segmenting labelled structures from EM volumes using computer-assisted strategies. We also tested non-destructive X-ray imaging on whole Drosophila brains to evaluate contrast staining. This enabled us to target specific regions for EM volume acquisition. PMID:27958322

  4. Laboratory-Based Cryogenic Soft X-ray Tomography with Correlative Cryo-Light and Electron Microscopy

    SciTech Connect

    Carlson, David B.; Gelb, Jeff; Palshin, Vadim; Evans, James E.

    2013-02-01

    Here we present a novel laboratory-based cryogenic soft X-ray microscope for whole cell tomography of frozen hydrated samples. We demonstrate the capabilities of this compact cryogenic microscope by visualizing internal sub-cellular structures of Saccharomyces cerevisiae cells. The microscope is shown to achieve better than 50 nm spatial resolution with a Siemens star test sample. For whole biological cells, the microscope can image specimens up to 5 micrometers thick. Structures as small as 90 nm can be detected in tomographic reconstructions at roughly 70 nm spatial resolution following a low cumulative radiation dose of only 7.2 MGy. Furthermore, the design of the specimen chamber utilizes a standard sample support that permits multimodal correlative imaging of the exact same unstained yeast cell via cryo-fluorescence light microscopy, cryo-soft x-ray microscopy and cryo-transmission electron microscopy. This completely laboratory-based cryogenic soft x-ray microscope will therefore enable greater access to three-dimensional ultrastructure determination of biological whole cells without chemical fixation or physical sectioning.

  5. Synchrotron radiation induced x-ray micro analysis: A realistic alternative for electron- and ion beam microscopy

    SciTech Connect

    Janssens, K.; Adams, F. . Dept. of Chemistry); Rivers, M.L.; Jones, K.W. )

    1992-01-01

    Synchrotron Radiation induced X-ray micro Fluorescence analysis ([mu]-SRXRF) is compared with more conventional microanalytical techniques such as Secondary Ion Microscopy (SIMS) and Electron Probe X-ray Microanalysis (EPXMA) for two typical microanalytical applications. SRXRF and EPXMA are employed for the analysis of individual particles, showing the complementary character of both techniques. By means of element mapping of trace constituents in a heterogeneous feldspar, the strong and weak points of SRXRF in comparison to EPXMA and SIMS are illustrated. The most striking difference between SRXRF and the other two microanalytical methods is the ability of SRXRF to probe deep into the investigated Material, whereas SIMS and EPXMA only investigate the upper surface of the material. The possibilities of SRXRF at third generation synchrotron rings is also briefly discussed.

  6. Synchrotron radiation induced x-ray micro analysis: A realistic alternative for electron- and ion beam microscopy?

    SciTech Connect

    Janssens, K.; Adams, F.; Rivers, M.L.; Jones, K.W.

    1992-10-01

    Synchrotron Radiation induced X-ray micro Fluorescence analysis ({mu}-SRXRF) is compared with more conventional microanalytical techniques such as Secondary Ion Microscopy (SIMS) and Electron Probe X-ray Microanalysis (EPXMA) for two typical microanalytical applications. SRXRF and EPXMA are employed for the analysis of individual particles, showing the complementary character of both techniques. By means of element mapping of trace constituents in a heterogeneous feldspar, the strong and weak points of SRXRF in comparison to EPXMA and SIMS are illustrated. The most striking difference between SRXRF and the other two microanalytical methods is the ability of SRXRF to probe deep into the investigated Material, whereas SIMS and EPXMA only investigate the upper surface of the material. The possibilities of SRXRF at third generation synchrotron rings is also briefly discussed.

  7. Uranium aerosols at a nuclear fuel fabrication plant: Characterization using scanning electron microscopy and energy dispersive X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Hansson, E.; Pettersson, H. B. L.; Fortin, C.; Eriksson, M.

    2017-05-01

    Detailed aerosol knowledge is essential in numerous applications, including risk assessment in nuclear industry. Cascade impactor sampling of uranium aerosols in the breathing zone of nuclear operators was carried out at a nuclear fuel fabrication plant. Collected aerosols were evaluated using scanning electron microscopy and energy dispersive X-ray spectroscopy. Imaging revealed remarkable variations in aerosol morphology at the different workshops, and a presence of very large particles (up to ≅ 100 × 50 μm2) in the operator breathing zone. Characteristic X-ray analysis showed varying uranium weight percentages of aerosols and, frequently, traces of nitrogen, fluorine and iron. The analysis method, in combination with cascade impactor sampling, can be a powerful tool for characterization of aerosols. The uranium aerosol source term for risk assessment in nuclear fuel fabrication appears to be highly complex.

  8. Composition measurement in substitutionally disordered materials by atomic resolution energy dispersive X-ray spectroscopy in scanning transmission electron microscopy.

    PubMed

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

    2017-05-01

    The increasing use of energy dispersive X-ray spectroscopy in atomic resolution scanning transmission electron microscopy invites the question of whether its success in precision composition determination at lower magnifications can be replicated in the atomic resolution regime. In this paper, we explore, through simulation, the prospects for composition measurement via the model system of AlxGa1-xAs, discussing the approximations used in the modelling, the variability in the signal due to changes in configuration at constant composition, and the ability to distinguish between different compositions. Results are presented in such a way that the number of X-ray counts, and thus the expected variation due to counting statistics, can be gauged for a range of operating conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Comparison of synchrotron x-ray microanalysis with electron and proton microscopy for individual particle analysis

    SciTech Connect

    Janssens, K.H.; van Langevelde, F.; Adams, F.C.; Vis, R.D.; Sutton, S.R.; Rivers, M.L.; Jones, K.W.; Bowen, D.K.

    1991-12-31

    This paper is concerned with the evaluation of the use of synchrotron/radiation induced x-ray fluorescences ({mu}-SRXRF) as implemented at two existing X-ray microprobes for the analysis of individual particles. As representative environmental particulates, National Institutes of Science and Technology (NIST) K227, K309, K441 and K961 glass microspheres were analyzed using two types of X-ray micro probes: the white light microprobe at beamline X26A of the monochromatic (15 keV) X-ray microprobe at station 7.6 of the SRS. For reference, the particles were also analyzed with microanalytical techniques more commonly employed for individual particles analysis such as EPMA and micro-PIXE.

  10. Comparison of synchrotron x-ray microanalysis with electron and proton microscopy for individual particle analysis

    SciTech Connect

    Janssens, K.H.; van Langevelde, F.; Adams, F.C. ); Vis, R.D. ); Sutton, S.R.; Rivers, M.L. ); Jones, K.W. ); Bowen, D.K. )

    1991-01-01

    This paper is concerned with the evaluation of the use of synchrotron/radiation induced x-ray fluorescences ({mu}-SRXRF) as implemented at two existing X-ray microprobes for the analysis of individual particles. As representative environmental particulates, National Institutes of Science and Technology (NIST) K227, K309, K441 and K961 glass microspheres were analyzed using two types of X-ray micro probes: the white light microprobe at beamline X26A of the monochromatic (15 keV) X-ray microprobe at station 7.6 of the SRS. For reference, the particles were also analyzed with microanalytical techniques more commonly employed for individual particles analysis such as EPMA and micro-PIXE.

  11. X-ray diffraction and electron microscopy studies of frozen erythrocyte membrane preparations.

    PubMed

    Rzepecki, L M; Berriman, J; Finean, J B

    1980-07-16

    Well-defined X-ray diffraction patterns have been recorded from erythrocyte membranes in the frozen state. At -40 degrees C, lamellar periodicities range from 19 to 95 nm depending on the glycerol content (0--40%, respectively). Freeze-fracture electon micrographs of samples frozen in two stages to approximate to the diffraction conditions show ice formation external to membrane stacks. The membrane stacks have periodicities of the same order of magnitude as those obtained by X-ray diffraction.

  12. Multivariate statistics applications in scanning transmission electron microscopy X-ray spectrum imaging

    SciTech Connect

    Parish, Chad M

    2011-01-01

    A modern scanning transmission electron microscope (STEM) fitted with an energy dispersive X-ray spectroscopy (EDS) system can quickly and easily produce spectrum image (SI) datasets containing so much information (hundreds to thousands of megabytes) that they cannot be comprehensively interrogated by a human analyst. Therefore, advanced mathematical techniques are needed to glean materials science and engineering insight into the processing-structure-properties relationship of the examined material from the SI data. This review will discuss recent advances in the application of multivariate statistical analysis (MVSA) methods to STEM-EDS SI experiments. In particular, the fundamental mathematics of principal component analysis (PCA) and related methods are reviewed, and advanced methods such as multivariate curve resolution (MCR) are discussed. The applications of PCA and MCR-based techniques to solve difficult materials science problems, such as the analysis of a particle fully embedded in a matrix phase are discussed, as well as confounding effects such as rank deficiency that can confuse the results of MVSA computations. Possible future advances and areas in need of study are also mentioned.

  13. Equilibrium, FTIR, scanning electron microscopy and small wide angle X-ray scattering studies of chromates adsorption on modified bentonite

    NASA Astrophysics Data System (ADS)

    Majdan, Marek; Maryuk, Oksana; Pikus, Stanisław; Olszewska, Elzbieta; Kwiatkowski, Ryszard; Skrzypek, Henryk

    2005-04-01

    The study presents a discussion about the adsorption mechanism of chromate anions on bentonite modified by hexadecyltrimethylammonium bromide (HDTMA-Br). The formation of alkylammonium chromates: HDTMAHCrO 4, (HDTMA) 2Cr 2O 7 and to the lesser extent (HDTMA) 2CrO 4 at the water-bentonite interface is examined based on the Scanning Electron Microscopy and surface tension measurements. The histograms of HDTMA/Cr(VI) molar ratio on the bentonite surface, found from Scanning Electron Microscopy (SEM) measurements, show that for the majority of points of bentonite surface the value of this ratio is in 1-2 range. FTIR spectra of modified bentonite samples show the change from gauche to trans conformation in the surfactant arrangement in the clay interlayer accompanying its concentration increase. In turn Small Wide Angle X-Ray Scattering (SWAXS) patterns evidently suggest incorporation of chromate anions into the interlamellar space of bentonite structure.

  14. Scanning Transmission X-Ray, Laser Scanning, and Transmission Electron Microscopy Mapping of the Exopolymeric Matrix of Microbial Biofilms

    PubMed Central

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

    2003-01-01

    Confocal laser scanning microscopy (CLSM), transmission electron microscopy (TEM), and soft X-ray scanning transmission X-ray microscopy (STXM) were used to map the distribution of macromolecular subcomponents (e.g., polysaccharides, proteins, lipids, and nucleic acids) of biofilm cells and matrix. The biofilms were developed from river water supplemented with methanol, and although they comprised a complex microbial community, the biofilms were dominated by heterotrophic bacteria. TEM provided the highest-resolution structural imaging, CLSM provided detailed compositional information when used in conjunction with molecular probes, and STXM provided compositional mapping of macromolecule distributions without the addition of probes. By examining exactly the same region of a sample with combinations of these techniques (STXM with CLSM and STXM with TEM), we demonstrate that this combination of multimicroscopy analysis can be used to create a detailed correlative map of biofilm structure and composition. We are using these correlative techniques to improve our understanding of the biochemical basis for biofilm organization and to assist studies intended to investigate and optimize biofilms for environmental remediation applications. PMID:12957944

  15. Soft x-ray laser microscopy

    SciTech Connect

    DiCicco, D.; Meixler, L.; Skinner, C.H.; Suckewer, S.; Hirschberg, J.; Kohen, E.

    1987-12-31

    Microscopes based on soft X-ray lasers possess unique advantages in bridging the gap between high resolution electron microscopy of dehydrated, stained cells and light microscopy at comparatively low resolution of unaltered live cells. The high brightness and short pulse duration of soft X-ray lasers make them ideal for flash imaging of live specimens. The Princeton soft X-ray laser is based on a magnetically confined laser produced carbon plasma. Radiation cooling after the laser pulse produces rapid recombination which produces a population inversion and high gain. A full account is given in a companion paper in this volume. The important characteristics of the laser beam produced by this device are 1 to 3 mJ of 18.2 nm radiation in a 10 to 30 nsec pulse with a divergence of 5 mrad. The 18.2 nm wavelength, while outside the water window, does provide a factor of 3 difference in absorption coefficients between oxygen and carbon.

  16. Soft x-ray laser microscopy

    SciTech Connect

    DiCicco, D. ); Meixler, L.; Skinner, C.H.; Suckewer, S. . Plasma Physics Lab.); Hirschberg, J.; Kohen, E. . Dept. of Physics)

    1987-01-01

    Microscopes based on soft X-ray lasers possess unique advantages in bridging the gap between high resolution electron microscopy of dehydrated, stained cells and light microscopy at comparatively low resolution of unaltered live cells. The high brightness and short pulse duration of soft X-ray lasers make them ideal for flash imaging of live specimens. The Princeton soft X-ray laser is based on a magnetically confined laser produced carbon plasma. Radiation cooling after the laser pulse produces rapid recombination which produces a population inversion and high gain. A full account is given in a companion paper in this volume. The important characteristics of the laser beam produced by this device are 1 to 3 mJ of 18.2 nm radiation in a 10 to 30 nsec pulse with a divergence of 5 mrad. The 18.2 nm wavelength, while outside the water window, does provide a factor of 3 difference in absorption coefficients between oxygen and carbon.

  17. X-ray and electron microscopy studies on the biodistribution and biomodification of iron oxide nanoparticles in Daphnia magna.

    PubMed

    Kwon, Dongwook; Nho, Hyun Woo; Yoon, Tae Hyun

    2014-10-01

    Biodistribution and biomodification of iron oxide (Fe3O4 and α-Fe2O3) nanoparticles (NPs) in a well-known toxicity test organism, Daphnia magna (D. magna), were investigated using transmission electron microscopy (TEM) and scanning transmission X-ray microscopy (STXM). In addition to the morphological changes in the gut tissues of D. magna, biodistribution and biomodification of iron oxide NPs in the digestive tract of D. magna were also monitored in this study. Upon exposures to both iron oxide NPs, unique morphological changes (e.g., irregular shaped microvilli, epithelial cell protrusion, and dilatation of cytoplasmic inclusion) in the gut tissues of D. magna were observed along with bacterial colonization of the gut lumen. However, despite their heavy accumulations in the digesitive tract, TEM and STXM images confirmed us that both Fe3O4 and α-Fe2O3 NPs were not penetrating into the gut tissues of D. magna. Moreover, for the Fe3O4 NPs in direct contact with the gut microvilli of D. magna, slight but significant spectral changes were observed in their Fe L-edge X-ray absorption near edge structure (XANES) spectra, which indicated that there were biomodifications of Fe3O4 NPs, probably involving oxidative dissolution of Fe3O4 NPs followed by rapid precipitation of ferric oxide or hydroxide. However, no significant changes were observed in the Fe L-edge XANES spectra of the α-Fe2O3 NPs present in the gut lumen of D. magna. These X-ray and electron microscopic observations confirmed us that, despite similarities in core sizes and chemical compositions, NPs with different crystalline phase and dissolution rates can interact quite differently with their local environment, may result in different biodistribution and cause completely dissimilar toxicities.

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

    NASA Astrophysics Data System (ADS)

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

    2017-09-01

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

  19. Employing Electron Microscopy integrated with X-ray Spectroscopy for Kuntawa Landslide Assessment

    NASA Astrophysics Data System (ADS)

    Dikedi, P. N.

    2016-12-01

    This work centres on Kuntawa landslide assessment owing to the enigmatic nature of a 2003 landslide which buried 4 people and a truck in Kuntawa village, of Nigeria. A Phenom ProX Scanning Electron Microscope (SEM) integrated with Energy dispersive X-ray Spectroscopy (EDS) and Particlemetric software was employed to generate the morphology, particle size data, elemental identification data and topography (at 3500x) of earth samples scooped from the landslide site. For a core sample 1 at depth, d=3.75m, average circle equivalent diameter dav, area a and volume by area Va of 11.5 µm, 249 µm² and 3680µm³ were generated respectively; at d=3.785m, dav , a and Va of 6.19µm, 30.1µm² and 124µm³ were generated respectively; at d=3.82m, dav , a and Va of 11.5 µm, 130 µm² and 1380µm³ were generated respectively. For a core sample 2, at d=3.75m, dav, a and Va of 5.54 µm, 26 µm² and 108µm³ were generated respectively; at d=3.82m, dav , a and Va of 19.4µm, 338µm² and 5240µm³ were generated respectively; a total of 243 particles were scanned. One of the results from specific surface for samples 1 and 2, reveals that it would take twice and four times the amount of water needed to wet an entire surface both at d=3.82m than at d=3.785m and d=3.75m respectively. Additional laboratory facilities reveal that soil water content Š, volumetric water content Vwc, porosity Φ, soil water-filled pore space Wps, increased with increasing d; bulk density ρb, decreased with increasing d. Elemental composition at the landslide site were generated from the EDS: oxygen (O), Silicon (Si), Bromine (Br), iron (Fe), Carbon (C) and Aluminium (Al). O and C had the highest and lowest concentration of elemental compositions of 68.5% at 3.75m depth and 1% at 3.82m depth for samples 1 and 2, respectively. Keywords: EDS, Particlemetric, SEM.

  20. Development of wavelength-dispersive soft X-ray emission spectrometers for transmission electron microscopes--an introduction of valence electron spectroscopy for transmission electron microscopy.

    PubMed

    Terauchi, Masami; Koike, Masato; Fukushima, Kurio; Kimura, Atsushi

    2010-01-01

    Two types of wavelength-dispersive soft X-ray spectrometers, a high-dispersion type and a conventional one, for transmission electron microscopes were constructed. Those spectrometers were used to study the electronic states of valence electrons (bonding electrons). Both spectrometers extended the acceptable energy regions to higher than 2000 eV. The best energy resolution of 0.08 eV was obtained for an Al L-emission spectrum by using the high-dispersion type spectrometer. By using the spectrometer, C K-emission of carbon allotropes, Cu L-emission of Cu(1-x)Zn(x) alloys and Pt M-emission spectra were presented. The FWHM value of 12 eV was obtained for the Pt Malpha-emission peak. The performance of the conventional one was also presented for ZnS and a section specimen of a multilayer device. W-M and Si-K emissions were clearly resolved. Soft X-ray emission spectroscopy based on transmission electron microscopy (TEM) has an advantage for obtaining spectra from a single crystalline specimen with a defined crystal setting. As an example of anisotropic soft X-ray emission, C K-emission spectra of single crystalline graphite with different crystal settings were presented. From the spectra, density of states of pi- and sigma-bondings were separately derived. These results demonstrated a method to analyse the electronic states of valence electrons of materials in the nanometre scale based on TEM.

  1. Electron Microscopy and Analytical X-ray Characterization of Compositional and Nanoscale Structural Changes in Fossil Bone

    NASA Astrophysics Data System (ADS)

    Boatman, Elizabeth Marie

    The nanoscale structure of compact bone contains several features that are direct indicators of bulk tissue mechanical properties. Fossil bone tissues represent unique opportunities to understand the compact bone structure/property relationships from a deep time perspective, offering a possible array of new insights into bone diseases, biomimicry of composite materials, and basic knowledge of bioapatite composition and nanoscale bone structure. To date, most work with fossil bone has employed microscale techniques and has counter-indicated the survival of bioapatite and other nanoscale structural features. The obvious disconnect between the use of microscale techniques and the discernment of nanoscale structure has prompted this work. The goal of this study was to characterize the nanoscale constituents of fossil compact bone by applying a suite of diffraction, microscopy, and spectrometry techniques, representing the highest levels of spatial and energy resolution available today, and capable of complementary structural and compositional characterization from the micro- to the nanoscale. Fossil dinosaur and crocodile long bone specimens, as well as modern ratite and crocodile femurs, were acquired from the UC Museum of Paleontology. Preserved physiological features of significance were documented with scanning electron microscopy back-scattered imaging. Electron microprobe wavelength-dispersive X-ray spectroscopy (WDS) revealed fossil bone compositions enriched in fluorine with a complementary loss of oxygen. X-ray diffraction analyses demonstrated that all specimens were composed of apatite. Transmission electron microscopy (TEM) imaging revealed preserved nanocrystallinity in the fossil bones and electron diffraction studies further identified these nanocrystallites as apatite. Tomographic analyses of nanoscale elements imaged by TEM and small angle X-ray scattering were performed, with the results of each analysis further indicating that nanoscale structure is

  2. Diffusion of Ag into organic semiconducting materials: a combined analytical study using transmission electron microscopy and X-ray reflectivity.

    PubMed

    Fladischer, Stefanie; Neuhold, Alfred; Kraker, Elke; Haber, Thomas; Lamprecht, Bernhard; Salzmann, Ingo; Resel, Roland; Grogger, Werner

    2012-10-24

    This study shows that the morphology of organic/metal interfaces strongly depends on process parameters and the involved materials. The interface between organic n-type blocking layer materials and the top Ag cathode within an organic photodiode was investigated. Ag was deposited on either amorphous tris-8-hydroxyquinolinato-aluminum (Alq(3)) or crystalline 4,7-diphenyl-1,10-phenanthroline (Bphen) using different deposition techniques such as electron beam deposition, ion beam sputtering, and vacuum thermal evaporation at various deposition rates. The interfaces were studied by transmission electron microscopy and X-ray reflectivity. It was found that Bphen does not show any Ag diffusion no matter which deposition technique was used, whereas the Ag diffusion into Alq(3) depends on the deposition technique and the deposition rate. The highest amount of Ag diffusion into Alq(3) occurred by using thermal vacuum deposition at low deposition rates.

  3. Comparative analysis of isolated cellular organelles by means of soft X-ray contact microscopy with laser-plasma source and transmission electron microscopy.

    PubMed

    Limongi, T; Palladino, L; Tomassetti, G; Reale, L; Cesare, P; Flora, F; Aimola, P; Ragnelli, A M

    2004-04-01

    Soft X-ray contact microscopy (SXCM) is, at present, a useful tool for the examination at submicrometre resolution of biological systems maintained in their natural hydrated conditions. Among current X-ray-generating devices, laser-plasma sources are now easily available and, owing to their pulse nature, offer the opportunity to observe living biological samples before radiation damage occurs, even if the resolution achievable is not as high as with synchrotron-produced X-rays. To assess the potential of laser-plasma source SXCM in the study of cellular organelles, we applied it for the analysis of chloroplasts extracted from spinach leaves and mitochondria isolated from bovine heart and liver. X-ray radiation was generated by a nanosecond laser-plasma source, produced by a single shot excimer XeCl laser focused onto an yttrium target. The images obtained with SXCM were then compared with those produced by transmission electron microscopy observation of the same samples prepared with negative staining, a technique requiring no chemical fixation, in order to facilitate their interpretation and test the applicability of SXCM imaging.

  4. HERMES: a soft X-ray beamline dedicated to X-ray microscopy.

    PubMed

    Belkhou, Rachid; Stanescu, Stefan; Swaraj, Sufal; Besson, Adrien; Ledoux, Milena; Hajlaoui, Mahdi; Dalle, Didier

    2015-07-01

    The HERMES beamline (High Efficiency and Resolution beamline dedicated to X-ray Microscopy and Electron Spectroscopy), built at Synchrotron SOLEIL (Saint-Auban, France), is dedicated to soft X-ray microscopy. The beamline combines two complementary microscopy methods: XPEEM (X-ray Photo Emitted Electron Microscopy) and STXM (Scanning Transmission X-ray Microscopy) with an aim to reach spatial resolution below 20 nm and to fully exploit the local spectroscopic capabilities of the two microscopes. The availability of the two methods within the same beamline enables the users to select the appropriate approach to study their specific case in terms of sample environment, spectroscopy methods, probing depth etc. In this paper a general description of the beamline and its design are presented. The performance and specifications of the beamline will be reviewed in detail. Moreover, the article is aiming to demonstrate how the beamline performances have been specifically optimized to fulfill the specific requirements of a soft X-ray microscopy beamline in terms of flux, resolution, beam size etc. Special attention has been dedicated to overcome some limiting and hindering problems that are usually encountered on soft X-ray beamlines such as carbon contamination, thermal stability and spectral purity.

  5. Localization and chemical forms of cadmium in plant samples by combining analytical electron microscopy and X-ray spectromicroscopy

    NASA Astrophysics Data System (ADS)

    Isaure, Marie-Pierre; Fayard, Barbara; Sarret, Géraldine; Pairis, Sébastien; Bourguignon, Jacques

    2006-12-01

    Cadmium (Cd) is a metal of high toxicity for plants. Resolving its distribution and speciation in plants is essential for understanding the mechanisms involved in Cd tolerance, trafficking and accumulation. The model plant Arabidopsis thaliana was exposed to cadmium under controlled conditions. Elemental distributions in the roots and in the leaves were determined using scanning electron microscopy coupled with energy dispersive X-ray microanalysis (SEM-EDX), and synchrotron-based micro X-ray fluorescence (μ-XRF), which offers a better sensitivity. The chemical form(s) of cadmium was investigated using Cd L III-edge (3538 eV) micro X-ray absorption near edge structure (μ-XANES) spectroscopy. Plant μ-XANES spectra were fitted by linear combination of Cd reference spectra. Biological sample preparation and conditioning is a critical point because of possible artifacts. In this work we compared freeze-dried samples analyzed at ambient temperature and frozen hydrated samples analyzed at -170 °C. Our results suggest that in the roots Cd is localized in vascular bundles, and coordinated to S ligands. In the leaves, trichomes (epidermal hairs) represent the main compartment of Cd accumulation. In these specialized cells, μ-XANES results show that the majority of Cd is bound to O/N ligands likely provided by the cell wall, and a minor fraction could be bound to S-containing ligands. No significant difference in Cd speciation was observed between freeze-dried and frozen hydrated samples. This work illustrates the interest and the sensitivity of Cd L III-edge XANES spectroscopy, which is applied here for the first time to plant samples. Combining μ-XRF and Cd L III-edge μ-XANES spectroscopy offers promising tools to study Cd storage and trafficking mechanisms in plants and other biological samples.

  6. Multi-scale 3D investigations of a commercial 18650 Li-ion battery with correlative electron- and X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Gelb, Jeff; Finegan, Donal P.; Brett, Dan J. L.; Shearing, Paul R.

    2017-07-01

    In the present study, a commercial 18650 Li-ion cylindrical cell is investigated with non-destructive 3D X-ray microscopy across a range of length scales, beginning with a survey of the entire cell and non-destructively enlarging a smaller section. Active materials are extracted from a disassembled cell and imaging performed using a combination of sub-micron X-ray microscopy and 2D scanning-electron microscopy, which point toward the need for multi-scale analysis in order to accurately characterize the cell. Furthermore, a small section is physically isolated for 3D nano-scale X-ray microscopy, which provides a measurement of porosity and enables the effective diffusivity and 3-dimensional tortuosities to be calculated via computer simulation. Finally, the 3D X-ray microscopy data is loaded into a correlative microscopy environment, where a representative sub-surface region is identified and, subsequently, analyzed using electron microscopy and energy-dispersive X-ray spectroscopy. The results of this study elucidate the microstructural characteristics and potential degradation mechanisms of a commercial NCA battery and, further, establish a technique for extracting the Bruggeman exponent for a real-world microstructure using correlative microscopy.

  7. X-ray deconvolution microscopy.

    PubMed

    Ehn, Sebastian; Epple, Franz Michael; Fehringer, Andreas; Pennicard, David; Graafsma, Heinz; Noël, Peter; Pfeiffer, Franz

    2016-04-01

    Recent advances in single-photon-counting detectors are enabling the development of novel approaches to reach micrometer-scale resolution in x-ray imaging. One example of such a technology are the MEDIPIX3RX-based detectors, such as the LAMBDA which can be operated with a small pixel size in combination with real-time on-chip charge-sharing correction. This characteristic results in a close to ideal, box-like point spread function which we made use of in this study. The proposed method is based on raster-scanning the sample with sub-pixel sized steps in front of the detector. Subsequently, a deconvolution algorithm is employed to compensate for blurring introduced by the overlap of pixels with a well defined point spread function during the raster-scanning. The presented approach utilizes standard laboratory x-ray equipment while we report resolutions close to 10 μm. The achieved resolution is shown to follow the relationship [Formula: see text] with the pixel-size p of the detector and the number of raster-scanning steps n.

  8. X-ray deconvolution microscopy

    PubMed Central

    Ehn, Sebastian; Epple, Franz Michael; Fehringer, Andreas; Pennicard, David; Graafsma, Heinz; Noël, Peter; Pfeiffer, Franz

    2016-01-01

    Recent advances in single-photon-counting detectors are enabling the development of novel approaches to reach micrometer-scale resolution in x-ray imaging. One example of such a technology are the MEDIPIX3RX-based detectors, such as the LAMBDA which can be operated with a small pixel size in combination with real-time on-chip charge-sharing correction. This characteristic results in a close to ideal, box-like point spread function which we made use of in this study. The proposed method is based on raster-scanning the sample with sub-pixel sized steps in front of the detector. Subsequently, a deconvolution algorithm is employed to compensate for blurring introduced by the overlap of pixels with a well defined point spread function during the raster-scanning. The presented approach utilizes standard laboratory x-ray equipment while we report resolutions close to 10 μm. The achieved resolution is shown to follow the relationship pn with the pixel-size p of the detector and the number of raster-scanning steps n. PMID:27446649

  9. X-ray omni microscopy.

    PubMed

    Paganin, D; Gureyev, T E; Mayo, S C; Stevenson, A W; Nesterets, Ya I; Wilkins, S W

    2004-06-01

    The science of wave-field phase retrieval and phase measurement is sufficiently mature to permit the routine reconstruction, over a given plane, of the complex wave-function associated with certain coherent forward-propagating scalar wave-fields. This reconstruction gives total knowledge of the information that has been encoded in the complex wave-field by passage through a sample of interest. Such total knowledge is powerful, because it permits the emulation in software of the subsequent action of an infinite variety of coherent imaging systems. Such 'virtual optics', in which software forms a natural extension of the 'hardware optics' in an imaging system, may be useful in contexts such as quantitative atom and X-ray imaging, in which optical elements such as beam-splitters and lenses can be realized in software rather than optical hardware. Here, we develop the requisite theory to describe such hybrid virtual-physical imaging systems, which we term 'omni optics' because of their infinite flexibility. We then give an experimental demonstration of these ideas by showing that a lensless X-ray point projection microscope can, when equipped with the appropriate software, emulate an infinite variety of optical imaging systems including those which yield interferograms, Zernike phase contrast, Schlieren imaging and diffraction-enhanced imaging.

  10. Fine structure and X-ray microanalysis of silicified woods from a Tertiary basin Pohang, Korea by scanning electron microscopy.

    PubMed

    Kim, Ki Woo; Yoon, Chul Jong; Kim, Pan-Gi; Lee, Myung Bo; Lim, Joo-Hoon

    2009-01-01

    Anatomical descriptions are provided on silicified woods from a Tertiary basin Pohang, Korea by scanning electron microscopy and X-ray microanalysis. The silicified woods appeared to retain the original exterior morphology of the once grown trees, and exhibited various colors on the surface. As a component of the axial system in the secondary xylem, pores were oval to globose and measured approximately 200-300 microm in diameter in transverse planes. Seemingly bordered pits were also frequently observed in the tracheary elements. As a component of the axial system in the secondary phloem, sieve elements were found to have many sieve pores that were filled with numerous fine particles. In tangential planes, rays in the vascular cambium were approximately 500 microm long, and usually several cells wide (multiseriate). Meanwhile, several forms of microbial growth such as bacterial chains and hyphal growth of either fungi or actinomycetes were evident in the vessel lumens of unpolished silicified wood pieces. Some fracture surfaces were mainly characterized by the occurrence of polyhedral crystals, probably quartz, in the fissures. By X-ray microanalysis, iron was detected from the brown-colored regions, whereas calcium was also detected together with iron in the black-colored regions. Based on the rare occurrence of tracheids as the axial system in the secondary xylem, the silicified woods in this study can be intrinsically categorized into angiosperm groups in the region.

  11. The architecture of amyloid-like peptide fibrils revealed by X-ray scattering, diffraction and electron microscopy

    SciTech Connect

    Langkilde, Annette E.; Morris, Kyle L.; Serpell, Louise C.; Svergun, Dmitri I.; Vestergaard, Bente

    2015-04-01

    The aggregation process and the fibril state of an amyloidogenic peptide suggest monomer addition to be the prevailing mechanism of elongation and a model of the peptide packing in the fibrils has been obtained. Structural analysis of protein fibrillation is inherently challenging. Given the crucial role of fibrils in amyloid diseases, method advancement is urgently needed. A hybrid modelling approach is presented enabling detailed analysis of a highly ordered and hierarchically organized fibril of the GNNQQNY peptide fragment of a yeast prion protein. Data from small-angle X-ray solution scattering, fibre diffraction and electron microscopy are combined with existing high-resolution X-ray crystallographic structures to investigate the fibrillation process and the hierarchical fibril structure of the peptide fragment. The elongation of these fibrils proceeds without the accumulation of any detectable amount of intermediate oligomeric species, as is otherwise reported for, for example, glucagon, insulin and α-synuclein. Ribbons constituted of linearly arranged protofilaments are formed. An additional hierarchical layer is generated via the pairing of ribbons during fibril maturation. Based on the complementary data, a quasi-atomic resolution model of the protofilament peptide arrangement is suggested. The peptide structure appears in a β-sheet arrangement reminiscent of the β-zipper structures evident from high-resolution crystal structures, with specific differences in the relative peptide orientation. The complexity of protein fibrillation and structure emphasizes the need to use multiple complementary methods.

  12. Scanning electron microscopy and energy-dispersive X-ray microanalysis of Penicillium brevicompactum treated with cobalt.

    PubMed

    Farrag, Rasha M; Mohamadein, Mohamed M; Mekawy, Amal A

    2008-01-01

    Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) were used to study the morphology and elemental composition of the conidia, phialids and hyphae of Penicillium brevicompactum grown in the presence of cobalt concentrations of 0, 50, 200, 500, 800 and 1000 ppm (mg/l). Cobalt uptake was through the hyphae, phialids and the conidia with maximum uptake being by the conidia at a concentration of 1000 ppm. EDX revealed the increase in the percentage of calcium and magnesium in the hyphae, conidia and phialids, compared to corresponding controls, accompanying the increase in cobalt uptake. Alternatively a decrease in sulfur percentage was observed. This study might reflect the possibility of using SEM-EDX as a new technique in understanding the mechanism of tolerance.

  13. Nail Damage (Severe Onychodystrophy) Induced by Acrylate Glue: Scanning Electron Microscopy and Energy Dispersive X-Ray Investigations

    PubMed Central

    Pinteala, Tudor; Chiriac, Anca Eduard; Rosca, Irina; Larese Filon, Francesca; Pinteala, Mariana; Chiriac, Anca; Podoleanu, Cristian; Stolnicu, Simona; Coros, Marius Florin; Coroaba, Adina

    2017-01-01

    Background Scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) techniques have been used in various fields of medical research, including different pathologies of the nails; however, no studies have focused on obtaining high-resolution microscopic images and elemental analysis of disorders caused by synthetic nails and acrylic adhesives. Methods Damaged/injured fingernails caused by the use of acrylate glue and synthetic nails were investigated using SEM and EDX methods. Results SEM and EDX proved that synthetic nails, acrylic glue, and nails damaged by contact with acrylate glue have a different morphology and different composition compared to healthy human nails. Conclusions SEM and EDX analysis can give useful information about the aspects of topography (surface sample), morphology (shape and size), hardness or reflectivity, and the elemental composition of nails. PMID:28232921

  14. Energy-dispersive and x-ray photoelectron spectroscopy and electron microscopy of new quininium-plastic membrane electrodes.

    PubMed

    Shoukry, Adel F; Maraffie, Hayat M; Al-Shatti, Laila A

    2007-10-01

    New quininium (Qn) plastic membrane electrodes of the conventional type were constructed and characterized. They are based on incorporation of Qn-reineckate (QnRn) ion-pair, Qn-phosphotungstate (Qn3-PT), or Qn-phosphomolybdate (Qn3PM) ion associate into a poly(vinyl chloride) membrane. The electrodes are selective for Qn and have been successfully used for the determination of Qn2SO4 in pharmaceutical tablets. Nevertheless, they showed, as almost all other ion-selective electrodes, limited life times. Energy dispersive- (EDS) and X-ray photoelectron spectroscopy (XPS), as well as electron microscopy were applied to investigate the cause of this limitation in the life times of the electrodes. The results indicated that the electrodes lose their activity after prolonged soaking as a result of leaching of the ion exchanger from the membranes into the test solution in addition to deformation at the surface of the expired electrode.

  15. Analysis of Individual Environmental Particles Using Modern Methods of Electron Microscopy and X-Ray Microanalysis

    SciTech Connect

    Laskin, Alexander; Cowin, James P.; Iedema, Martin J.

    2006-02-01

    Understanding the composition of particles in the atmosphere is critical because of their health effects and their direct and indirect effects on radiative forcing, and hence on climate. In this manuscript, we demonstrate the utility of single particle off-line analysis to investigate the chemistry of individual atmospheric particles using modern, state-of-the-art electron microscopy and time-of-flight secondary ionization mass spectrometry techniques. We show that these methods provide specific, detailed data on particle composition, chemistry, morphology, phase and internal structure. This information is crucial for evaluating hygroscopic properties of aerosols, understanding aerosol aging and reactivity, and correlating the characteristics of aerosols with their optical properties. The manuscript presents a number of analytical advances in methods of electron probe particle analysis along with a brief review of a number of the research projects carried out in the authors’ laboratory on the chemical characterization of environmental particles. The obtained data offers a rich set of qualitative and quantitative information on the particle chemistry, composition and the mechanisms of gas-particle interactions which are of high importance to atmospheric processes involving particulate matter and air pollution.

  16. Cryo-electron microscopy and X-ray crystallography: complementary approaches to structural biology and drug discovery.

    PubMed

    Vénien-Bryan, Catherine; Li, Zhuolun; Vuillard, Laurent; Boutin, Jean Albert

    2017-04-01

    The invention of the electron microscope has greatly enhanced the view scientists have of small structural details. Since its implementation, this technology has undergone considerable evolution and the resolution that can be obtained for biological objects has been extended. In addition, the latest generation of cryo-electron microscopes equipped with direct electron detectors and software for the automated collection of images, in combination with the use of advanced image-analysis methods, has dramatically improved the performance of this technique in terms of resolution. While calculating a sub-10 Å resolution structure was an accomplishment less than a decade ago, it is now common to generate structures at sub-5 Å resolution and even better. It is becoming possible to relatively quickly obtain high-resolution structures of biological molecules, in particular large ones (>500 kDa) which, in some cases, have resisted more conventional methods such as X-ray crystallography or nuclear magnetic resonance (NMR). Such newly resolved structures may, for the first time, shed light on the precise mechanisms that are essential for cellular physiological processes. The ability to attain atomic resolution may support the development of new drugs that target these proteins, allowing medicinal chemists to understand the intimacy of the relationship between their molecules and targets. In addition, recent developments in cryo-electron microscopy combined with image analysis can provide unique information on the conformational variability of macromolecular complexes. Conformational flexibility of macromolecular complexes can be investigated using cryo-electron microscopy and multiconformation reconstruction methods. However, the biochemical quality of the sample remains the major bottleneck to routine cryo-electron microscopy-based determination of structures at very high resolution.

  17. Soft x-ray holographic microscopy

    SciTech Connect

    Stickler, Daniel; Froemter, Robert; Stillrich, Holger; Menk, Christian; Oepen, Hans Peter; Tieg, Carsten; Streit-Nierobisch, Simone; Sprung, Michael; Gutt, Christian; Stadler, Lorenz-M.; Leupold, Olaf; Gruebel, Gerhard

    2010-01-25

    We present a new x-ray microscopy technique based on Fourier transform holography (FTH), where the sample is separate from the optics part of the setup. The sample can be shifted with respect to the holography optics, thus large-scale or randomly distributed objects become accessible. As this extends FTH into a true microscopy technique, we call it x-ray holographic microscopy (XHM). FTH allows nanoscale imaging without the need for nanometer-size beams. Simple Fourier transform yields an unambiguous image reconstruction. We demonstrate XHM by studying the magnetic domain evolution of a Co/Pt multilayer film as function of locally varied iron overlayer thickness.

  18. Automated scanning electron microscopy and x-ray microanalysis for in situ quantification of gadolinium deposits in skin.

    PubMed

    Thakral, Charu; Abraham, Jerrold L

    2007-10-01

    Gadolinium (Gd) has been identified as a possible causative agent of an emerging cutaneous and systemic fibrosing disorder, nephrogenic systemic fibrosis (NSF), which can cause serious disability and even death. To date, there are only two known associations with this disorder--renal insufficiency and Gd enhanced magnetic resonance imaging (MRI). We developed an automated quantitative scanning electron microscopy (SEM) and Energy dispersive x-ray spectroscopy (EDS) method for Gd in tissue of NSF patients. Freshly cut paraffin block surfaces examined using the variable pressure mode under standardized conditions and random search of the tissue area allow in situ detection and semiquantitative morphometric (volumetric) analysis of insoluble higher atomic number features using backscattered electron imaging. We detected Gd ranging from 1 to 2270 cps/mm2 in 57 cutaneous biopsies of NSF. Gd was associated with P, Ca, and usually Na in tissue deposits. Our method reproducibly determines the elemental composition, relative concentration, and spatial distribution of detected features within the tissue. However, we cannot detect features below our spatial resolution, nor concentrations below the detection limit of our SEM/EDS system. The findings confirm transmetallation and release of toxic Gd ions in NSF and allow dose-response analysis at the histologic level.

  19. X-ray photoelectron spectroscopy and transmission electron microscopy analysis of silver-coated gold nanorods designed for bionanotechnology applications

    NASA Astrophysics Data System (ADS)

    Watanabe, Fumiya; Nima, Zeid A.; Honda, Takumi; Mitsuhara, Masatoshi; Nishida, Minoru; Biris, Alexandru S.

    2017-01-01

    Multicomponent nano-agents were designed and built via a core-shell approach to enhance their surface enhanced Raman scattering (SERS) signals. These nano-agents had 36 nm × 12 nm gold nanorod cores coated by 4 nm thick silver shell films and a subsequent thin bifunctional thiolated polyethylene glycol (HS-PEG-COOH) layer. Ambient time-lapsed SERS signal measurements of these functionalized nanorods taken over a two-week period indicated no signal degradation, suggesting that large portions of the silver shells remained in pure metallic form. The morphology of the nanorods was characterized by transmission electron microscopy (TEM) and ultra-high resolution scanning TEM. X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES) were utilized to assess the oxidation states of the silver shells covered by HS-PEG-COOH. The binding energies of Ag 3d XPS spectra yielded very small chemical shifts with oxidation; however, the AES peak shapes gave meaningful information about the extent of oxidation undergone by the nano-agent. While the silver shells without HS-PEG-COOH coatings oxidized significantly, the silver shells with HS-PEG-COOH remained predominantly metallic. In fact, six month-old samples still retained mostly metallic silver shells. These findings further demonstrate the stability and longevity of the nanostructures, indicating their significant potential as plasmonically active agents for highly sensitive detection in various biological systems, including cancer cells, tissues, or even organisms.

  20. X-ray microscopy as an approach to increasing accuracy and efficiency of serial block-face imaging for correlated light and electron microscopy of biological specimens.

    PubMed

    Bushong, Eric A; Johnson, Donald D; Kim, Keun-Young; Terada, Masako; Hatori, Megumi; Peltier, Steven T; Panda, Satchidananda; Merkle, Arno; Ellisman, Mark H

    2015-02-01

    The recently developed three-dimensional electron microscopic (EM) method of serial block-face scanning electron microscopy (SBEM) has rapidly established itself as a powerful imaging approach. Volume EM imaging with this scanning electron microscopy (SEM) method requires intense staining of biological specimens with heavy metals to allow sufficient back-scatter electron signal and also to render specimens sufficiently conductive to control charging artifacts. These more extreme heavy metal staining protocols render specimens light opaque and make it much more difficult to track and identify regions of interest (ROIs) for the SBEM imaging process than for a typical thin section transmission electron microscopy correlative light and electron microscopy study. We present a strategy employing X-ray microscopy (XRM) both for tracking ROIs and for increasing the efficiency of the workflow used for typical projects undertaken with SBEM. XRM was found to reveal an impressive level of detail in tissue heavily stained for SBEM imaging, allowing for the identification of tissue landmarks that can be subsequently used to guide data collection in the SEM. Furthermore, specific labeling of individual cells using diaminobenzidine is detectable in XRM volumes. We demonstrate that tungsten carbide particles or upconverting nanophosphor particles can be used as fiducial markers to further increase the precision and efficiency of SBEM imaging.

  1. X-ray microscopy of human malaria

    SciTech Connect

    Magowan, C.; Brown, J.T.; Mohandas, N.; Meyer-Ilse, W.

    1997-04-01

    Associations between intracellular organisms and host cells are complex and particularly difficult to examine. X-ray microscopy provides transmission images of subcellular structures in intact cells at resolutions superior to available methodologies. The spatial resolution is 50-60nm with a 1 micron depth of focus, superior to anything achievable with light microscopy. Image contrast is generated by differences in photoelectric absorption by the atoms in different areas (i.e. subcellular structures) throughout the full thickness of the sample. Absorption due to carbon dominates among all the elements in the sample at 2.4 nm x-ray wavelength. Thus images show features or structures, in a way not usually seen by other types of microscopy. The authors used soft x-ray microscopy to investigate structural development of Plasmodium falciparum malaria parasites in normal and genetically abnormal erythrocytes, and in infected erythrocytes treated with compounds that have anti-malarial effects. X-ray microscopy showed newly elaborated structures in the cytosol of unstained, intact erythrocytes, redistribution of mass (carbon) in infected erythrocytes, and aberrant parasite morphology. Better understanding of the process of intracellular parasite maturation and the interactions between the parasite and its host erythrocyte can help define new approaches to the control of this deadly disease.

  2. Lung dust content in idiopathic pulmonary fibrosis: a study with scanning electron microscopy and energy dispersive x ray analysis.

    PubMed Central

    Monsó, E; Tura, J M; Pujadas, J; Morell, F; Ruiz, J; Morera, J

    1991-01-01

    Examination with an optical microscope and polarised light is not sensitive enough to detect low diameter asbestos fibres. This limitation implies that some cases of asbestosis can be erroneously diagnosed as idiopathic pulmonary fibrosis (IPF) if asbestos bodies are not found in the standard examination of abnormal tissue. To determine whether IPF is over-diagnosed, a study was carried out with scanning electron microscopy (SEM) and energy dispersive x ray analysis (EDXA) on 25 samples previously diagnosed as IPF at the standard examination. Scanning electron microscopy will show the presence of low diameter fibres in the lung without tissue destruction, and these fibres can be identified using EDXA. The quantitative and qualitative results for lung tissue from patients diagnosed as having IPF were compared with the results of the examination of 25 samples of normal lung. Most of the samples from patients diagnosed as having IPF showed only occasional inorganic particles (less than 10 particles/SEM field at 160 x), results equivalent to the results obtained in normal lung. Two cases of IPF, however, showed innumerable asbestos fibres (greater than 100 fibres/SEM field). One of these two patients had an antecedent of brief exposure to asbestos. No environmental antecedent was found in the second patient. Asbestosis was the final diagnosis for these two patients. The examination of inorganic particles in normal lungs showed mainly non-fibrous silicates (61.4%) and particles of heavy elements (34.9%). Only one asbestos fibre was found (0.9%). It is concluded that standard pathological techniques overdiagnose IPF in a few cases in which asbestos bodies are not found with the optical microscope. Images PMID:2039745

  3. Characterization of leaf-level particulate matter for an industrial city using electron microscopy and X-ray microanalysis.

    PubMed

    Sgrigna, G; Baldacchini, C; Esposito, R; Calandrelli, R; Tiwary, A; Calfapietra, C

    2016-04-01

    This study reports application of monitoring and characterization protocol for particulate matter (PM) deposited on tree leaves, using Quercus ilex as a case study species. The study area is located in the industrial city of Terni in central Italy, with high PM concentrations. Four trees were selected as representative of distinct pollution environments based on their proximity to a steel factory and a street. Wash off from leaves onto cellulose filters were characterized using scanning electron microscopy and energy dispersive X-ray spectroscopy, inferring the associations between particle sizes, chemical composition, and sampling location. Modeling of particle size distributions showed a tri-modal fingerprint, with the three modes centered at 0.6 (factory related), 1.2 (urban background), and 2.6μm (traffic related). Chemical detection identified 23 elements abundant in the PM samples. Principal component analysis recognized iron and copper as source-specific PM markers, attributed mainly to industrial and heavy traffic pollution respectively. Upscaling these results on leaf area basis provided a useful indicator for strategic evaluation of harmful PM pollutants using tree leaves.

  4. NASA Li/CF(x) cell problem analysis: Scanning electron microscopy with energy dispersive x ray spectrometry

    NASA Astrophysics Data System (ADS)

    Baker, John

    1991-05-01

    An analysis was made of Lithium/carbon fluoride cell parts for possible chloride contamination induced by exposure to thionyl chloride (SOCl2); various samples were submitted for analysis. Only a portion of the analysis which has been conducted is covered, herein, namely analysis by scanning electron microscopy with energy dispersive x ray spectrometry (SEM/EDS). A strip of nickel was exposed to SOCl2 vapors to observe variations in surface concentrations of sulfur and chlorine with time. By detecting chlorine one can not infer contamination by SOCl2 only that contamination is present. Six samples of stainless steel foil were analyzed for chlorine using EDS. Chlorine was not detected on background samples but was detected on the samples which had been handled including those which had been cleaned. Cell covers suspected of being contaminated while in storage and covers which were not exposed to the same storage conditions were analyzed for chlorine. Although no chlorine was found on the covers from cells, it was found on all stored covers. Results are presented with techniques shown for analysis and identification. Relevant photomicrographs are presented.

  5. Investigation of corrosion and container integrity in metal food containers using scanning electron microscopy-X-ray microanalysis.

    PubMed

    Charbonneau, J E

    2001-01-01

    Scanning electron microscopy and x-ray microanalysis were used to investigate microleakage, two incidences of loss of coating integrity, filiform corrosion, and sulfide black corrosion in enamel-lined metal food containers. Microleakage developed in a canned cheese sauce at the side seam weld and was traced to a hot weld and a cold weld defect. An enamel-blistering problem developed in an aseptically processed milk-based product when the tinplate was heated above its melting point; the tin melted under the enamel coating, causing the blistering. An enamel-blistering problem, due to silicon contamination of the metal surface prior to enameling, developed on the bottom of a two-piece can that contained a chicken-based product. A sulfide black problem developed in canned clams, caused by scratches in the coating that were introduced during can manufacturing. A filiform corrosion problem developed on the outside of the easy score line of enameled tinplate lids with a light tin coating 0.08 microns thick.

  6. Synchrotron X-ray diffraction and scanning electron microscopy to understand enamel affected by metabolic disorder mucopolysaccharidosis.

    PubMed

    Khan, Malik Arshman; Addison, Owen; James, Alison; Hendriksz, Christian J; Al-Jawad, Maisoon

    2016-04-01

    Mucopolysaccharidosis (MPS) is an inherited metabolic disorder that can affect the tooth structure leading to defects. Synchrotron X-ray diffraction being a state of the art technique has been used to determine the enamel crystallite orientation in deciduous enamel affected by Mucopolysaccharidosis Type I and Mucopolysaccharidosis Type IVA and comparing these with that of healthy deciduous enamel. Using this technique it was observed that there is a loss of texture in deciduous enamel affected by Mucopolysaccharidosis Type I and Mucopolysaccharidosis Type IVA when compared to the healthy deciduous enamel. Generally it was observed that the incisal surface of the deciduous teeth possessed a higher texture or preferred orientation of enamel crystallites and on progression towards the cervical region there was a decrease in the texture or preferred orientation of enamel crystallites. Scanning electron microscopy showed that the presence of a poorly calcified layer between the enamel and dentine at the enamel-dentine junction (EDJ) in MPS affected samples was likely to be responsible for rendering the tooth structure weak and prone to fracture as is often the case in MPS affected deciduous enamel.

  7. NASA Li/CF(x) cell problem analysis: Scanning electron microscopy with energy dispersive x ray spectrometry

    NASA Technical Reports Server (NTRS)

    Baker, John

    1991-01-01

    An analysis was made of Lithium/carbon fluoride cell parts for possible chloride contamination induced by exposure to thionyl chloride (SOCl2); various samples were submitted for analysis. Only a portion of the analysis which has been conducted is covered, herein, namely analysis by scanning electron microscopy with energy dispersive x ray spectrometry (SEM/EDS). A strip of nickel was exposed to SOCl2 vapors to observe variations in surface concentrations of sulfur and chlorine with time. By detecting chlorine one can not infer contamination by SOCl2 only that contamination is present. Six samples of stainless steel foil were analyzed for chlorine using EDS. Chlorine was not detected on background samples but was detected on the samples which had been handled including those which had been cleaned. Cell covers suspected of being contaminated while in storage and covers which were not exposed to the same storage conditions were analyzed for chlorine. Although no chlorine was found on the covers from cells, it was found on all stored covers. Results are presented with techniques shown for analysis and identification. Relevant photomicrographs are presented.

  8. Scanning electron microscopy and energy-dispersive X-ray analysis of defects in mature rat incisor enamel after thyroparathyroidectomy.

    PubMed

    Chardin, H; Acevedo, A C; Risnes, S

    1998-04-01

    The surface and the structure of the erupted enamel of the continuously growing rat incisor were studied by scanning electron microscopy (SEM) to analyse the effect of thyroparathyroidectomy on enamel formation. Ten male 21-day-old Wistar rats were thyroparathyroidectomized and five sham-operated rats were used as controls. Two months after surgery the rats were perfused with 1% glutaraldehyde and their mandibles dissected. The erupted ends of the incisors were cut off and routinely processed for SEM. An energy-dispersive analysis of X-rays (EDX analysis) was performed for the calcium:iron ratio of the enamel surface defects. Thyroparathyroidectomy induced surface defects and structural abnormalities in the outer layer of the mature erupted enamel. It was established that the surface and structural defects were related. The EDX analysis of the outer enamel showed that the enamel defects were associated with an abnormal elevation of the iron content. The SEM appearance and the EDX analyses indicated that these defects were hypomineralized and rich in iron. The reddish colour of the enamel is due to the high concentrations of iron.

  9. An analysis of FtsZ assembly using small angle X-ray scattering and electron microscopy.

    PubMed

    Kuchibhatla, Anuradha; Abdul Rasheed, A S; Narayanan, Janaky; Bellare, Jayesh; Panda, Dulal

    2009-04-09

    Small angle X-ray scattering (SAXS) was used for the first time to study the self-assembly of the bacterial cell division protein, FtsZ, with three different additives: calcium chloride, monosodium glutamate and DEAE-dextran hydrochloride in solution. The SAXS data were analyzed assuming a model form factor and also by a model-independent analysis using the pair distance distribution function. Transmission electron microscopy (TEM) was used for direct observation of the FtsZ filaments. By sectioning and negative staining with glow discharged grids, very high bundling as well as low bundling polymers were observed under different assembly conditions. FtsZ polymers formed different structures in the presence of different additives and these additives were found to increase the bundling of FtsZ protofilaments by different mechanisms. The combined use of SAXS and TEM provided us a significant insight of the assembly of FtsZ and microstructures of the assembled FtsZ polymers.

  10. Scanning electron microscopy and energy-dispersive X-ray microanalysis studies of several human calculi containing calcium phosphate crystals.

    PubMed

    Kodaka, T; Debari, K; Sano, T; Yamada, M

    1994-01-01

    Human calcium phosphate calculi: two sialoliths, a urolith, a rhinolith, and a tonsillolith were investigated by scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDX). The sialoliths and urolith had appositional shells with thick cortices, respectively, around several nuclei composed of calcospherulites and a rubber-film fragment. The rhinolith had a thin cortex with appositional laminations around a glomerulus-like mass of calcified cotton-like strings. The tonsillolith had a rough cortex with appositional laminations. Its porous interior was composed of numerous calcified conglomerates with microorganisms and calcified masses with fine appositional laminations around the conglomerates. The major crystals were identified as biological apatites (AP) with a sand-grain rather than a needle-like shape, and plate-shaped octacalcium phosphate (OCP). The AP deposits of the rhinolith probably were associated with magnesium (Mg) phosphates or contained Mg. No OCP was found in the rhinolith. The AP deposits were mainly formed by extracellular calcification. Hexahedral crystals, identified as Mg-containing whitlockite (WH), were precipitated in the internal spaces of the AP and OCP deposits. The rhinolith nucleus consisted of WH crystal deposits only.

  11. NASA Li/CF(x) cell problem analysis: Scanning electron microscopy with energy dispersive x ray spectrometry

    NASA Technical Reports Server (NTRS)

    Baker, John

    1991-01-01

    An analysis was made of Lithium/carbon fluoride cell parts for possible chloride contamination induced by exposure to thionyl chloride (SOCl2); various samples were submitted for analysis. Only a portion of the analysis which has been conducted is covered, herein, namely analysis by scanning electron microscopy with energy dispersive x ray spectrometry (SEM/EDS). A strip of nickel was exposed to SOCl2 vapors to observe variations in surface concentrations of sulfur and chlorine with time. By detecting chlorine one can not infer contamination by SOCl2 only that contamination is present. Six samples of stainless steel foil were analyzed for chlorine using EDS. Chlorine was not detected on background samples but was detected on the samples which had been handled including those which had been cleaned. Cell covers suspected of being contaminated while in storage and covers which were not exposed to the same storage conditions were analyzed for chlorine. Although no chlorine was found on the covers from cells, it was found on all stored covers. Results are presented with techniques shown for analysis and identification. Relevant photomicrographs are presented.

  12. Minerals discovered in paleolithic black pigments by transmission electron microscopy and micro-X-ray absorption near-edge structure

    NASA Astrophysics Data System (ADS)

    Chalmin, E.; Vignaud, C.; Salomon, H.; Farges, F.; Susini, J.; Menu, M.

    2006-05-01

    Analysis of archeological materials aims to rediscover the know-how of prehistoric men by determining the nature of the painting matter, its preparation mode, and the geographic origin of its raw materials. The preparation mode of the painting matter of the paleolithic rock art apparently consisted of mixing, grinding, and also heat-treatment. In this study, we focus on black pigments and more particularly manganese oxides. Using the combined approach of transmission electron microscopy (TEM) and Mn K-edge X-ray absorption near-edge structure (XANES) spectroscopy, we analyzed a variety of archeological black painted samples. The studied pigments arise from the caves of Ekain (Basque country, Spain), Labastide and Gargas (Hautes-Pyrénées, France). In addition, a black “crayon” (i.e., a “pen”) from the cave of Combe Saunière (Dordogne, France) was also investigated. From the analysis of these painting matters, several unusual minerals have been identified as black pigment, such as manganite, groutite, todorokite and birnessite. These conclusions enable us to estimate the technical level of paleolithic artists: they didn’t use heat-treatment to prepare black painting matter. Consequently, the unusual mineralogy found in some of these pigments suggests that some of the manganese ores are coming from geological settings that are sometimes relatively far away from the Dordogne and Basque region such as in Ariège (central-oriental Pyrénées).

  13. Contact x-ray microscopy using Asterix

    NASA Astrophysics Data System (ADS)

    Conti, Aldo; Batani, Dimitri; Botto, Cesare; Masini, Alessandra; Bernardinello, A.; Bortolotto, Fulvia; Moret, M.; Poletti, G.; Piccoli, S.; Cotelli, F.; Lora Lamia Donin, C.; Stead, Anthony D.; Marranca, A.; Eidmann, Klaus; Flora, Francesco; Palladino, Libero; Reale, Lucia

    1997-10-01

    The use of a high energy laser source for soft x-ray contact microscopy is discussed. Several different targets were used and their emission spectra compared. The x-ray emission, inside and outside the Water Window, was characterized in detail by means of many diagnostics, including pin hole and streak cameras. Up to 12 samples holders per shot were exposed thanks to the large x-ray flux and the geometry of the interaction chamber. Images of several biological samples were obtained, including Chlamydomonas and Crethidia green algae, fish and boar sperms and Saccharomyces Cerevisiae yeast cells. A 50 nm resolution was reached on the images of boar sperm. Original information concerning the density of inner structures of Crethidia green algae were obtained.

  14. Effects of Pamidronate on Dental Enamel Formation Assessed by Light Microscopy, Energy-Dispersive X-Ray Analysis, Scanning Electron Microscopy, and Microhardness Testing.

    PubMed

    Soares, Ana P; do Espírito Santo, Renan F; Line, Sérgio R P; Pinto, Maria das G F; Santos, Pablo de M; Toralles, Maria Betania P; do Espírito Santo, Alexandre R

    2016-06-01

    The aim of the present work was to investigate birefringence and morphology of the secretory-stage enamel organic extracellular matrix (EOECM), and structural and mechanical properties of mature enamel of upper incisors from adult rats that had been treated with pamidronate disodium (0.5 mg/kg/week for 56 days), using transmitted polarizing and bright-field light microscopies (TPLM and BFLM), energy-dispersive X-ray (EDX) analysis, scanning electron microscopy (SEM) and microhardness testing. BFLM showed no morphological changes of the EOECM in pamidronate and control groups, but TPLM revealed a statistically significant reduction in optical retardation values of birefringence brightness of pamidronate-treated rats when compared with control animals (p0.05). The present study indicates that pamidronate can affect birefringence of the secretory-stage EOECM, which does not seem to be associated with significant changes in morphological and/or mechanical properties of mature enamel.

  15. A false report of product tampering involving a rodent and soft drink can: light microscopy, image analysis and scanning electron microscopy/energy dispersive X-ray analysis.

    PubMed

    Platek, F; Ranieri, N; Wolnik, K A

    1997-11-01

    The "Pepsi Tamperings" of 1993 resulted in a large number of cases involving foreign objects reportedly found inside canned soft drinks. Although the majority of cases involved medical syringes and metallic objects, one case involved the report of a mouse found inside a can of Caffeine-Free Diet Pepsi. Using light and polarized light microscopy and computer-assisted image analysis, trace evidence and tooth structure from the suspect mouse were matched to scratches and indentions on the suspect can. Scanning electron microscopy and energy dispersive X-ray analysis were used to compare and match particles of gnawed metal from the lid of the suspect can to other particles recovered from the muzzle and stomach of the suspect mouse. The forensic analyses in this case proved the mouse could not have been canned in the soft drink product and refuted the defendant's sworn statements.

  16. Atmospheric electron x-ray spectrometer

    NASA Technical Reports Server (NTRS)

    Feldman, Jason E. (Inventor); George, Thomas (Inventor); Wilcox, Jaroslava Z. (Inventor)

    2002-01-01

    The present invention comprises an apparatus for performing in-situ elemental analyses of surfaces. The invention comprises an atmospheric electron x-ray spectrometer with an electron column which generates, accelerates, and focuses electrons in a column which is isolated from ambient pressure by a:thin, electron transparent membrane. After passing through the membrane, the electrons impinge on the sample in atmosphere to generate characteristic x-rays. An x-ray detector, shaping amplifier, and multi-channel analyzer are used for x-ray detection and signal analysis. By comparing the resultant data to known x-ray spectral signatures, the elemental composition of the surface can be determined.

  17. Electron beam parallel X-ray generator

    NASA Technical Reports Server (NTRS)

    Payne, P.

    1967-01-01

    Broad X ray source produces a highly collimated beam of low energy X rays - a beam with 2 to 5 arc minutes of divergence at energies between 1 and 6 keV in less than 5 feet. The X ray beam is generated by electron bombardment of a target from a large area electron gun.

  18. Electron probe X-ray microanalysis of cultured myogenic C2C12 cells with scanning and scanning transmission electron microscopy.

    PubMed

    Tylko, G; Karasiński, J; Wróblewski, R; Roomans, G M; Kilarski, W M

    2000-01-01

    Heterogeneity of the elemental content of myogenic C2C12 cultured cells was studied by electron probe X-ray microanalysis (EPXMA) with scanning (SEM EPXMA) and scanning transmission electron microscopy (STEM EPXMA). The best plastic substrate for growing cells was Thermanox. For STEM EPXMA, a Formvar film coated with carbon was found to be suitable substrate. The cells examined by scanning transmission electron microscopy showed great heterogeneity in their elemental content in comparison with the cells examined in the scanning electron microscope despite of an almost identical preparation procedure for EPXMA. Nevertheless the K/Na ratios obtained from both methods of EPXMA were very close (4.1 and 4.3). We conclude that the observed discrepancy in the elemental content obtained by the two methods may be due to differences in instrumentation and this must be taken into account when planning a comparative study.

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

    PubMed

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

    2015-06-01

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

  20. Soft x-ray reflectometry, hard x-ray photoelectron spectroscopy and transmission electron microscopy investigations of the internal structure of TiO2(Ti)/SiO2/Si stacks

    PubMed Central

    Filatova, Elena O; Kozhevnikov, Igor V; Sokolov, Andrey A; Ubyivovk, Evgeniy V; Yulin, Sergey; Gorgoi, Mihaela; Schäfers, Franz

    2012-01-01

    We developed a mathematical analysis method of reflectometry data and used it to characterize the internal structure of TiO2/SiO2/Si and Ti/SiO2/Si stacks. Atomic concentration profiles of all the chemical elements composing the samples were reconstructed from the analysis of the reflectivity curves measured versus the incidence angle at different soft x-ray reflection (SXR) photon energies. The results were confirmed by the conventional techniques of hard x-ray photoelectron spectroscopy (HXPES) and high-resolution transmission electron microscopy (HRTEM). The depth variation of the chemical composition, thicknesses and densities of individual layers extracted from SXR and HXPES measurements are in close agreement and correlate well with the HRTEM images. PMID:27877468

  1. Laboratory cryo soft X-ray microscopy.

    PubMed

    Hertz, H M; von Hofsten, O; Bertilson, M; Vogt, U; Holmberg, A; Reinspach, J; Martz, D; Selin, M; Christakou, A E; Jerlström-Hultqvist, J; Svärd, S

    2012-02-01

    Lens-based water-window X-ray microscopy allows two- and three-dimensional (2D and 3D) imaging of intact unstained cells in their near-native state with unprecedented contrast and resolution. Cryofixation is essential to avoid radiation damage to the sample. Present cryo X-ray microscopes rely on synchrotron radiation sources, thereby limiting the accessibility for a wider community of biologists. In the present paper we demonstrate water-window cryo X-ray microscopy with a laboratory-source-based arrangement. The microscope relies on a λ=2.48-nm liquid-jet high-brightness laser-plasma source, normal-incidence multilayer condenser optics, 30-nm zone-plate optics, and a cryo sample chamber. We demonstrate 2D imaging of test patterns, and intact unstained yeast, protozoan parasites and mammalian cells. Overview 3D information is obtained by stereo imaging while complete 3D microscopy is provided by full tomographic reconstruction. The laboratory microscope image quality approaches that of the synchrotron microscopes, but with longer exposure times. The experimental image quality is analyzed from a numerical wave-propagation model of the imaging system and a path to reach synchrotron-like exposure times in laboratory microscopy is outlined. Copyright © 2011 Elsevier Inc. All rights reserved.

  2. Scanning electron microscopy/energy dispersive spectrometry fixedbeam or overscan x-ray microanalysis of particles can miss the real structure: x-ray spectrum image mapping reveals the true nature

    NASA Astrophysics Data System (ADS)

    Newbury, Dale E.; Ritchie, Nicholas W. M.

    2013-05-01

    The typical strategy for analysis of a microscopic particle by scanning electron microscopy/energy dispersive spectrometry x-ray microanalysis (SEM/EDS) is to use a fixed beam placed at the particle center or to continuously overscan to gather an "averaged" x-ray spectrum. While useful, such strategies inevitably concede any possibility of recognizing microstructure within the particle, and such fine scale structure is often critical for understanding the origins, behavior, and fate of particles. Elemental imaging by x-ray mapping has been a mainstay of SEM/EDS analytical practice for many years, but the time penalty associated with mapping with older EDS technology has discouraged its general use and reserved it more for detailed studies that justified the time investment. The emergence of the high throughput, high peak stability silicon drift detector (SDD-EDS) has enabled a more effective particle mapping strategy: "flash" x-ray spectrum image maps can now be recorded in seconds that capture the spatial distribution of major (concentration, C > 0.1 mass fraction) and minor (0.01 <= C <= 0.1) constituents. New SEM/SDD-EDS instrument configurations feature multiple SDDs that view the specimen from widely spaced azimuthal angles. Multiple, simultaneous measurements from different angles enable x-ray spectrometry and mapping that can minimize the strong geometric effects of particles. The NIST DTSA-II software engine is a powerful aid for quantitatively analyzing EDS spectra measured individually as well as for mapping information (available free for Java platforms at: http://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html).

  3. Gunshot residue testing in suicides: Part I: Analysis by scanning electron microscopy with energy-dispersive X-ray.

    PubMed

    Molina, D Kimberley; Martinez, Michael; Garcia, James; DiMaio, Vincent J M

    2007-09-01

    Several different methods can be employed to test for gunshot residue (GSR) on a deceased person's hands, including scanning electron microscopy with energy-dispersive x-ray spectroscopy (SEM-EDX) and inductively coupled plasma-atomic emission spectrometry (ICP-AES). Each of these techniques has been extensively studied, especially on living individuals. The current studies (Part I and Part II) were designed to compare the use and utility of the different GSR testing techniques in a medical examiner setting. In Part I, the hands of deceased persons who died from undisputed suicidal handgun wounds were tested for GSR by SEM-EDX over a 4-year period. A total of 116 cases were studied and analyzed for caliber of weapon, proximity of wound, and results of GSR testing, including spatial deposition upon the hands. It was found that in only 50% of cases with a known self-inflicted gunshot wound was SEM-EDX positive for at least 1 specific particle for GSR. In 18% of the cases there was a discernible pattern (spatial distribution) of the particles on the hand such that the manner in which the weapon was held could be determined. Since only 50% of cases where the person is known to have fired a weapon immediately prior to death were positive for GSR by SEM-EDX, this test should not be relied upon to determine whether a deceased individual has discharged a firearm. Furthermore, in only 18% of cases was a discernible pattern present indicating how the firearm was held. The low sensitivity, along with the low percentage of cases with a discernible pattern, limits the usefulness of GSR test results by SEM-EDX in differentiating self-inflicted from non-self-inflicted wounds.

  4. Recent case histories of food product-metal container interactions using scanning electron microscopy-x-ray microanalysis.

    PubMed

    Charbonneau, J E

    1997-10-01

    Scanning electron microscopy (SEM) and x-ray microanalysis (EDS) were used to investigate stress corrosion cracking (SCC) in plain tinplate food cans, product discoloration, filiform corrosion, pitting/perforation corrosion, and loss of coating adhesion in enameled food cans. Intergranular SCC of uncoated tinplate occurred in canned pineapple juice. This is a rare occurrence in acid food products. The fracture developed in the can headspace only at the product line/metal interface by an interaction of the detinned metal surface with stress-inducing compounds in the product. Black discoloration of rice granules in the can headspace of a chicken and rice product was caused by the formation of metal sulfides. The source of the metal contamination was traced to metallic dirt in the coating on the tin-free-steel end. Blackening of light tan-colored olives and brine occurred after 1 year of storage in enameled tinplate containers as a result of pitting corrosion at the side seam weld. The cause of the pitting was a defective side seam stripe which failed to protect the weld. A perforation problem occurred at the score line of aluminum-tinplate bimetallic cans. The failure was caused by the high chloride content of the fruit product. Filiform corrosion resulted in perforations that occurred on the outside surfaces of two-piece tin-free steel cans packed with tuna. The cause of the corrosion was related to scratch defects in the exterior coating and the presence of chloride and sulfate cannery residues in the corroded areas. An enamel adhesion failure developed inside two-piece tin-free steel cans that contained mushrooms. Wrinkles in the coating which were introduced during can manufacture were cracked. The fractures were pathways for product-steel interaction which resulted in container failure.

  5. Chemical elements characterization of root canal sealers using scanning electron microscopy and energy dispersive X-ray analysis.

    PubMed

    Sampaio, Felipe Cavalcanti; Alencar, Ana Helena Gonçalves; Guedes, Orlando Aguirre; Veloso, Heloisa Helena Pinho; Santos, Tatiane Oliveira; Estrela, Carlos

    2014-03-01

    The aim of this study was to evaluate the chemical elements composition of root canal filling materials using Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray analysis (EDX). Eighteen standard polyethylene tubes were filled with the following materials: Sealapex(®), Sealer 26(®), MTA Fillapex(®), Pulp Canal Sealer(®), Endofill(®) and AH Plus(®). After 48 hours at 37°C and 95% relative humidity, the samples were surface-sputtered with gold and analyzed using SEM at 5000X magnification. Their chemical composition and element distributionwere determined using EDX. Results were evaluated qualitatively (SEM images and elemental mapping) and quantitatively (weight percentage). Calcium oxide- and hydroxide-based sealers (Sealapex(®) and Sealer 26(®)) had calcium peaks of 53.58 wt% and 65.00 wt%. MTA Fillapex(®) had 30.58 wt% of calcium and high amounts of silicon (31.02 wt%) and bismuth (27.38 wt%). Zinc oxide- and eugenol-based sealers, Pulp Canal Sealer(®) and Endofill(®), had 67.74 wt% and 63.16 wt% of zinc each. AH Plus(®) had a higher amount of zirconium (64.24 wt%). All materials had elements other than those described by the manufacturers. Surface analysis using EDX revealed that regularity varied, element distribution was uniform, and particles had similar sizes and variable shapes. Most chemical elements were those described by the manufacturers, but percentages were different. The surface of root canal sealers had different regularity findings, uniform distribution and particles of similar sizes but variable shapes.

  6. Characterization of voids in shock-loaded Al single crystal by combining X-ray tomography and electron microscopy

    NASA Astrophysics Data System (ADS)

    Hong, Chuanshi; Fæster, Søren; Hansen, Niels; Huang, Xiaoxu; Barabash, Rozaliya I.

    2017-07-01

    A combination of X-ray tomography and electron backscatter diffraction (EBSD) was applied to investigate both the shape of voids and the plastic deformation around voids in an Al single crystal shock-loaded in the <1 2 3> direction. The combination of these two techniques allows the addition of crystallographic information to X-ray tomography and allows the addition of three-dimensional information to EBSD data. It is found that the voids are octahedral with {1 1 1} faces and that regular patterns of lattice reorientation exist around individual voids. The results provide new insights to the process of void growth during shock loading, which is important for both civil and military applications.

  7. Towards high-resolution ptychographic x-ray diffraction microscopy

    SciTech Connect

    Takahashi, Yukio; Suzuki, Akihiro; Yamauchi, Kazuto; Zettsu, Nobuyuki; Kohmura, Yoshiki; Ishikawa, Tetsuya; Senba, Yasunori; Ohashi, Haruhiko

    2011-06-01

    Ptychographic x-ray diffraction microscopy is a lensless imaging technique with a large field of view and high spatial resolution, which is also useful for characterizing the wavefront of an x-ray probe. The performance of this technique is degraded by positioning errors due to the drift between the sample and illumination optics. We propose an experimental approach for correcting the positioning errors and demonstrate success by two-dimensionally reconstructing both the wavefront of the focused x-ray beam and the complex transmissivity of the weakly scattering objects at the pixel resolution of better than 10 nm in the field of view larger than 5 {mu}m. This method is applicable to not only the observation of organelles inside cells or nano-mesoscale structures buried within bulk materials but also the characterization of probe for single-shot imaging with x-ray free electron lasers.

  8. Recent trends of projection X-ray microscopy in Japan

    NASA Astrophysics Data System (ADS)

    Yada, K.

    2009-08-01

    Recent activities of projection X-ray microscopy in Japan are reviewed. 1) By employing high brightness Schottky electron gun, resolution of 0.1 µm is realized by Tohken CO. group and some application examples are shown. 2) Deblurring of Fresnel diffracted image formed by synchrotron orbital radiation (SOR) X-rays is successfully tried by Chiba University group. Remarkable Fresnel fringes appearing at HeLa cell are mostly reconstructed by an iteration method. 3) Element analysis is carried out by Meiji University group utilizing absorption-edge characteristics between two kinds of X-ray targets without X-ray spectrometer. Actually, Cu and Ni targets are used with an inter-changeable system for elemental analysis of Fe 2O 3 particles and iron component in a mosquito larva.

  9. Structure of the Lassa virus nucleoprotein revealed by X-ray crystallography, small-angle X-ray scattering, and electron microscopy.

    PubMed

    Brunotte, Linda; Kerber, Romy; Shang, Weifeng; Hauer, Florian; Hass, Meike; Gabriel, Martin; Lelke, Michaela; Busch, Carola; Stark, Holger; Svergun, Dmitri I; Betzel, Christian; Perbandt, Markus; Günther, Stephan

    2011-11-04

    The nucleoprotein (NP) of Lassa virus (LASV) strain AV was expressed in a recombinant baculovirus system. The crystal structure of full-length NP was solved at a resolution of 2.45 Å. The overall fold corresponds to that of NP of LASV strain Josiah (Qi, X., Lan, S., Wang, W., Schelde, L. M., Dong, H., Wallat, G. D., Ly, H., Liang, Y., and Dong, C. (2010) Nature 468, 779-783) with a root mean square deviation of 0.67 Å for all atoms (6.3% difference in primary sequence). As the packing in the crystal offers two different trimer architectures for the biological assembly, the quaternary structure of NP in solution was determined by small-angle x-ray scattering and EM. After classification and averaging of >6000 EM raw images, trimeric centrosymmetric structures were obtained, which correspond in size and shape to one trimer in the crystal structure formed around a crystallographic 3-fold rotation axis (symmetric trimer). The symmetric trimer is also a good model for the small-angle x-ray scattering data and could be well embedded into the ab initio model. The N-terminal domain of NP contains a deep nucleotide-binding cavity that has been proposed to bind cellular cap structures for priming viral mRNA synthesis. All residues implicated in m(7)GpppN binding were exchanged, and the transcription/replication phenotype of the NP mutant was tested using a LASV replicon system. None of the mutants showed a specific defect in mRNA expression; most were globally defective in RNA synthesis. In conclusion, we describe the full-length crystal structure and the quaternary structure in solution of LASV NP. The nucleotide-binding pocket of NP could not be assigned a specific role in viral mRNA synthesis.

  10. Progress in high-resolution x-ray holographic microscopy

    SciTech Connect

    Jacobsen, C.; Kirz, J.; Howells, M.; McQuaid, K.; Rothman, S.; Feder, R.; Sayre, D.

    1987-07-01

    Among the various types of x-ray microscopes that have been demonstrated, the holographic microscope has had the largest gap between promise and performance. The difficulties of fabricating x-ray optical elements have led some to view holography as the most attractive method for obtaining the ultimate in high resolution x-ray micrographs; however, we know of no investigations prior to 1987 that clearly demonstrated submicron resolution in reconstructed images. Previous efforts suffered from problems such as limited resolution and dynamic range in the recording media, low coherent x-ray flux, and aberrations and diffraction limits in visible light reconstruction. We have addressed the recording limitations through the use of an undulator x-ray source and high-resolution photoresist recording media. For improved results in the readout and reconstruction steps, we have employed metal shadowing and transmission electron microscopy, along with numerical reconstruction techniques. We believe that this approach will allow holography to emerge as a practical method of high-resolution x-ray microscopy. 30 refs., 4 figs.

  11. Muscle cell membranes from early degeneration muscle cell fibers in Solenopsis are leaky to lanthanum: electron microscopy and X-ray analysis

    SciTech Connect

    Jones, R.G.; Davis, W.L.

    1985-06-01

    Lanthanum infusion techniques, transmission electron microscopy, and X-ray microanalysis were utilized to compare the permeability of muscle cell membranes from normal and degenerating muscle fibers of Solenopsis spp. In normal fibers, the electron-dense tracer was limited to components of the sarcotubular system. However, the insemination-induced degeneration of muscle fibers was characterized by the presence of an electron-dense precipitate within the myofibrils and mitochondria as well as in the extramyofibrillar spaces. The electron-dense material was subsequently identified by elemental analysis to be lanthanum. Such data indicate that one of the earliest stages of muscle degeneration involves an alteration in cell membrane permeability.

  12. Exploring nanomagnetism with soft x-ray microscopy

    SciTech Connect

    Fischer, P.; Kim, D.-H.; Mesler, B.L.; Chao, W.; Sakdinawat,A.E.; Anderson, E.H.

    2006-10-30

    Magnetic soft X-ray microscopy images magnetism in nanoscale systems with a spatial resolution down to 15nm provided by state-of-the-art Fresnel zone plate optics. X-ray magnetic circular dichroism (X-MCD) is used as element-specific magnetic contrast mechanism similar to photoemission electron microscopy (PEEM), however, with volume sensitivity and the ability to record the images in varying applied magnetic fields which allows to study magnetization reversal processes at fundamental length scales. Utilizing a stroboscopic pump-probe scheme one can investigate fast spin dynamics with a time resolution down to 70 ps which gives access to precessional and relaxation phenomena as well as spin torque driven domain wall dynamics in nanoscale systems. Current developments in zone plate optics aim for a spatial resolution towards 10nm and at next generation X-ray sources a time resolution in the fsec regime can be envisioned.

  13. Cryogenic coherent X-ray diffraction imaging of biological samples at SACLA: a correlative approach with cryo-electron and light microscopy.

    PubMed

    Takayama, Yuki; Yonekura, Koji

    2016-03-01

    Coherent X-ray diffraction imaging at cryogenic temperature (cryo-CXDI) allows the analysis of internal structures of unstained, non-crystalline, whole biological samples in micrometre to sub-micrometre dimensions. Targets include cells and cell organelles. This approach involves preparing frozen-hydrated samples under controlled humidity, transferring the samples to a cryo-stage inside a vacuum chamber of a diffractometer, and then exposing the samples to coherent X-rays. Since 2012, cryo-coherent diffraction imaging (CDI) experiments have been carried out with the X-ray free-electron laser (XFEL) at the SPring-8 Ångstrom Compact free-electron LAser (SACLA) facility in Japan. Complementary use of cryo-electron microscopy and/or light microscopy is highly beneficial for both pre-checking samples and studying the integrity or nature of the sample. This article reports the authors' experience in cryo-XFEL-CDI of biological cells and organelles at SACLA, and describes an attempt towards reliable and higher-resolution reconstructions, including signal enhancement with strong scatterers and Patterson-search phasing.

  14. Size dependent behavior of Fe3O4 crystals during electrochemical (de)lithiation: an in situ X-ray diffraction, ex situ X-ray absorption spectroscopy, transmission electron microscopy and theoretical investigation.

    PubMed

    Bock, David C; Pelliccione, Christopher J; Zhang, Wei; Timoshenko, Janis; Knehr, K W; West, Alan C; Wang, Feng; Li, Yan; Frenkel, Anatoly I; Takeuchi, Esther S; Takeuchi, Kenneth J; Marschilok, Amy C

    2017-08-09

    The iron oxide magnetite, Fe3O4, is a promising conversion type lithium ion battery anode material due to its high natural abundance, low cost and high theoretical capacity. While the close packing of ions in the inverse spinel structure of Fe3O4 enables high energy density, it also limits the kinetics of lithium ion diffusion in the material. Nanosizing of Fe3O4 to reduce the diffusion path length is an effective strategy for overcoming this issue and results in improved rate capability. However, the impact of nanosizing on the multiple structural transformations that occur during the electrochemical (de)lithiation reaction in Fe3O4 is poorly understood. In this study, the influence of crystallite size on the lithiation-conversion mechanisms in Fe3O4 is investigated using complementary X-ray techniques along with transmission electron microscopy (TEM) and continuum level simulations on electrodes of two different Fe3O4 crystallite sizes. In situ X-ray diffraction (XRD) measurements were utilized to track the changes to the crystalline phases during (de)lithiation. X-ray absorption spectroscopy (XAS) measurements at multiple points during the (de)lithiation processes provided local electronic and atomic structural information. Tracking the crystalline and nanocrystalline phases during the first (de)lithiation provides experimental evidence that (1) the lithiation mechanism is non-uniform and dependent on crystallite size, where increased Li(+) diffusion length in larger crystals results in conversion to Fe(0) metal while insertion of Li(+) into spinel-Fe3O4 is still occurring, and (2) the disorder and size of the Fe metal domains formed when either material is fully lithiated impacts the homogeneity of the FeO phase formed during the subsequent delithiation.

  15. Direct imaging of spin relaxation in stepped α-Fe2O3/Ni81Fe19 bilayers using x-ray photoemission electron microscopy

    NASA Astrophysics Data System (ADS)

    Bali, R.; Marchetto, H.; Barcza, A.; Blamire, M. G.; Dhesi, S. S.

    2012-07-01

    The magnetic domain structure of stepped ferromagnetic Ni81Fe19 films, exchange coupled to antiferromagnetic α-Fe2O3, has been studied using x-ray photoemission electron microscopy combined with x-ray magnetic circular dichroism. Annealing the α-Fe2O3/Ni81Fe19 bilayers in a magnetic field, applied parallel or perpendicular to the step edges, results in a significant increase in the domain size compared to the as-grown bilayer. Subsequent zero-field annealing induces spin-relaxation along the crystallographic axes of the α-Fe2O3. The spin-relaxation process is found to depend on the magnetic field direction during annealing with the domain structure determined by a competition between the step-induced uniaxial anisotropy and the exchange anisotropy.

  16. Stimulated Electronic X-Ray Raman Scattering

    NASA Astrophysics Data System (ADS)

    Weninger, Clemens; Purvis, Michael; Ryan, Duncan; London, Richard A.; Bozek, John D.; Bostedt, Christoph; Graf, Alexander; Brown, Gregory; Rocca, Jorge J.; Rohringer, Nina

    2013-12-01

    We demonstrate strong stimulated inelastic x-ray scattering by resonantly exciting a dense gas target of neon with femtosecond, high-intensity x-ray pulses from an x-ray free-electron laser (XFEL). A small number of lower energy XFEL seed photons drive an avalanche of stimulated resonant inelastic x-ray scattering processes that amplify the Raman scattering signal by several orders of magnitude until it reaches saturation. Despite the large overall spectral width, the internal spiky structure of the XFEL spectrum determines the energy resolution of the scattering process in a statistical sense. This is demonstrated by observing a stochastic line shift of the inelastically scattered x-ray radiation. In conjunction with statistical methods, XFELs can be used for stimulated resonant inelastic x-ray scattering, with spectral resolution smaller than the natural width of the core-excited, intermediate state.

  17. Stimulated electronic x-ray Raman scattering.

    PubMed

    Weninger, Clemens; Purvis, Michael; Ryan, Duncan; London, Richard A; Bozek, John D; Bostedt, Christoph; Graf, Alexander; Brown, Gregory; Rocca, Jorge J; Rohringer, Nina

    2013-12-06

    We demonstrate strong stimulated inelastic x-ray scattering by resonantly exciting a dense gas target of neon with femtosecond, high-intensity x-ray pulses from an x-ray free-electron laser (XFEL). A small number of lower energy XFEL seed photons drive an avalanche of stimulated resonant inelastic x-ray scattering processes that amplify the Raman scattering signal by several orders of magnitude until it reaches saturation. Despite the large overall spectral width, the internal spiky structure of the XFEL spectrum determines the energy resolution of the scattering process in a statistical sense. This is demonstrated by observing a stochastic line shift of the inelastically scattered x-ray radiation. In conjunction with statistical methods, XFELs can be used for stimulated resonant inelastic x-ray scattering, with spectral resolution smaller than the natural width of the core-excited, intermediate state.

  18. Cryotomography x-ray microscopy state

    SciTech Connect

    Le Gros, Mark; Larabell, Carolyn A.

    2010-10-26

    An x-ray microscope stage enables alignment of a sample about a rotation axis to enable three dimensional tomographic imaging of the sample using an x-ray microscope. A heat exchanger assembly provides cooled gas to a sample during x-ray microscopic imaging.

  19. X-ray microscopy of live biological micro-organisms

    NASA Astrophysics Data System (ADS)

    Raja Al-Ani, Ma'an Nassar

    Real-time, compact x-ray microscopy has the potential to benefit many scientific fields, including microbiology, pharmacology, organic chemistry, and physics. Single frame x-ray micro-radiography, produced by a compact, solid-state laser plasma source, allows scientists to use x-ray emission for elemental analysis, and to observe biological specimens in their natural state. In this study, x-ray images of mouse kidney tissue, live bacteria, Pseudomonas aeruginosa and Burkholderia cepacia, and the bacteria's interaction with the antibiotic gentamicin, are examined using x-ray microscopy. For the purposes of comparing between confocal microscopy and x-ray microscopy, we introduced to our work the technique of gold labeling. Indirect immunofluorescence staining and immuno-gold labeling were applied on human lymphocytes and human tumor cells. Differential interference contrast microscopy (DIC) showed the lymphocyte body and nucleus, as did x-ray microscopy. However, the high resolution of x-ray microscopy allows us to differentiate between the gold particles bound to the antibodies and the free gold. A compact, tabletop Nd: glass laser is used in this study to produce x-rays from an Yttrium target. An atomic force microscope is used to scan the x-ray images from the developed photo-resist. The use of compact, tabletop laser plasma sources, in conjunction with x-ray microscopy, is a new technique that has great potential as a flexible, user-friendly scientific research tool.

  20. Faradaurate-940: synthesis, mass spectrometry, electron microscopy, high-energy X-ray diffraction, and X-ray scattering study of Au∼940±20(SR)∼160±4 nanocrystals.

    PubMed

    Kumara, Chanaka; Zuo, Xiaobing; Cullen, David A; Dass, Amala

    2014-06-24

    Obtaining monodisperse nanocrystals and determining their composition to the atomic level and their atomic structure is highly desirable but is generally lacking. Here, we report the discovery and comprehensive characterization of a 2.9 nm plasmonic nanocrystal with a composition of Au940±20(SCH2CH2Ph)160±4, which is the largest mass spectrometrically characterized gold thiolate nanoparticle produced to date. The compositional assignment has been made using electrospray ionization and matrix-assisted laser desorption ionization mass spectrometry (MS). The MS results show an unprecedented size monodispersity, where the number of Au atoms varies by only 40 atoms (940 ± 20). The mass spectrometrically determined composition and size are supported by aberration-corrected scanning transmission electron microscopy (STEM) and synchrotron-based methods such as atomic pair distribution function (PDF) and small-angle X-ray scattering (SAXS). Lower-resolution STEM images show an ensemble of particles-1000s per frame-visually demonstrating monodispersity. Modeling of SAXS data on statistically significant nanoparticle population-approximately 10(12) individual nanoparticles-shows that the diameter is 3.0 ± 0.2 nm, supporting mass spectrometry and electron microscopy results on monodispersity. Atomic PDF based on high-energy X-ray diffraction experiments shows decent match with either a Marks decahedral or truncated octahedral structure. Atomic resolution STEM images of single particles and their fast Fourier transform suggest face-centered cubic arrangement. UV-visible spectroscopy data show that Faradaurate-940 supports a surface plasmon resonance peak at ̃505 nm. These monodisperse plasmonic nanoparticles minimize averaging effects and have potential application in solar cells, nano-optical devices, catalysis, and drug delivery.

  1. X-ray holographic microscopy: Improved images of zymogen granules

    SciTech Connect

    Jacobsen, C.; Howells, M.; Kirz, J.; McQuaid, K.; Rothman, S.

    1988-10-01

    Soft x-ray holography has long been considered as a technique for x-ray microscopy. It has been only recently, however, that sub-micron resolution has been obtained in x-ray holography. This paper will concentrate on recent progress we have made in obtaining reconstructed images of improved quality. 15 refs., 6 figs.

  2. Functional biocompatible magnetite-cellulose nanocomposite fibrous networks: Characterization by fourier transformed infrared spectroscopy, X-ray powder diffraction and field emission scanning electron microscopy analysis

    NASA Astrophysics Data System (ADS)

    Habibi, Neda

    2015-02-01

    The preparation and characterization of functional biocompatible magnetite-cellulose nano-composite fibrous material is described. Magnetite-cellulose nano-composite was prepared by a combination of the solution-based formation of magnetic nano-particles and subsequent coating with amino celluloses. Characterization was accomplished using X-ray powder diffraction (XRD), fourier transformed infrared (FTIR) and field emission scanning electron microscopy (FESEM) analysis. The peaks of Fe3O4 in the XRD pattern of nanocomposite confirm existence of the nanoparticles in the amino cellulose matrix. Magnetite-cellulose particles exhibit an average diameter of roughly 33 nm as demonstrated by field emission scanning electron microscopy. Magnetite nanoparticles were irregular spheres dispersed in the cellulose matrix. The vibration corresponding to the Nsbnd CH3 functional group about 2850 cm-1 is assigned in the FTIR spectra. Functionalized magnetite-cellulose nano-composite polymers have a potential range of application as targeted drug delivery system in biomedical field.

  3. Analysis of InGaN nanodots grown by droplet heteroepitaxy using grazing incidence small-angle X-ray scattering and electron microscopy

    NASA Astrophysics Data System (ADS)

    Woodward, J. M.; Nikiforov, A. Yu.; Ludwig, K. F.; Moustakas, T. D.

    2017-08-01

    We present a detailed structural investigation of self-assembled indium gallium nitride nanodots grown on c-plane aluminum nitride templates by the droplet heteroepitaxy technique in a plasma-assisted molecular beam epitaxy reactor. Various growth parameters, including the total coverage of the metal species, relative and total metal effusion fluxes, and nitridation temperature were investigated. Analyses of in situ reflection high-energy electron diffraction patterns and comparison with simulations showed that the resulting crystal structure was a mixture of wurtzite and twinned zinc blende phases, with the zinc blende phase increasingly dominant for lower metal coverages and lower nitridation temperatures, and the wurtzite phase increasingly dominant for higher nitridation temperature. Studies by field emission scanning electron microscopy and atomic force microscopy revealed that the nanodots exhibit trimodal size distributions, with the dot morphologies of the intermediate size mode often resembling aggregations of distinct clusters. Nanodots grown at higher nitridation temperatures had larger inter-dot spacings, with hexagonal in-plane ordering observable at a sufficiently high temperature. Using grazing incidence small angle X-ray scattering, we determined the nanodots to be approximately truncated cone shaped, and extracted the mean radius, height, and inter-dot distance for each distribution. Microstructural investigations of the nanodots by cross-sectional transmission electron microscopy indicated that the majority of the dots were formed in dislocation-free regions, and confirmed that the intermediate size dots were approximately truncated cone shaped and consisted of both zinc blende and wurtzite regions. Mapping of the elemental distributions by energy dispersive X-ray spectroscopy in scanning transmission electron microscopy mode indicated highly nonuniform indium distributions within both small and intermediate size dots which are potentially

  4. Green synthesis and characterization of Carica papaya leaf extract coated silver nanoparticles through X-ray diffraction, electron microscopy and evaluation of bactericidal properties.

    PubMed

    Banala, Rajkiran Reddy; Nagati, Veera Babu; Karnati, Pratap Reddy

    2015-09-01

    The evolution of nanotechnology and the production of nanomedicine from various sources had proven to be of intense value in the field of biomedicine. The smaller size of nanoparticles is gaining importance in research for the treatment of various diseases. Moreover the production of nanoparticles is eco-friendly and cost effective. In the present study silver nanoparticles were synthesized from Carica papaya leaf extract (CPL) and characterized for their size and shape using scanning electron microscopy and transmission electron microscopy, respectively. Fourier transform infrared spectroscopy (FTIR), Energy dispersive X-ray spectroscopy (EDS/EDX) and X-ray diffraction spectroscopy (XRD) were conducted to determine the concentration of metal ions, the shape of molecules. The bactericidal activity was evaluated using Luria Bertani broth cultures and the minimum inhibition concentration (MIC) and minimum bactericidal concentration (MBC) were estimated using turbidimetry. The data analysis showed size of 50-250 nm spherical shaped nanoparticles. The turbidimetry analysis showed MIC and MBC was >25 μg/mL against both Gram positive and Gram negative bacteria in Luria Bertani broth cultures. In summary the synthesized silver nanoparticles from CPL showed acceptable size and shape of nanoparticles and effective bactericidal activity.

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

    DOE PAGES

    Ajo, Henry; Blankenship, Donnie; Clark, Elliot

    2014-07-25

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

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

    SciTech Connect

    Ajo, Henry; Blankenship, Donnie; Clark, Elliot

    2014-07-25

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

  7. Soft x-ray holography and microscopy of biological cells

    NASA Astrophysics Data System (ADS)

    Chen, Jianwen; Gao, Hongyi; Xie, Honglan; Li, Ruxin; Xu, Zhizhan

    2003-10-01

    Some experimental results on soft X-ray microscopy and holography imaging of biological specimens are presented in the paper. As we know, due to diffraction effects, there exists a resolution limit determined by wavelength λ and numerical aperture NA in conventional optical microscopy. In order to improve resolution, the num erical aperture should be made as large as possible and the wavelength as short as possible. Owing to the shorter wavelength, X-rays provide the potential of higher resolution in X-ray microscopy, holography image and allow for exam ination the interior structures of thicker specimens. In the experiments, we used synchrotron radiation source in Hefei as light source. Soft X-rays come from a bending magnet in 800 M eV electron storage ring with characteristic wavelength of 2.4 nm. The continuous X-ray spectrums are monochromatized by a zone-plate and a pinhole with 300 m diameter. The experimental set-up is typical contact microscopic system, its main advantage is simplicity and no special optical element is needed. The specimens used in the experiments of microscopic imaging are the colibacillus, the gingko vascular hundle and the fritillaries ovary karyon. The specimen for holographic imaging is the spider filam ents. The basic structures of plant cells such as the cell walls, the cytoplasm and the karyon especially the joint structures between the cells are observed clearly. An experimental study on a thick biological specimen that is a whole sporule w ith the thickness of about 30 μm is performed. In the holographic experiments, the experimental setup is typical Gabor in-line holography. The specimen is placed in line with X-ray source, which provides both the reference w aves and specimen illum ination. The specimen is some spider filament, which adhere to a Si3N4 film. The recording medium is PM M A, which is placed at recording distance of about 400 μm from the specimen. The hologram s were reconstructed by digital method with 300 nm

  8. Transmission Electron Microscopy and Scanning Transmission X-Ray Microscopy Studies on the Bioaccumulation and Tissue Level Absorption of TiO2 Nanoparticles in Daphnia magna.

    PubMed

    Kwon, Dongwook; Nho, Hyun Woo; Yoon, Tae Hyun

    2015-06-01

    In this study, bioaccumulation and tissue-level absorption of TiO2 nanoparticles (NPs) in freshwater invertebrates were investigated using transmission electron microscopy (TEM) and scanning transmission X-ray microscopy (STXM). The TiO2 NPs were used to test impacts of core sizes (i.e., 5 ± 2 nm and 23 ± 7 nm for TiO2(SYN) and TiO2(P25), respectively) and agglomerations (i.e., well dispersed vs. highly agglomerated) on the uptake of TiO2 NPs in Daphnia magna (D. magna). Highly agglomerated TiO2 NPs, regardless of their core sizes, were heavily taken up into the digestive tract of D. magna and no detectable penetration of both TiO2 NPs into the gut epithelial cells of D. magna was observed in TEM and STXM images. However, significant damages involving morphological changes in the microvilli and gut epithelial cells (e.g., irregular shaped microvilli, epithelial cell protrusion, and dilatation of cytoplasmic inclusion) were observed only with the commercial TiO2 NPs (TiO2(P25)) with larger core size and mixed crystalline phase, while the laboratory synthesized TiO2 NPs (TiO2(Syn)) with smaller core size and single crystalline phase showed slight morphological changes in the gut microvilli and epithelial cells. In the case of D. magna exposed to the well dispersed synthetic TiO2 NP ((Cit)TiO2(Syn)), only a negligible amount of TiO2 NPs were found within the digestive tract of the D. magna without any significant damages in the gut microvilli and epithelial cells and any detectable penetrations of TiO2 NPs into epithelial cells of D. magna gut. These TEM and STXM observations confirmed us that uptake of NP into D. magna are strongly dependent on their agglomeration (i.e., hydrodynamic sizes), rather than their core sizes, while direct penetration of NPs into tissues of digestive tract seems unlikely without significant morphological changes (e.g., collapse of the epithelial tissue) caused by high toxicity of NPs or released metal ions.

  9. Find your way with X-Ray: Using microCT to correlate in vivo imaging with 3D electron microscopy.

    PubMed

    Karreman, Matthia A; Ruthensteiner, Bernhard; Mercier, Luc; Schieber, Nicole L; Solecki, Gergely; Winkler, Frank; Goetz, Jacky G; Schwab, Yannick

    2017-01-01

    Combining in vivo imaging with electron microscopy (EM) uniquely allows monitoring rare and critical events in living tissue, followed by their high-resolution visualization in their native context. A major hurdle, however, is to keep track of the region of interest (ROI) when moving from intravital microscopy (IVM) to EM. Here, we present a workflow that relies on correlating IVM and microscopic X-ray computed tomography to predict the position of the ROI inside the EM-processed sample. The ROI can then be accurately and quickly targeted using ultramicrotomy and imaged using EM. We outline how this procedure is used to retrieve and image tumor cells arrested in the vasculature of the mouse brain. Copyright © 2017 Elsevier Inc. All rights reserved.

  10. Innovative analytical methodology combining micro-x-ray diffraction, scanning electron microscopy-based mineral maps, and diffuse reflectance infrared fourier transform spectroscopy to characterize archeological artifacts.

    PubMed

    Cardell, Carolina; Guerra, Isabel; Romero-Pastor, Julia; Cultrone, Giuseppe; Rodriguez-Navarro, Alejandro

    2009-01-15

    Excavations at the 14th century Moorish rampart (Granada, Spain) unearthed a brick oven alongside black ash and bone stratigraphic layers. In situ evidence suggests the oven served to fabricate a wall coating including powdered burnt bones. Original ad hoc analyses improved on conventional methods were used to confirm this hypothesis. These methods enable (i) nondestructive micro-X-ray diffraction (mu-XRD) for fast mineralogical data acquisition (approximately 10 s) and moderately high spatial (approximately 500 microm) resolution and (ii) identification and imaging of crystalline components in sample cross-sections via mineral maps, yielding outstanding visualization of grain distribution and morphology in composite samples based on scanning electron microscopy-energy dispersion X-ray spectrometry (SEM-EDX) elemental maps. Benefits are shown for applying diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) vs transmittance-FT-IR (T-FT-IR) to analyze organic and inorganic components in single samples. Complementary techniques to fully characterize artifacts were gas chromatography/mass spectroscopy (GC/MS), optical microscopy (OM), conventional powder XRD, and (14)C dating. Bone-hydroxyapatite was detected in the coating. Mineralogical transformations in the bricks indicate oven temperatures well above 1000 degrees C, supporting the hypothesis.

  11. Characterization of the nonlamellar cubic and HII structures of lipid A from Salmonella enterica serovar Minnesota by X-ray diffraction and freeze-fracture electron microscopy.

    PubMed

    Brandenburg, K; Richter, W; Koch, M H; Meyer, H W; Seydel, U

    1998-01-01

    The aggregate structures of lipid A, the 'endotoxic principle' of bacterial lipopolysaccharide (LPS), from rough mutant Salmonella enterica sv. Minnesota R595 was analyzed at different water content, cation (Mg2+) concentration, and temperature applying synchrotron radiation X-ray diffraction and, in selected cases, freeze-fracture electron microscopy. The X-ray diffraction spectra prove the existence of different lamellar, mixed lamellar/cubic, various cubic, and inverted hexagonal (HII) structures depending on ambient conditions. The three mainly bicontinuous cubic phases Q224, Q229, and Q230 can be observed between 30 and 50 degrees C in narrow water and cation concentration ranges. Above 50 degrees C, Q212 an intermediate phase between bicontinuous and micellar is adopted. In freeze-fracture electron microscopic experiments, cubic structures of these symmetries are not readily detected, which can be understood in the light of changes in hydration during freezing and the metastability of these phases. However, 'lipidic particles' closely related to cubic phases are observed. Above 65-70 degrees C, the existence of the HII phase with hexagonal periodicities dH between 4.0 and 6.0 nm for different hydration states is shown using both techniques. Possible biological implications for the preference of lipid A for nonlamellar structures are discussed.

  12. Exceptional case of bone resorption in an osteo-odonto-keratoprosthesis. A scanning electron microscopy and X-ray microanalysis study

    SciTech Connect

    Caiazza, S.; Falcinelli, G.; Pintucci, S. )

    1990-01-01

    This article reports the findings of investigations on an osteo-odonto-keratoprosthesis in an eye that was enucleated owing to severe complications 12 years after implantation. Scanning electron microscopy and electron probe X-ray microanalysis showed extensive resorption of the bone that was used as a supporting element in the kind of transcorneal prosthesis developed by Strampelli. The destructive process, in addition to surgical trauma, has been associated with the early and recurrent bacterial infections relating to the presence of Staphylococcus epidermidis. The need to control the occurrence of primary bacterial infections in traumatized tissues during operations as well as further infectious situations, given the enhanced antibiotic-resistence of bacteria, is emphasized.

  13. Imaging bacterial spores by soft-x-ray microscopy

    SciTech Connect

    Stead, A.D.; Ford, T.W.; Judge, J.

    1997-04-01

    Bacterial spores are able to survive dehydration, but neither the physiological nor structural basis of this have been fully elucidated. Furthermore, once hydrated, spores often require activation before they will germinate. Several treatments can be used to activate spores, but in the case of Bacillus subtlis the most effective is heat treatment. The physiological mechanism associated with activation is also not understood, but some workers suggest that the loss of calcium from the spores may be critical. However, just prior to germination, the spores change from being phase bright to phase dark when viewed by light microscopy. Imaging spores by soft x-ray microscopy is possible without fixation. Thus, in contrast to electron microscopy, it is possible to compare the structure of dehydrated and hydrated spores in a manner not possible previously. A further advantage is that it is possible to monitor individual spores by phase contrast light microscopy immediately prior to imaging with soft x-rays; whereas, with both electron microscopy and biochemical studies, it is a population of spores being studied without knowledge of the phase characteristics of individual spores. This study has therefore tried to compare dehydrated and hydrated spores and to determine if there is a mass loss from individual spores as they pass the transition from being phase bright to phase dark.

  14. Characterization of individual submicrometer aerosol particles collected in Incheon, Korea, by quantitative transmission electron microscopy energy-dispersive X-ray spectrometry

    NASA Astrophysics Data System (ADS)

    Geng, Hong; Kang, Sujin; Jung, Hae-Jin; ChoëL, Marie; Kim, Hyekyeong; Ro, Chul-Un

    2010-08-01

    For the last decade the Monte Carlo calculation method has been proven to be an excellent tool for accurately simulating electron-solid interactions in atmospheric individual particles of micrometer size. Although it was designed for application to scanning electron microscopy, in the present study it is demonstrated that the Monte Carlo calculation can also be applied in a quantitative single particle analysis using transmission electron microscopy (TEM) with an ultrathin window energy-dispersive X-ray (EDX) spectrometer with a high accelerating voltage (200 kV). By utilizing an iterative reverse Monte Carlo simulation combined with successive approximation, atomic elemental concentrations (including low-Z elements) of submicrometer standard particles were determined with high accuracy for electron beam refractory particles such as NaCl, KCl, SiO2, Fe2O3, Na2SO4, K2SO4, CaCO3, and CaSO4. On the basis of quantitative X-ray analysis together with morphological information from TEM images, overall 1638 submicrometer individual particles from 10 sets of aerosol samples collected in Incheon, Korea, were identified. The most frequently encountered particle types are carbonaceous and (NH4)2SO4/NH4HSO4-containing particles, followed by mineral (e.g., aluminosilicate, SiO2, CaCO3), sea salt, K-rich (e.g., K2SO4 and KCl), Fe-rich, fly ash, and transition or heavy-metal-containing (e.g., ZnSO4, ZnCl2, PbSO4) particles. The relative abundances of the submicrometer particle types vary among samples collected in different seasons and also depend on different air mass transport routes. This study demonstrates that the quantitative TEM-EDX individual particle analysis is a useful and reliable technique in characterizing urban submicrometer aerosol particles.

  15. Effect of bleaching agents having a neutral pH on the surface of mineral trioxide aggregate using electron microscopy and energy dispersive X-ray microanalysis

    PubMed Central

    Kazia, Nooh; Suvarna, Nithin; Shetty, Harish Kumar; Kumar, Pradeep

    2016-01-01

    Aim: To investigate the effect of bleaching agents having a neutral pH on the surface of mineral trioxide aggregate (MTA) used as a coronal seal material for nonvital bleaching, beneath the bleaching agent, with the help of energy dispersive X-ray microanalysis and scanning electron microscopy (SEM). Materials and Methods: Six samples of plastic tubes filled with white MTA (Angelus white) were kept in 100% humidity for 21 days. Each sample was divided into 2 and made into 12 samples. These were then divided into three groups. Group A was exposed to Opalescence Boost 40% hydrogen peroxide (HP) (Ultradent). Group B to Opalescence 10% carbamide peroxide (Ultradent) and Group C (control group) not exposed to any bleaching agent. After recommended period of exposure to bleaching agents according to manufacturers’ instructions, the samples were observed under SEM with an energy dispersive X-ray microanalysis system (JSM-6380 LA). Results: There were no relevant changes in color and no statistically significant surface structure changes of the MTA in both the experimental groups. Conclusion: The present findings suggest that even high concentration HP containing bleaching agents with neutral pH can be used on the surface of MTA without causing structural changes. The superior sealing ability of MTA and the high alkalinity would prevent cervical resorption postbleaching. PMID:27656061

  16. Structure and Composition of Isolated Core-Shell (In ,Ga )N /GaN Rods Based on Nanofocus X-Ray Diffraction and Scanning Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    Krause, Thilo; Hanke, Michael; Nicolai, Lars; Cheng, Zongzhe; Niehle, Michael; Trampert, Achim; Kahnt, Maik; Falkenberg, Gerald; Schroer, Christian G.; Hartmann, Jana; Zhou, Hao; Wehmann, Hergo-Heinrich; Waag, Andreas

    2017-02-01

    Nanofocus x-ray diffraction is used to investigate the structure and local strain field of an isolated (In ,Ga )N /GaN core-shell microrod. Because the high spatial resolution of the x-ray beam is only 80 ×90 nm2, we are able to investigate several distinct volumes on one individual side facet. Here, we find a drastic increase in thickness of the outer GaN shell along the rod height. Additionally, we performed high-angle annular dark-field scanning-transmission-electron-microscopy measurements on several rods from the same sample showing that (In,Ga)N double-quantum-well and GaN barrier thicknesses also increase strongly along the height. Moreover, plastic relaxation is observed in the top part of the rod. Based on the experimentally obtained structural parameters, we simulate the strain-induced deformation using the finite-element method, which serves as the input for subsequent kinematic scattering simulations. The simulations reveal a significant increase of elastic in-plane relaxation along the rod height. However, at a certain height, the occurrence of plastic relaxation yields a decrease of the elastic strain. Because of the experimentally obtained structural input for the finite-element simulations, we can exclude unknown structural influences on the strain distribution, and we are able to translate the elastic relaxation into an indium concentration which increases by a factor of 4 from the bottom to the height where plastic relaxation occurs.

  17. Direct comparison between X-ray nanotomography and scanning electron microscopy for the microstructure characterization of a solid oxide fuel cell anode

    SciTech Connect

    Quey, R.; Suhonen, H.; Laurencin, J.; Cloetens, P.; Bleuet, P.

    2013-04-15

    X-ray computed nanotomography (nano-CT) and scanning electron microscopy (SEM) have been applied to characterize the microstructure of a Solid Oxide Fuel Cell (SOFC) anode. A direct comparison between the results of both methods is conducted on the same region of the microstructure to assess the spatial resolution of the nano-CT microstructure, SEM being taken as a reference. A registration procedure is proposed to find out the position of the SEM image within the nano-CT volume. It involves a second SEM observation, which is taken along an orthogonal direction and gives an estimate reference SEM image position, which is then refined by an automated optimization procedure. This enables an unbiased comparison between the cell porosity morphologies provided by both methods. In the present experiment, nano-CT is shown to underestimate the number of pores smaller than 1 μm and overestimate the size of the pores larger than 1.5 μm. - Highlights: ► X-ray computed nanotomography (nano-CT) and SEM are used to characterize an SOFC anode. ► A methodology is proposed to compare the nano-CT and SEM data on the same region. ► The spatial resolution of the nano-CT data is assessed from that comparison.

  18. A simple method for detection of gunshot residue particles from hands, hair, face, and clothing using scanning electron microscopy/wavelength dispersive X-ray (SEM/WDX).

    PubMed

    Kage, S; Kudo, K; Kaizoji, A; Ryumoto, J; Ikeda, H; Ikeda, N

    2001-07-01

    We devised a simple and rapid method for detection of gunshot residue (GSR) particles, using scanning electron microscopy/wavelength dispersive X-ray (SEM/WDX) analysis. Experiments were done on samples containing GSR particles obtained from hands, hair, face, and clothing, using double-sided adhesive coated aluminum stubs (tape-lift method). SEM/WDX analyses for GSR were carried out in three steps: the first step was map analysis for barium (Ba) to search for GSR particles from lead styphnate primed ammunition, or tin (Sn) to search for GSR particles from mercury fulminate primed ammunition. The second step was determination of the location of GSR particles by X-ray imaging of Ba or Sn at a magnification of x 1000-2000 in the SEM, using data of map analysis, and the third step was identification of GSR particles, using WDX spectrometers. Analysis of samples from each primer of a stub took about 3 h. Practical applications were shown for utility of this method.

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

    NASA Astrophysics Data System (ADS)

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

    2013-01-01

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

  20. Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by charge flipping method

    SciTech Connect

    Chinthaka Silva, G.W.; Kercher, Andrew A.; Hunn, John D.; Martin, Rodger C.; Jellison, Gerald E.; Meyer, Harry M.

    2012-10-15

    Samples with five different zirconium carbide compositions (C/Zr molar ratio=0.84, 0.89, 0.95, 1.05, and 1.17) have been fabricated and studied using a variety of experimental techniques. Each sample was zone refined to ensure that the end product was polycrystalline with a grain size of 10-100 {mu}m. It was found that the lattice parameter was largest for the x=0.89 composition and smallest for the x=1.17 total C/Zr composition, but was not linear; this nonlinearity is possibly explained using electron densities calculated using charge flipping technique. Among the five samples, the unit cell of the ZrC{sub 0.89} sample showed the highest electron density, corresponding to the highest carbon incorporation and the largest lattice parameter. The ZrC{sub 0.84} sample showed the lowest carbon incorporation, resulting in a larger number of carbon vacancies and resultant strain. Samples with larger carbon ratios (x=0.95, 1.05, and 1.17) showed a slight decrease in lattice parameter, due to a decrease in electron density. Optical anisotropy measurements suggest that these three samples contained significant amounts of a graphitic carbon phase, not bonded to the Zr atoms. - Graphical abstract: Characterization of zirconium carbides using electron microscopy, optical anisotropy, Auger depth profiles, X-ray diffraction, and electron density calculated by the charge flipping method. Highlights: Black-Right-Pointing-Pointer The lattice parameter variation: ZrC{sub 0.89}>ZrC{sub 0.84}>ZrC{sub 0.95}>ZrC{sub 1.05}>ZrC{sub 1.17}. Black-Right-Pointing-Pointer Surface oxygen with no correlation to the lattice parameter variation. Black-Right-Pointing-Pointer ZrC{sub 0.89} had highest electron densities correspond to highest carbon incorporation. Black-Right-Pointing-Pointer Second highest lattice parameter in ZrC{sub 0.84} due to strain. Black-Right-Pointing-Pointer Unit cell electron density order: ZrC{sub 0.95}>ZrC{sub 1.05}>ZrC{sub 1.17}.

  1. Dislocation Substructure in the Cold-Rolled Ni-20 Mass Pct Cr Alloy Analyzed by X-ray Diffraction, Positron Annihilation Lifetime, and Transmission Electron Microscopy

    NASA Astrophysics Data System (ADS)

    Yonemura, Mitsuharu; Inoue, Koji

    2016-12-01

    The systematic change in the dislocation density and characteristics that develop under cold rolling as a simulated deformation was studied in order to examine the fundamental behavior of dislocations in terms of the dislocation substructure formation. In particular, the dislocation density was quantified by X-ray line profile analysis (XLPA), which is effective for quantifying the dislocation density and character; positron annihilation lifetime (PAL), which is sensitive to vacancy-type lattice defects; the Bailey-Hirsch equation from the hardness (Hv); and transmission electron microscopy (TEM). The strain dependency of the dislocation density analyzed by XLPA, PAL, TEM, and Hv showed a similar tendency with an increase in the dislocation. In particular, the dislocation density by XLPA had good agreement with the results of TEM at low strain levels and with PAL at high strain levels. As a result, a combination of these techniques successfully showed the behavior of the dislocation substructure.

  2. Nanometer-scale, quantitative composition mappings of InGaN layers from a combination of scanning transmission electron microscopy and energy dispersive x-ray spectroscopy.

    PubMed

    Pantzas, K; Patriarche, G; Troadec, D; Gautier, S; Moudakir, T; Suresh, S; Largeau, L; Mauguin, O; Voss, P L; Ougazzaden, A

    2012-11-16

    Using elastic scattering theory we show that a small set of energy dispersive x-ray spectroscopy (EDX) measurements is sufficient to experimentally evaluate the scattering function of electrons in high-angle annular dark field scanning transmission microscopy (HAADF-STEM). We then demonstrate how to use this function to transform qualitative HAADF-STEM images of InGaN layers into precise, quantitative chemical maps of the indium composition. The maps obtained in this way combine the resolution of HAADF-STEM and the chemical precision of EDX. We illustrate the potential of such chemical maps by using them to investigate nanometer-scale fluctuations in the indium composition and their impact on the growth of epitaxial InGaN layers.

  3. Microstructural changes in CdSe-coated ZnO nanowires evaluated by in situ annealing in transmission electron microscopy and x-ray diffraction.

    PubMed

    Majidi, Hasti; Winkler, Christopher R; Taheri, Mitra L; Baxter, Jason B

    2012-07-05

    We report on the crystallite growth and phase change of electrodeposited CdSe coatings on ZnO nanowires during annealing. Both in situ transmission electron microscopy (TEM) and x-ray diffraction (XRD) reveal that the nanocrystal size increases from ∼3 to ∼10 nm upon annealing at 350 °C for 1 h and then to more than 30 nm during another 1 h at 400 °C, exhibiting two distinct growth regimes. Nanocrystal growth occurs together with a structural change from zinc blende to wurtzite. The structural transition begins at 350 °C, which results in the formation of stacking faults. Increased crystallite size, comparable to the coating thickness, can improve charge separation in extremely thin absorber solar cells. We demonstrate a nearly two-fold improvement in power conversion efficiency upon annealing.

  4. X-ray and transmission electron microscopy characterization of twinned CdO thin films grown on a-plane sapphire by metalorganic vapour phase epitaxy

    NASA Astrophysics Data System (ADS)

    Martínez-Tomás, M. C.; Zúñiga-Pérez, J.; Vennéguès, P.; Tottereau, O.; Muñoz-Sanjosé, V.

    2007-07-01

    In the frame of studying II VI oxides of interest in optoelectronic technologies, the structural properties of CdO films grown by metalorganic vapour phase epitaxy on a-plane sapphire substrates have been analysed. The study has been performed by means of X-ray diffraction and cross-sectional transmission electron microscopy measurements. CdO films have been found to grow along [111] with the presence of twinned domains. Asymmetrical reflections have been used to study the crystalline quality of the twinned domains, independent of each other, as well as to determine their relative population. The analysis has been made as a function of growth conditions: VI/II precursors molar ratio and growth temperature.

  5. Remineralization of demineralized enamel by toothpastes: a scanning electron microscopy, energy dispersive X-ray analysis, and three-dimensional stereo-micrographic study.

    PubMed

    Gjorgievska, Elizabeta S; Nicholson, John W; Slipper, Ian J; Stevanovic, Marija M

    2013-06-01

    Remineralization of hard dental tissues is thought to be a tool that could close the gap between prevention and surgical procedures in clinical dentistry. The purpose of this study was to examine the remineralizing potential of different toothpaste formulations: toothpastes containing bioactive glass, hydroxyapatite, or strontium acetate with fluoride, when applied to demineralized enamel. Results obtained by scanning electron microscopy (SEM) and SEM/energy dispersive X-ray analyses proved that the hydroxyapatite and bioactive glass-containing toothpastes were highly efficient in promoting enamel remineralization by formation of deposits and a protective layer on the surface of the demineralized enamel, whereas the toothpaste containing 8% strontium acetate and 1040 ppm fluoride as NaF had little, if any, remineralization potential. In conclusion, the treatment of demineralized teeth with toothpastes containing hydroxyapatite or bioactive glass resulted in repair of the damaged tissue.

  6. Intact αIIbβ3 Integrin Is Extended after Activation as Measured by Solution X-ray Scattering and Electron Microscopy*

    PubMed Central

    Eng, Edward T.; Smagghe, Benoit J.; Walz, Thomas; Springer, Timothy A.

    2011-01-01

    Integrins are bidirectional signaling molecules on the cell surface that have fundamental roles in regulating cell behavior and contribute to cell migration and adhesion. Understanding of the mechanism of integrin signaling and activation has been advanced with truncated ectodomain preparations; however, the nature of conformational change in the full-length intact integrin molecule remains an active area of research. Here we used small angle x-ray scattering and electron microscopy to study detergent-solubilized, intact platelet integrin αIIbβ3. In the resting state, the intact αIIbβ3 adopted a compact, bent conformation. Upon activation with Mn2+, the average integrin extension increased. Further activation by addition of ligand led to stabilization of the extended state and opening of the headpiece. The observed extension and conformational rearrangement upon activation are consistent with the extension and headpiece opening model of integrin activation. PMID:21832081

  7. Assessment of in vitro binding of isolated pectic domains to cellulose by adsorption isotherms, electron microscopy, and X-ray diffraction methods.

    PubMed

    Zykwinska, Agata; Gaillard, Cédric; Buléon, Alain; Pontoire, Bruno; Garnier, Catherine; Thibault, Jean-François; Ralet, Marie-Christine

    2007-01-01

    Isolated pectic domains representative of the pectic backbone and the neutral sugar side chains were tested for their ability to interact with cellulose in comparison to the well-known binding of xyloglucan. Pectic side chains displayed a significant in vitro binding capacity to cellulose, whereas pectic backbone domains exhibited only slight adsorption to cellulose microfibrils. To support the binding results, electron microscopy and X-ray diffraction were applied. Celluloses from bacteria and sugar beet cell walls were used as substrates for the precipitation of isolated pectic domains or xyloglucan by acetone vapor diffusion. Pectic side chains grew attached to the cellulose surfaces, whereas pectic backbone domains were observed separately from cellulose microfibrils. Xyloglucan seeded with cellulose provoked a decrease of microfibrils entanglement, but no clear cross-links between neighboring microfibrils were observed. These results led to the elucidation of the pectic domains responsible for binding with cellulose microfibrils.

  8. X-ray absorption measurement by scanning capacitance microscopy

    NASA Astrophysics Data System (ADS)

    Ishii, Masashi; Uchihashi, Takayuki

    2003-12-01

    This paper describes a demonstration of scanning capacitance microscopy (SCM) as a technique for measuring X-ray absorption fine structure (XAFS) in what is called the SCM-XAFS method. This method achieves the simultaneous analysis of the electrical and chemical characteristics of surface-trapping centers. In obtaining the XAFS spectrum of trapping centers, the method takes advantage of the fact that the X-ray-induced photoemission of a localized electron leads to a change in capacitance. When the Fermi level corresponds to the trapping level, the photoemission process is sensitively detected. Therefore, a specific trapping center may be selectively observed by controlling the bias. From SCM-XAFS measurements of a GaAs surface, we found that gallium oxide trapping centers capture electrons in the positive bias voltage region. Moreover, experimental findings that resonant intra-transition and resonant scattering of emitted photoelectrons enhance the SCM-XAFS signal at particular X-ray photon energy reveal the local density of states of the gallium oxide and the complex structure of the trapping centers.

  9. Electron microscopy, micro-analysis, and X-ray diffraction characterization of the mineral-like tissue deposited by human cementum tumor-derived cells.

    PubMed

    Arzate, H; Alvarez-Pérez, M A; Alvarez-Fregoso, O; Wusterhaus-Chávez, A; Reyes-Gasga, J; Ximénez-Fyvie, L A

    2000-01-01

    The nature and characteristics of the mineralized-like tissue deposited by cementoblasts are not well-known due to the difficulties in obtaining and culturing cells representing the cementum phenotype. We hypothesized that a putative cementoblastic cell line derived from a human cementoblastoma could serve as a suitable model to study the physical, chemical, and morphological features of the cementum-like tissue deposited in vitro. The cementoblastoma cell line was studied by transmission electron, high resolution, scanning, and atomic force microscopy and compared with human cellular cementum, human osteoblasts, and human alveolar bone. The analyses of the crystals and mineral-like tissue in the cell line were performed by x-ray diffraction microscopy and energy-dispersive x-ray micro-analysis. TEM examination of cementoblastoma cells revealed the presence of electron-dense intracellular vesicles surrounded by a membrane that contained filaments and needle-like structures. The diffraction patterns obtained from the intracellular material and human cellular cementum were similar, with D-spacings of 3.36 and 2.8, consistent with those of hydroxyapatite (3.440 and 2.814). The composition of the mineral-like tissue had a Ca/P ratio of 1.60 for cementoblastoma cells and 1.97 for human cellular cementum. Na (5.29%) and Cl (1.47%) were present in the composition of cementoblastoma cells. Human cellular cementum additionally contained Mg (4.95%). Osteoblastic cells showed a Ca/P ratio of 1.6280. Na represented 4.52% and Cl 1.22% of its composition. Human alveolar bone had a Ca/P ratio value of 2.01. Na (6.63%), Mg (2.10%), and Cl (0.84%) were also present. All samples examined represented biological-type hydroxyapatite. Based on the compositional and morphological features, these findings indicate that cementoblastoma-derived cells express the human cellular cementum phenotype.

  10. Hard x-ray Zernike microscopy reaches 30 nm resolution.

    SciTech Connect

    Chen, Y.; Chen, T.; Yi, J.; Chu, Y.; Lee, W.-K.; Wang, C.; Kempson, I.; Hwu, Y.; Gajdosik, V.; Margaritondo, G.

    2011-03-30

    Since its invention in 1930, Zernike phase contrast has been a pillar in optical microscopy and more recently in x-ray microscopy, in particular for low-absorption-contrast biological specimens. We experimentally demonstrate that hard-x-ray Zernike microscopy now reaches a lateral resolution below 30?nm while strongly enhancing the contrast, thus opening many new research opportunities in biomedicine and materials science.

  11. Hard x-ray Zernike Microscopy Reaches 30 nm Resolution

    SciTech Connect

    Chen, Y.T.; Chu, Y.; Chen, T-Y.; Yi, J.; Lee, W-K.; Wang, C-L.; Kempson, I. M.; Hwu, Y.; Gajdosik, V.; Margaritondo, G.

    2011-03-30

    Since its invention in 1930, Zernike phase contrast has been a pillar in optical microscopy and more recently in x-ray microscopy, in particular for low-absorption-contrast biological specimens. We experimentally demonstrate that hard-x-ray Zernike microscopy now reaches a lateral resolution below 30 nm while strongly enhancing the contrast, thus opening many new research opportunities in biomedicine and materials science.

  12. The prospects for soft x-ray contact microscopy using laser plasmas as an x-ray source

    SciTech Connect

    Stead, A.D.; Page, A.M.; Ford, T.W.

    1995-12-31

    Since its invention, a major concern of those using a microscope has been to improve the resolution without the introduction of artifacts. While light microscopy carries little risk of the introduction of artifacts, because the preparative techniques are often minimal, the resolution is somewhat limited. The advent of the electron microscope offered greatly improved resolution but since biological specimens require extensive preparation, the possibility of causing structural damage to the specimen is also increased. The ideal technique for structural studies of biological specimens would enable hydrated material to be examined without any preparation and with a resolution equal to that of electron microscopy. Soft x-ray microscopy certainly enables living material to be examined and whilst the resolution does not equal that of electron microscopy it exceeds that attainable by light microscopy. This paper briefly reviews the limitations of light and electron microscopy for the biologist and considers the various ways that soft x-rays might be used to image hydrated biological material. Consideration is given to the different sources that have been used for soft x-ray microscopy and the relative merits of laser-plasma sources are discussed.

  13. The Scanning X-Ray Microprobe at the Esrf ``X-Ray Microscopy'' Beamline

    NASA Astrophysics Data System (ADS)

    Susini, J.; Salomé, M.; Fayard, B.; Ortega, R.; Kaulich, B.

    The development of high brilliance X-ray sources coupled with advances in manufacturing technologies of focusing optics has led to significant improvements in submicrometer probes for spectroscopy, diffraction and imaging applications. For instance, X-ray microscopy in the 1-10 keV energy range is better-suited for analyzing trace elements in fluorescence yield. This article will be biased towards submicron fluorescence microscopy developed on the ID21 beamline at the ESRF. The main technical developments, involving new focusing lenses or novel phase contrast method, are presented. Strengths and weaknesses of X-ray microscopy and spectromicroscopy techniques are discussed and illustrated by examples in biology, materials science and geology.

  14. X-ray laser microscopy of rat sperm nuclei

    SciTech Connect

    Da Silva, L.B. ); Trebes, J.E.; Balhorn, R.; Mrowka, S.; Barbee, T.W.Jr.; Brase, J.; Corzett, M.; Koch, J.A.; Lee, C.; London, R.A.; MacGowan, B.J.; Matthews, D.L.; Stone, G. ); Anderson, E.; Attwood, D.T. ); Gray, J. ); Kern, D. )

    1992-10-09

    The development of high brightness and short pulse width x-ray lasers now offers biologists the possibility of high-resolution imaging of specimens in an aqueous environment without the blurring effects associated with natural motions and chemical erosion. As a step toward developing the capabilities of this type of x-ray microscopy, a tantalum x-ray laser at 44.83 angstrom wavelength was used together with an x-ray zone plate lens to image both unlabeled and selectively gold-labeled dried rat sperm nuclei. The observed images show {approximately}500 angstrom features, illustrate the importance of x-ray microscopy in determining chemical composition, and provide information about the uniformity of sperm chromatin organization and the extent of sperm chromatin hydration.

  15. X-ray laser microscopy of rat sperm nuclei.

    PubMed

    Da Silva, L B; Trebes, J E; Balhorn, R; Mrowka, S; Anderson, E; Attwood, D T; Barbee, T W; Brase, J; Corzett, M; Gray, J

    1992-10-09

    The development of high brightness and short pulse width (< 200 picoseconds) x-ray lasers now offers biologists the possibility of high-resolution imaging of specimens in an aqueous environment without the blurring effects associated with natural motions and chemical erosion. As a step toward developing the capabilities of this type of x-ray microscopy, a tantalum x-ray laser at 44.83 angstrom wavelength was used together with an x-ray zone plate lens to image both unlabeled and selectively gold-labeled dried rat sperm nuclei. The observed images show approximately 500 angstrom features, illustrate the importance of x-ray microscopy in determining chemical composition, and provide information about the uniformity of sperm chromatin organization and the extent of sperm chromatin hydration.

  16. Development of Cell Staining Technique for X-Ray Microscopy

    SciTech Connect

    Tseng, P. Y.; Shih, Y. T.; Liu, C. J.; Hsu, T.; Chien, C. C.; Leng, W. H.; Liang, K. S.; Yin, G. C.; Chen, F. R.; Je, J. H.; Margaritondo, G.; Hwu, Y.

    2007-01-19

    We report a technique for detection of sub-cellular organelles and proteins with hard x-ray microscopy. Several metals were used for enhancing contrast for x-ray microscopy. Osmium tetroxide provides an excellent stain for lipid and can delineate cell membrane. Uranyl acetate has high affinity for nucleotide and can stain nucleus. Immunolocalization of specific proteins and sub-cellular organelles was achieved by 3'3 diaminobenzidine (DAB) with nickel enhancement and nanogold-conjugated secondary antibody with silver enhancement. The x-rays emitted from synchrotron source was monochromatized by double crystal monochromator, the photon energy was fixed at 8 keV to optimize the focusing efficiency of the zone plates. The estimated resolution is about 60 nm. When compared with visible light and conventional confocal microscopy, the X-ray microscopy provides a superior resolution to both conventional optical microscopes.

  17. Refractive Optics for Hard X-ray Transmission Microscopy

    SciTech Connect

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

    2011-09-09

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

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

    USDA-ARS?s Scientific Manuscript database

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

  19. Scanning electron microscopy coupled with energy-dispersive X-ray spectrometry for quick detection of sulfur-oxidizing bacteria in environmental water samples

    NASA Astrophysics Data System (ADS)

    Sun, Chengjun; Jiang, Fenghua; Gao, Wei; Li, Xiaoyun; Yu, Yanzhen; Yin, Xiaofei; Wang, Yong; Ding, Haibing

    2017-01-01

    Detection of sulfur-oxidizing bacteria has largely been dependent on targeted gene sequencing technology or traditional cell cultivation, which usually takes from days to months to carry out. This clearly does not meet the requirements of analysis for time-sensitive samples and/or complicated environmental samples. Since energy-dispersive X-ray spectrometry (EDS) can be used to simultaneously detect multiple elements in a sample, including sulfur, with minimal sample treatment, this technology was applied to detect sulfur-oxidizing bacteria using their high sulfur content within the cell. This article describes the application of scanning electron microscopy imaging coupled with EDS mapping for quick detection of sulfur oxidizers in contaminated environmental water samples, with minimal sample handling. Scanning electron microscopy imaging revealed the existence of dense granules within the bacterial cells, while EDS identified large amounts of sulfur within them. EDS mapping localized the sulfur to these granules. Subsequent 16S rRNA gene sequencing showed that the bacteria detected in our samples belonged to the genus Chromatium, which are sulfur oxidizers. Thus, EDS mapping made it possible to identify sulfur oxidizers in environmental samples based on localized sulfur within their cells, within a short time (within 24 h of sampling). This technique has wide ranging applications for detection of sulfur bacteria in environmental water samples.

  20. Functional biocompatible magnetite-cellulose nanocomposite fibrous networks: Characterization by fourier transformed infrared spectroscopy, X-ray powder diffraction and field emission scanning electron microscopy analysis.

    PubMed

    Habibi, Neda

    2015-02-05

    The preparation and characterization of functional biocompatible magnetite-cellulose nano-composite fibrous material is described. Magnetite-cellulose nano-composite was prepared by a combination of the solution-based formation of magnetic nano-particles and subsequent coating with amino celluloses. Characterization was accomplished using X-ray powder diffraction (XRD), fourier transformed infrared (FTIR) and field emission scanning electron microscopy (FESEM) analysis. The peaks of Fe3O4 in the XRD pattern of nanocomposite confirm existence of the nanoparticles in the amino cellulose matrix. Magnetite-cellulose particles exhibit an average diameter of roughly 33nm as demonstrated by field emission scanning electron microscopy. Magnetite nanoparticles were irregular spheres dispersed in the cellulose matrix. The vibration corresponding to the NCH3 functional group about 2850cm(-1) is assigned in the FTIR spectra. Functionalized magnetite-cellulose nano-composite polymers have a potential range of application as targeted drug delivery system in biomedical field. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Quantitative study of particle size distribution in an in-situ grown Al–TiB{sub 2} composite by synchrotron X-ray diffraction and electron microscopy

    SciTech Connect

    Tang, Y.; Chen, Z.; Borbély, A.; Ji, G.; Zhong, S.Y.; Schryvers, D.; Ji, V.

    2015-04-15

    Synchrotron X-ray diffraction and transmission electron microscopy (TEM) were applied to quantitatively characterize the average particle size and size distribution of free-standing TiB{sub 2} particles and TiB{sub 2} particles in an in-situ grown Al–TiB{sub 2} composite. The detailed evaluations were carried out by X-ray line profile analysis using the restricted moment method and multiple whole profile fitting procedure (MWP). Both numerical methods indicate that the formed TiB{sub 2} particles are well crystallized and free of crystal defects. The average particle size determined from different Bragg reflections by the restricted moment method ranges between 25 and 55 nm, where the smallest particle size is determined using the 110 reflection suggesting the highest lateral-growth velocity of (110) facets. The MWP method has shown that the in-situ grown TiB{sub 2} particles have a very low dislocation density (~ 10{sup 11} m{sup −} {sup 2}) and their size distribution can be described by a log-normal distribution. Good agreement was found between the results obtained from the restricted moment and MWP methods, which was further confirmed by TEM. - Highlights: • Accurate quantitative characterization of in-situ grown T{sub i}B{sub 2} particles has been achieved. • Particle size anisotropy was revealed indicating 110 facets being largest during T{sub i}B{sub 2} growth. • A wide size distribution was observed for T{sub i}B{sub 2} particles with a dominant size smaller than 100 nm.

  2. Comparison between MCNP and PENELOPE for the simulation of X-ray spectra in electron microscopy in the keV range

    NASA Astrophysics Data System (ADS)

    Roet, D.; Ceballos, C.; Van Espen, P.

    2006-10-01

    In this paper two Monte Carlo codes, MCNP (version 4C2) and PENELOPE (version 2001), were used in a cluster environment to simulate the X-ray spectra emerging from bombarding pure element bulk targets with mono energetic electrons in the keV range (30 keV). The simulation results were compared to experimental data measured on a JEOL-6300 electron microscope with energy dispersive X-ray detector. The results from both codes were compared amongst each other as to find the best in terms of accuracy, ease of use and speed of the calculations.

  3. X-Ray Diffraction Microscopy of Magnetic Structures

    SciTech Connect

    Turner, J.; Lima, E.; Huang, X.; Krupin, O.; Seu, K.; Parks, D.; Kevan, S.; Kisslinger, K.; McNulty, I.; Gambino, R.; Mangin, S.; Roy, S. and Fischer, P.

    2011-07-14

    We report the first proof-of-principle experiment of iterative phase retrieval from magnetic x-ray diffraction. By using the resonant x-ray excitation process and coherent x-ray scattering, we show that linearly polarized soft x rays can be used to image both the amplitude and the phase of magnetic domain structures. We recovered the magnetic structure of an amorphous terbium-cobalt thin film with a spatial resolution of about 75 nm at the Co L{sub 3} edge at 778 eV. In comparison with soft x-ray microscopy images recorded with Fresnel zone plate optics at better than 25 nm spatial resolution, we find qualitative agreement in the observed magnetic structure.

  4. A hard X-ray nanoprobe beamline for nanoscale microscopy

    PubMed Central

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

    2012-01-01

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

  5. X-ray Free-electron Lasers

    SciTech Connect

    Feldhaus, J.; Arthur, J.; Hastings, J.B.; /SLAC

    2007-02-23

    In a free-electron laser (FEL) the lasing medium is a high-energy beam of electrons flying with relativistic speed through a periodic magnetic field. The interaction between the synchrotron radiation that is produced and the electrons in the beam induces a periodic bunching of the electrons, greatly increasing the intensity of radiation produced at a particular wavelength. Depending only on a phase match between the electron energy and the magnetic period, the wavelength of the FEL radiation can be continuously tuned within a wide spectral range. The FEL concept can be adapted to produce radiation wavelengths from millimeters to Angstroms, and can in principle produce hard x-ray beams with unprecedented peak brightness, exceeding that of the brightest synchrotron source by ten orders of magnitude or more. This paper focuses on short-wavelength FELs. It reviews the physics and characteristic properties of single-pass FELs, as well as current technical developments aiming for fully coherent x-ray radiation pulses with pulse durations in the 100 fs to 100 as range. First experimental results at wavelengths around 100 nm and examples of scientific applications planned on the new, emerging x-ray FEL facilities are presented.

  6. Analysis of x-ray spectrum obtained in electron cyclotron resonance x-ray source

    SciTech Connect

    Baskaran, R.; Selvakumaran, T.S.; Sunil Sunny, C.

    2006-03-15

    The analysis of the x-ray spectrum obtained in electron cyclotron resonance (ECR) x-ray source is carried out. Assuming single-particle motion, the electron acceleration and its final energy are calculated for TE{sub 111} cylindrical cavity field and uniform external dc magnetic field. In the calculation, initial coordinates of 40 000 electrons were uniformly selected over the central plane of the cavity using random number generator. The final energy of each electron when it hits the wall is stored and the electron energy distribution is obtained. Using the general purpose Monte Carlo N-particle transport code version 4A, the geometry of the ECR x-ray source is modeled. The x-ray energy spectrum is calculated for the geometry model and the numerically calculated electron energy distribution. The calculated x-ray spectrum is compared with the experimentally measured x-ray spectrum.

  7. A study of gunshot residue distribution for close-range shots with a silenced gun using optical and scanning electron microscopy, X-ray microanalysis and infrared spectroscopy.

    PubMed

    Brożek-Mucha, Zuzanna

    2017-03-01

    Detailed physical and chemical analysis of gunshot residue deposited in the nearest vicinity of a submachine gun alone and with a sound suppressor was performed. The studies were inspired by recent shooting cases with the use of a firearm with a silencer and the need to estimate the shooting distance to human body naked and covered with clothing. A series of experiments were performed in the shooting range using a machine pistol and the appropriate ammunition cal. 7.65mm Browning. Targets were placed in the range of 0-30cm from the gun and covered either with white cotton fabric or a porcine skin that mocked people's clothing and the naked skin. Both the organic and inorganic residue were examined by means of optical microscopy, infrared spectrometry as well as scanning electron microscopy and energy dispersive X-ray spectrometry. The influence of factors, such as sound suppressor, shooting distance and the substrate type on the mechanism of particles spread and their availability for research was established and discussed.

  8. Femtosecond laser-electron x-ray source

    DOEpatents

    Hartemann, Frederic V.; Baldis, Hector A.; Barty, Chris P.; Gibson, David J.; Rupp, Bernhard

    2004-04-20

    A femtosecond laser-electron X-ray source. A high-brightness relativistic electron injector produces an electron beam pulse train. A system accelerates the electron beam pulse train. The femtosecond laser-electron X-ray source includes a high intra-cavity power, mode-locked laser and an x-ray optics system.

  9. Sixth International Conference on X-ray Microscopy

    SciTech Connect

    Robinson, Arthur L.

    1999-08-23

    More than 180 participants from around the world crowded the Clark Kerr Campus of the University of California, Berkeley, from August 1-6, 1999 for the Sixth International Conference on X-Ray Microscopy (XRM99). Held every three years since 1983, the XRM conferences have become the primary international forum for the presentation and discussion of advances in high-spatial-resolution x-ray imaging and applications (including the use of x-ray spectroscopic and analytical techniques) in biological and medical sciences, environmental and soil sciences, and materials and surface sciences.

  10. Cryogenic X-Ray Diffraction Microscopy for Biological Samples

    SciTech Connect

    Lima, Enju; Wiegart, Lutz; Pernot, Petra; Howells, Malcolm; Timmins, Joanna; Zontone, Federico; Madsen, Anders

    2009-11-06

    X-ray diffraction microscopy (XDM) is well suited for nondestructive, high-resolution biological imaging, especially for thick samples, with the high penetration power of x rays and without limitations imposed by a lens. We developed nonvacuum, cryogenic (cryo-) XDM with hard x rays at 8 keV and report the first frozen-hydrated imaging by XDM. By preserving samples in amorphous ice, the risk of artifacts associated with dehydration or chemical fixation is avoided, ensuring the imaging condition closest to their natural state. The reconstruction shows internal structures of intact D. radiodurans bacteria in their natural contrast.

  11. Scanning Transmission X-ray microscopy Imaging of Aerosol Particles

    NASA Astrophysics Data System (ADS)

    Gilles, M. K.; Kilcoyne, A.; Tyliszczak, T.; Shuh, D. K.; Fakra, S.; Robinson, M.; Chase, K.

    2003-12-01

    Scanning transmission x-ray microscopes (STXM) are used to image a diversity of carbon and metal containing items such as biofilms in soils, magnetic materials, polymers and meteorites. Studies on particles collected on SiO2 filters from biomass burns in Flagstaff, Arizona and individual aerosols collected in South Africa on TEM grids are underway at beamlines 5.3.2 and 11.0.2 at the Advanced Light Source of Lawrence Berkeley National Laboratory. Sub micron particles are imaged in the transmission mode over the energy range of 280 - 1900 eV. Spectromicroscopic studies on individual particles using near edge x-ray absorption fine structure (NEXAFS) probe multiple species within or on the same particle. In (STXM) an X-ray beam is focused with a zone plate onto a sample and the transmitted radiation is detected. Since the signal is obtained in the transmission mode, optically thin samples are required. Hence, atmospheric aerosols with submicron thickness and diameter are well suited for this method. Near edge spectra of various elements were scanned in step sizes from 0.1-0.5 eV around characteristic absorption edges, creating 2 dimensional images at each energy. While STXM images are taken with a lower spatial resolution (currently 40 nm) than microscopies such as scanning electron microscopy, transmission electron microscopy, and atomic force microscopy, detailed chemical information with spatial distributions, and oxidation states is obtained. A particular focus of this work is to obtain more detailed information on the type of carbons, multiply, or singly bonded and whether or not carbon is bonded to oxygen. The ultimate goal is discrimination between organic and black carbon within individual aerosol particles and determining if organic carbon, black carbon, and metal species are distributed homogeneously throughout aerosol particles. Initial scans of the samples from Flagstaff show spectral evidence of aromatic carbon, without distinct C=O signatures. NEXAFS

  12. 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.

  13. Chemical and morphological study of gunshot residue persisting on the shooter by means of scanning electron microscopy and energy dispersive X-ray spectrometry.

    PubMed

    Brożek-Mucha, Zuzanna

    2011-12-01

    Persistence of gunshot residue (GSR) simultaneously collected from hands, face and hair, and clothing of the shooting person was examined. Samples were collected from five shooters in nine time intervals after a single shoot with a Luger 9 mm pistol, in the range of 0-4 h and examined with scanning electron microscopy and energy dispersive X-ray spectrometry. Numbers of particles, frequencies of occurrence of certain compositions of particles, and their sizes in function of the time intervals were inspected. The greatest numbers of particles were observed in samples collected from hands right after shooting, but they decrease quickly with time. In samples collected from the face smaller initial numbers of particles were found, but they lasted at a similar level longer. The estimated half-life times of particles were less than 1 h for samples taken from the hands, over 1 h for clothing and about 2-3 h for the face. In samples collected at longer intervals after shooting, there were particles present of small sizes and irregular shapes. The results demonstrate that including evidence collected from the suspect's face and hair may increase the probability of detection of GSR in cases when the suspect has not been apprehended immediately after the investigated incident.

  14. Scanning electron microscopy and X-ray microanalysis for chemical and morphological characterisation of the inorganic component of gunshot residue: selected problems.

    PubMed

    Brożek-Mucha, Zuzanna

    2014-01-01

    Chosen aspects of examinations of inorganic gunshot particles by means of scanning electron microscopy and energy dispersive X-ray spectrometry technique are presented. The research methodology of particles was worked out, which included a precise and repeatable procedure of the automatic detection and identification of particles as well as the representation of the obtained analytical data in the form of the frequencies of occurrence of particles of certain chemical or morphological class within the whole population of particles revealed in a specimen. On this basis, there were established relationships between the chemical and morphological properties of populations of particles and factors, such as the type of ammunition, the distance from the gun muzzle to the target, the type of a substrate the particles sediment on, and the time between shooting and collecting the specimens. Each of these aspects of examinations of particles revealed a great potential of being utilised in casework, while establishing various circumstances of shooting incidents leads to the reconstruction of the course of the studied incident.

  15. A Study of the Oxidation Behaviour of Pile Grade A (PGA) Nuclear Graphite Using Thermogravimetric Analysis (TGA), Scanning Electron Microscopy (SEM) and X-Ray Tomography (XRT).

    PubMed

    Payne, Liam; Heard, Peter J; Scott, Thomas B

    2015-01-01

    Pile grade A (PGA) graphite was used as a material for moderating and reflecting neutrons in the UK's first generation Magnox nuclear power reactors. As all but one of these reactors are now shut down there is a need to understand the residual state of the material prior to decommissioning of the cores, in particular the location and concentration of key radio-contaminants such as 14C. The oxidation behaviour of unirradiated PGA graphite was studied, in the temperature range 600-1050°C, in air and nitrogen using thermogravimetric analysis, scanning electron microscopy and X-ray tomography to investigate the possibility of using thermal degradation techniques to examine 14C distribution within irradiated material. The thermal decomposition of PGA graphite was observed to follow the three oxidation regimes historically identified by previous workers with limited, uniform oxidation at temperatures below 600°C and substantial, external oxidation at higher temperatures. This work demonstrates that the different oxidation regimes of PGA graphite could be developed into a methodology to characterise the distribution and concentration of 14C in irradiated graphite by thermal treatment.

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

    PubMed

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

    2017-06-01

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

  17. A Study of the Oxidation Behaviour of Pile Grade A (PGA) Nuclear Graphite Using Thermogravimetric Analysis (TGA), Scanning Electron Microscopy (SEM) and X-Ray Tomography (XRT)

    PubMed Central

    Payne, Liam; Heard, Peter J.; Scott, Thomas B.

    2015-01-01

    Pile grade A (PGA) graphite was used as a material for moderating and reflecting neutrons in the UK’s first generation Magnox nuclear power reactors. As all but one of these reactors are now shut down there is a need to understand the residual state of the material prior to decommissioning of the cores, in particular the location and concentration of key radio-contaminants such as 14C. The oxidation behaviour of unirradiated PGA graphite was studied, in the temperature range 600–1050°C, in air and nitrogen using thermogravimetric analysis, scanning electron microscopy and X-ray tomography to investigate the possibility of using thermal degradation techniques to examine 14C distribution within irradiated material. The thermal decomposition of PGA graphite was observed to follow the three oxidation regimes historically identified by previous workers with limited, uniform oxidation at temperatures below 600°C and substantial, external oxidation at higher temperatures. This work demonstrates that the different oxidation regimes of PGA graphite could be developed into a methodology to characterise the distribution and concentration of 14C in irradiated graphite by thermal treatment. PMID:26575374

  18. Structure refinement of the δ1p phase in the Fe–Zn system by single-crystal X-ray diffraction combined with scanning transmission electron microscopy

    PubMed Central

    Okamoto, Norihiko L.; Tanaka, Katsushi; Yasuhara, Akira; Inui, Haruyuki

    2014-01-01

    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. PMID:24675597

  19. Scanning Electron Microscopy and X-Ray Microanalysis for Chemical and Morphological Characterisation of the Inorganic Component of Gunshot Residue: Selected Problems

    PubMed Central

    Brożek-Mucha, Zuzanna

    2014-01-01

    Chosen aspects of examinations of inorganic gunshot particles by means of scanning electron microscopy and energy dispersive X-ray spectrometry technique are presented. The research methodology of particles was worked out, which included a precise and repeatable procedure of the automatic detection and identification of particles as well as the representation of the obtained analytical data in the form of the frequencies of occurrence of particles of certain chemical or morphological class within the whole population of particles revealed in a specimen. On this basis, there were established relationships between the chemical and morphological properties of populations of particles and factors, such as the type of ammunition, the distance from the gun muzzle to the target, the type of a substrate the particles sediment on, and the time between shooting and collecting the specimens. Each of these aspects of examinations of particles revealed a great potential of being utilised in casework, while establishing various circumstances of shooting incidents leads to the reconstruction of the course of the studied incident. PMID:25025050

  20. A case of hut lung: scanning electron microscopy with energy dispersive x-ray spectroscopy analysis of a domestically acquired form of pneumoconiosis.

    PubMed

    Mukhopadhyay, Sanjay; Gujral, Manmeet; Abraham, Jerrold L; Scalzetti, Ernest M; Iannuzzi, Michael C

    2013-07-01

    Hut lung is a pneumoconiosis caused by exposure to smoke derived from biomass fuels used for cooking in poorly ventilated huts. We report, to our knowledge, the first analysis of the dust deposited in the lungs in hut lung by scanning electron microscopy with energy dispersive x-ray spectroscopy (SEM/EDS). A Bhutanese woman presented with shortness of breath and an abnormal chest radiograph. Chest CT scan showed innumerable tiny bilateral upper lobe centrilobular nodules. Transbronchial biopsy revealed mild interstitial fibrosis with heavy interstitial deposition of black dust. SEM/EDS showed that the dust was carbonaceous, with smaller yet substantial numbers of silica and silicate particles. Additional history revealed use of a wood/coal-fueled stove in a small, poorly ventilated hut for 45 years. The possibility of hut lung should be considered in women from countries where use of biomass-fueled stoves for cooking is common. Our findings support the classification of this condition as a mixed-dust pneumoconiosis.

  1. X-ray fluorescence (conventional and 3D) and scanning electron microscopy for the investigation of Portuguese polychrome glazed ceramics: Advances in the knowledge of the manufacturing techniques

    NASA Astrophysics Data System (ADS)

    Guilherme, A.; Coroado, J.; dos Santos, J. M. F.; Lühl, L.; Wolff, T.; Kanngießer, B.; Carvalho, M. L.

    2011-05-01

    This work shows the first analytical results obtained by X-Ray Fluorescence (XRF) (conventional and 3D) and Scanning Electron Microscopy with Energy Dispersive System (SEM-EDS) on original Portuguese ceramic pieces produced between the 16th and 18th centuries in Coimbra and Lisbon. Experts distinguished these productions based only on the color, texture and brightness, which originates mislabeling in some cases. Thanks to lateral and spatial resolution in the micrometer regime, the results obtained with μ-XRF were essential in determining the glaze and pigment thicknesses by monitoring the profile of the most abundant element in each "layer". Furthermore, the dissemination of these elements throughout the glaze is different depending on the glaze composition, firing temperature and on the pigment itself. Hence, the crucial point of this investigation was to analyze and understand the interfaces color/glaze and glaze/ceramic support. Together with the XRF results, images captured by SEM and the corresponding semi-quantitative EDS data revealed different manufacturing processes used by the two production centers. Different capture modes were suitable to distinguish different crystals from the minerals that confer the color of the pigments used and to enhance the fact that some of them are very well spread through the glassy matrix, sustaining the theory of an evolved and careful procedure in the manufacturing process of the glaze.

  2. Chemical Differentiation of Osseous and Nonosseous Materials Using Scanning Electron Microscopy-Energy-Dispersive X-Ray Spectrometry and Multivariate Statistical Analysis.

    PubMed

    Meizel-Lambert, Cayli J; Schultz, John J; Sigman, Michael E

    2015-11-01

    Identification of osseous materials is generally established on gross anatomical features. However, highly fragmented or taphonomically altered materials may be problematic and may require chemical analysis. This research was designed to assess the use of scanning electron microscopy-energy-dispersive X-ray spectrometry (SEM/EDX), elemental analysis, and multivariate statistical analysis (principal component analysis) for discrimination of osseous and nonosseous materials of similar chemical composition. Sixty samples consisting of osseous (human and nonhuman bone and dental) and non-osseous samples were assessed. After outliers were removed a high overall correct classification of 97.97% was achieved, with 99.86% correct classification for osseous materials. In addition, a blind study was conducted using 20 samples to assess the applicability for using this method to classify unknown materials. All of the blind study samples were correctly classified resulting in 100% correct classification, further demonstrating the efficiency of SEM/EDX and statistical analysis for differentiation of osseous and nonosseous materials. © 2015 American Academy of Forensic Sciences.

  3. Optical and structural properties in type-II InAlAs/AlGaAs quantum dots observed by photoluminescence, X-ray diffraction and transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Ben Daly, A.; Craciun, D.; Laura Ursu, E.; Lemaître, A.; Maaref, M. A.; Iacomi, F.; Vasile, B. S.; Craciun, V.

    2017-10-01

    We present the effects of AlGaAs alloy composition on InAlAs quantum dots (QDs) optical and structural properties. Photoluminescence (PL) analysis of samples having a variety of aluminium composition values covering type-II transitions clearly in QDs showed the presence of two transitions X-Sh and X-Ph. High-resolution X-ray diffraction (HRXRD) investigations showed that the layers grew epitaxially on the GaAs substrate, with no relaxation regardless the Al content of AlGaAs layer. From the reciprocal space map (RSM) investigation around (004) and (115) diffraction peaks, it was shown that the InAlAs layer is fully strained, the in-plane lattice parameters (a and b, a = b) being identical to those of GaAs substrate, while the c lattice parameter was dependent on the In and Al concentrations, being larger than that of the substrate. High-resolution transmission electronic microscopy (HRTEM) investigations confirmed that films grew epitaxially on the GaAs substrate with no visible dislocations or other major defects within the InAlAs/GaAlAs QDs structure.

  4. Quick Detection of Sulfur Bacteria in Environmental Water Sample with SEM(scanning electron microscopy) coupled with Energy Dispersive X-ray Spectrometry

    NASA Astrophysics Data System (ADS)

    Sun, C.; Ding, H.; Wang, Y.; Jiang, F.; Li, X.; Gao, W.; Yin, X.

    2015-12-01

    Sulfur-oxidizing bacteria play important roles in global sulfur cycle. Sulfur bacteria detection has been largely dependent on targeted gene sequencing technology or traditional cell cultivation which usually takes from days to months to finish. This cannot meet the requirements of some time-sensitive samples and/or complicated environmental samples. Since Energy-Dispersive X-ray Spectrometry (EDS) can be used to simultaneously detect multiple elements including sulfur in a sample with minimal sample treatment, the technology was applied to detect sulfur bacteria through the high sulfur content in the bacteria cell. We report the application of SEM (scanning electron microscopy) imaging coupled with EDS mapping for direct and quick detection of sulfur oxidizer in contaminated environmental water samples. The presence of sulfur bacteria can be confirmed within 24 hours after sampling. Subsequent 16S RNA gene sequencing results found the bacteria detected had over 99% similarity to Chromatium Okenii, confirming the bacterium was a sulfur oxidizer. The developed technique made it possible to quickly detect sulfur oxidizer in environmental sample and could have wide applications in sulfur bacteria detection in environmental water samples.

  5. Investigation of defect clusters in ion-irradiated Ni and NiCo using diffuse X-ray scattering and electron microscopy

    SciTech Connect

    Olsen, Raina J.; Jin, Ke; Lu, Chenyang; Beland, Laurent K.; Wang, Lumin M.; Bei, Hongbin; Specht, Eliot D.; Larson, Bennett C.

    2016-01-01

    The nature of defect clusters in Ni and Ni$_{50}$Co$_{50}$ (NiCo) irradiated at room temperature with 2–16 MeV Ni ions is studied using asymptotic diffuse X-ray scattering and transmission electron microscopy (TEM). Analysis of the scattering data provides separate size distributions for vacancy and interstitial type defect clusters, showing that both types of defect clusters have a smaller size and higher density in NiCo than in Ni. Diffuse scattering results show good quantitative agreement with TEM results for cluster sizes greater than 4 nm diameter, but find that the majority of vacancy clusters are under 2 nm in NiCo, which, if not detected, would lead to the conclusion that defect density was actually lower in the alloy. Interstitial dislocation loops and stacking fault tetrahedra are identified by TEM. Lastly comparison of diffuse scattering lineshapes to those calculated for dislocation loops and SFTs indicates that most of the vacancy clusters are SFTs.

  6. Investigation of defect clusters in ion-irradiated Ni and NiCo using diffuse X-ray scattering and electron microscopy

    DOE PAGES

    Olsen, Raina J.; Jin, Ke; Lu, Chenyang; ...

    2016-01-01

    The nature of defect clusters in Ni and Nimore » $$_{50}$$Co$$_{50}$$ (NiCo) irradiated at room temperature with 2–16 MeV Ni ions is studied using asymptotic diffuse X-ray scattering and transmission electron microscopy (TEM). Analysis of the scattering data provides separate size distributions for vacancy and interstitial type defect clusters, showing that both types of defect clusters have a smaller size and higher density in NiCo than in Ni. Diffuse scattering results show good quantitative agreement with TEM results for cluster sizes greater than 4 nm diameter, but find that the majority of vacancy clusters are under 2 nm in NiCo, which, if not detected, would lead to the conclusion that defect density was actually lower in the alloy. Interstitial dislocation loops and stacking fault tetrahedra are identified by TEM. Lastly comparison of diffuse scattering lineshapes to those calculated for dislocation loops and SFTs indicates that most of the vacancy clusters are SFTs.« less

  7. Surface analysis of ProFile instruments by scanning electron microscopy and X-ray energy-dispersive spectroscopy: a preliminary study.

    PubMed

    Martins, R C; Bahia, M G A; Buono, V T L

    2002-10-01

    The purpose of this preliminary study was to analyze surface irregularities on ProFile nickel-titanium (NiTi) rotary instruments before use, after sterilization by two different methods and after instrumentation of molar root canals. Five new ProFile NiTi rotary instruments with 0.04 taper, size 20, five instruments with 0.04 taper, size 25 and five with 0.06 taper, size 20 were analyzed by scanning electron microscopy (SEM) and X-ray energy-dispersive spectroscopy (EDS). The instruments were then divided into two groups: three of each taper and size were sterilized in a dry heat sterilizer, whilst two of each taper and size were sterilized in an autoclave. After inspection by the same techniques, the files were used to instrument six molar root canals, and again analyzed by SEM/EDS. Together with the usual machining defects, a variable amount of material containing mainly carbon and sulphur was found on the surface of new instruments. This material was not removed by standard cleaning and sterilization procedures. The use of the files for instrumentation of root canals eliminated a considerable amount of the adhered substance, but deposits rich in calcium and phosphorus accumulated on the remaining impurities. The adherence of dentine on surface deposits found on new ProFile instruments requires special cleaning, prior to sterilization.

  8. Micro-computed tomography, scanning electron microscopy and energy X-ray spectroscopy studies of facet joint degeneration: A comparison to clinical imaging.

    PubMed

    Goehre, Felix; Ludtka, Christopher; Hamperl, Melanie; Friedmann, Andrea; Straube, Anja; Mendel, Thomas; Heilmann, Andreas; Meisel, Hans Jörg; Schwan, Stefan

    2017-09-01

    Segmental degeneration in the human lumbar spine affects both the intervertebral discs and facet joints. Facet joint degeneration not only affects the cartilage surface, but also alters the cellular properties of the cartilage tissue and the structure of the subchondral bone. The primary focus of this study is the investigation of these microstructural changes that are caused by facet joint degeneration. Microstructural analyses of degenerated facet joint samples, obtained from patients following operative lumbar interbody fusion, have not previously been extensively investigated. This study analyzes human facet joint samples from the inferior articular process using scanning electron microscopy, micro-computed tomography, and energy dispersive X-ray spectroscopy to evaluate parameters of interest in facet joint degeneration such as elemental composition, cartilage layer thickness and cell density, calcification zone thickness, subchondral bone portion, and trabecular bone porosity. These microstructural analyses demonstrate fragmentation, cracking, and destruction of the cartilage layer, a thickened calcification zone, localized calcification areas, and cell cluster formation as pathological manifestations of facet joint degeneration. The detailed description of these microstructural changes is critical for a comprehensive understanding of the pathology of facet joint degeneration, as well as the subsequent development and efficacy analysis of regenerative treatment strategies. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. In vivo ingestion of heavy metal particles of Se, Hg and W by murine macrophages. A study using scanning electron microscopy coupled with X-ray microanalysis.

    PubMed

    Cherdwongcharoensuk, Duangrudee; Cunha, Elisabete M; Upatham, Suchart; Pereira, António Sousa; Oliveira, Maria João R; Aguas, Artur P

    2002-09-01

    Several heavy metals that are currently employed in industry may become polluters of work and natural environments. As particulate matter, heavy metals are suitable for entering the human body through the respiratory and digestive systems. They often end up inside phagocytes; the size of the microscopic particles modulates both their phagocytosis, and the physiology of macrophages. Here we have adopted an experimental model to investigate the ingestion of particles of three industrial heavy metals (Se, Hg, W) by murine peritoneal macrophages in vivo. The phagocytes were studied by scanning electron microscopy coupled with X-ray elemental microanalysis (SEM-XRM), a method that allows specific identification of Se, W and Hg in cells at high resolution. We found that Hg that was taken up by macrophages was organized into small, round particles (0.31 +/- 0.14 microm). This was in contrast with the larger size of intracellular particles of Se (2.37 +/- 1.84 microm) or W (1.75 +/- 1.34 microm). Ingested particles of Se and W, but not Hg, often caused bulging of the cell surface of macrophages. We conclude that particulate matters of Se, W and Hg are organized in particles of different size inside macrophages. This size difference is likely to be associated with distinct phlogistic activities of these heavy metals, Se and W causing a milder inflammatory reaction than Hg.

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

    PubMed

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

    2016-02-01

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

  11. Computer-aided screening system for cervical precancerous cells based on field emission scanning electron microscopy and energy dispersive x-ray images and spectra

    NASA Astrophysics Data System (ADS)

    Jusman, Yessi; Ng, Siew-Cheok; Hasikin, Khairunnisa; Kurnia, Rahmadi; Osman, Noor Azuan Bin Abu; Teoh, Kean Hooi

    2016-10-01

    The capability of field emission scanning electron microscopy and energy dispersive x-ray spectroscopy (FE-SEM/EDX) to scan material structures at the microlevel and characterize the material with its elemental properties has inspired this research, which has developed an FE-SEM/EDX-based cervical cancer screening system. The developed computer-aided screening system consisted of two parts, which were the automatic features of extraction and classification. For the automatic features extraction algorithm, the image and spectra of cervical cells features extraction algorithm for extracting the discriminant features of FE-SEM/EDX data was introduced. The system automatically extracted two types of features based on FE-SEM/EDX images and FE-SEM/EDX spectra. Textural features were extracted from the FE-SEM/EDX image using a gray level co-occurrence matrix technique, while the FE-SEM/EDX spectra features were calculated based on peak heights and corrected area under the peaks using an algorithm. A discriminant analysis technique was employed to predict the cervical precancerous stage into three classes: normal, low-grade intraepithelial squamous lesion (LSIL), and high-grade intraepithelial squamous lesion (HSIL). The capability of the developed screening system was tested using 700 FE-SEM/EDX spectra (300 normal, 200 LSIL, and 200 HSIL cases). The accuracy, sensitivity, and specificity performances were 98.2%, 99.0%, and 98.0%, respectively.

  12. Scanning Electron Microscopy and Energy Dispersive X-ray Spectroscopy Studies on Processed Tooth Graft Material by Vacuum-ultrasonic Acceleration.

    PubMed

    Lee, Eun-Young; Kim, Eun-Suk; Kim, Kyung-Won

    2014-05-01

    The current gold standard for clinical jawbone formation involves autogenous bone as a graft material. In addition, demineralized dentin can be an effective graft material. Although demineralized dentin readily induces heterotopic bone formation, conventional decalcification takes three to five days, so, immediate bone grafting after extraction is impossible. This study evaluated the effect of vacuum ultrasonic power on the demineralization and processing of autogenous tooth material and documented the clinical results of rapidly processed autogenous demineralized dentin (ADD) in an alveolar defects patient. The method involves the demineralization of extracted teeth with detached soft tissues and pulp in 0.6 N HCl for 90 minutes using a heat controlled vacuum-ultrasonic accelerator. The characteristics of processed teeth were evaluated by scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). Bone grafting using ADD was performed for narrow ridges augmentation in the mandibular area. The new processing method was completed within two hours regardless of form (powder or block). EDS and SEM uniformly demineralized autotooth biomaterial. After six months, bone remodeling was observed in augmented sites and histological examination showed that ADD particles were well united with new bone. No unusual complications were encountered. This study demonstrates the possibility of preparing autogenous tooth graft materials within two hours, allowing immediate one-day grafting after extraction.

  13. Epitaxial BaTiO3(100) films on Pt(100): a low-energy electron diffraction, scanning tunneling microscopy, and x-ray photoelectron spectroscopy study.

    PubMed

    Förster, Stefan; Huth, Michael; Schindler, Karl-Michael; Widdra, Wolf

    2011-09-14

    The growth of epitaxial ultrathin BaTiO(3) films on a Pt(100) substrate has been studied by scanning tunneling microscopy (STM), low-energy electron diffraction (LEED), and x-ray photoelectron spectroscopy (XPS). The films have been prepared by radio-frequency-assisted magnetron sputter deposition at room temperature and develop a long-range order upon annealing at 900 K in O(2). By adjusting the Ar and O(2) partial pressures of the sputter gas, the stoichiometry was tuned to match that of a BaTiO(3)(100) single crystal as determined by XPS. STM reveals the growth of continuous BaTiO(3) films with unit cell high islands on top. With LEED already for monolayer thicknesses, the formation of a BaTiO(3)(100)-(1 × 1) structure has been observed. Films of 2-3 unit cell thickness show a brilliant (1 × 1) LEED pattern for which an extended set of LEED I-V data has been acquired. At temperatures above 1050 K the BaTiO(3) thin film starts to decay by formation of vacancy islands. In addition (4 × 4) and (3 × 3) surface reconstructions develop upon prolonged heating.

  14. Scanning Electron Microscopy-Energy-Dispersive X-Ray (SEM/EDX): A Rapid Diagnostic Tool to Aid the Identification of Burnt Bone and Contested Cremains.

    PubMed

    Ellingham, Sarah T D; Thompson, Tim J U; Islam, Meez

    2017-06-12

    This study investigates the use of Scanning electron microscopy-energy-dispersive X-ray (SEM-EDX) as a diagnostic tool for the determination of the osseous origin of samples subjected to different temperatures. Sheep (Ovis aries) ribs of two experimental groups (fleshed and defleshed) were burned at temperatures of between 100°C and 1100°C in 100°C increments and subsequently analyzed with the SEM-EDX to determine the atomic percentage of present elements. Three-factor ANOVA analysis showed that neither the exposure temperature, nor whether the burning occurred with or without soft tissue present had any significant influence on the bone's overall elemental makeup (p > 0.05). The Ca/P ratio remained in the osseous typical range of between 1.6 and 2.58 in all analyzed samples. This demonstrates that even faced with high temperatures, the overall gross elemental content and atomic percentage of elements in bone remain stable, creating a unique "fingerprint" for osseous material, even after exposure to extreme conditions. © 2017 American Academy of Forensic Sciences.

  15. Screening of cadmium and copper phytoremediation ability of Tagetes erecta, using biochemical parameters and scanning electron microscopy-energy-dispersive X-ray microanalysis.

    PubMed

    Goswami, Sunayana; Das, Suchismita

    2017-09-01

    Tagetes erecta thrived in phytotoxic levels of cadmium (Cd; 50-300 mg kg(-1) ) and copper (Cu; 150-400 mg kg(-1) ) for 21 d. It accumulated high metal contents in its above-ground tissues (3675 mg Cd kg(-1) dry wt and 3948 mg Cu kg(-1) dry wt) and showed greater root to shoot translocation and a high extraction coefficient, all of which pointed toward its potential as a hyperaccumulator. Both Cd stress and Cu stress reduced the plant biomass, foliar area, and number. In addition, there were significant declines in pigment contents as well as boosts in lipid peroxidation levels. However, the plant triggered a number of stress-mitigation strategies to abate reactive oxygen species formed as a result of Cd/Cu excess, mostly via significant augmentation of superoxide dismutase, catalase, glutathione peroxidase, and ascorbate peroxidase activities. Though the root and leaf anatomy revealed some signs of toxic symptoms at 50 mg Cd kg(-1) and at 150 mg Cu kg(-1) , as evidenced by scanning electron microscopy, the root showed maximum tolerance, with tolerance indexes of 85.4% and 91.7%, respectively. Energy-dispersive X-ray microanalysis showed specific Ca(2+) signals in both root and stomata, which could be associated with a specific signaling pathway leading to increased root metal uptake and stomatal closure. Environ Toxicol Chem 2017;36:2533-2542. © 2017 SETAC. © 2017 SETAC.

  16. Surface characterization of 7S and 11S globulin powders from soy protein examined by X-ray photoelectron spectroscopy and scanning electron microscopy.

    PubMed

    Zhao, Xiaoyan; Chen, Jun; Zhu, Qingjun; Du, Fangling; Ao, Qiang; Liu, Jie

    2011-09-01

    In this study the surface composition of 7S and 11S globulin powders from soybean proteins by aqueous buffer and reverse micelle extractions had been examined using X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Analysis by XPS revealed that the O and N atomic percentage of 7S and 11S globulin surfaces from bis(2-ethylhexyl) sodium sulfosuccinate (AOT) reverse micelle was higher than from aqueous buffer, but the C atomic percentage was lower. The O/C ratio of the 7S globulin powder from aqueous buffer and reverse micelle was similar while significant differences were obtained in the O/C ratio of the 11S globulin powder, N/C atom ratios of the 7S and 11S globulin powders and high-resolution XPS C 1s, N 1s, O 1s spectra. Powder microstructure after reverse micelle treatment showed the presence of small pores, indicating the effect of reverse micelle on the 7S and 11S globulin structure. The obtained results indicated that the reverse micelle could affect the C, O and N components on the surface of soybean proteins. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. Combining scanning probe microscopy and x-ray spectroscopy

    PubMed Central

    2011-01-01

    A new versatile tool, combining Shear Force Microscopy and X-Ray Spectroscopy was designed and constructed to obtain simultaneously surface topography and chemical mapping. Using a sharp optical fiber as microscope probe, it is possible to collect locally the visible luminescence of the sample. Results of tests on ZnO and on ZnWO4 thin layers are in perfect agreement with that obtained with other conventional techniques. Twin images obtained by simultaneous acquisition in near field of surface topography and of local visible light emitted by the sample under X-Ray irradiation in synchrotron environment are shown. Replacing the optical fibre by an X-ray capillary, it is possible to collect local X-ray fluorescence of the sample. Preliminary results on Co-Ti sample analysis are presented. PMID:21711848

  18. Hard X-ray Microscopy with Multilayer Laue Lenses

    NASA Astrophysics Data System (ADS)

    Kang, Hyon Chol

    2011-03-01

    The possibility of imaging at near-atomic resolution using x-rays has been a dream ever since the short-wavelength nature of x-rays was demonstrated by von Laue and coworkers nearly a century ago. Even today the scientific impact of atomic-scale focusing of electromagnetic radiation would be deep and broad, because x-ray microscopy provides capabilities (ability to penetrate, sensitive and accurate elemental and structural information) that are complementary to other high-resolution microscopies. Although hard x-rays can in principle be focused to spot sizes on the order of their wavelength (0.1 nm), this limit has never been approached because of the difficulty in fabricating the optics. Multilayer Laue lens(MLL) is a novel diffractive optic for hard x-ray nano-focusing, which can be fabricated by sputter deposition of zone plate structure on flat substrate. According to the theoretical results, MLL is capable of focusing x-rays to well below 1 nm. We have demonstrated 2-dimensional focusing of hard x-rays with MLLs to a spot size of 25 nm x 27 nm with an efficiency of 2% at a photon energy of 12 keV, while 1-dimensional focus of 16 nm has been achieved. In this talk, we will present an overview of MLL microscopy and recent accomplishments for the determination of chemical composition in nanoscale systems. Lastly, we will give the capabilities of MLL microscopy that have the potential to significantly advance materials science, nanoscience, bio-medical science and environmental science.

  19. Broadband X-ray full field microscopy at a superbend

    NASA Astrophysics Data System (ADS)

    Stampanoni, M.; Marone, F.; Mikuljan, G.; Jefimovs, K.; Trtik, P.; Vila-Comamala, J.; David, C.; Abela, R.

    2009-09-01

    Over the last decade, synchrotron-radiation based X-ray Tomographic Microscopy (SRXTM) has established itself as a fundamental tool for non-invasive, quantitative investigations of a broad variety of samples, with application ranging from space research and materials science to biology and medicine. The beamline for TOmographic Microscopy and Coherent rAdiology experimenTs (TOMCAT) has been recently equipped with a full field, hard X-ray microscope with a theoretical pixel size down to 30 nm and a field of view of 50 microns. The nanoscope performs well at X-ray energies between 8 and 12 keV: here we illustrate the experimental setup and the performance of the instrument in both microscopy and tomography mode.

  20. The effect of phytostabilization on Zn speciation in a dredged contaminated sediment using scanning electron microscopy, X-ray fluorescence, EXAFS spectroscopy, and principal components analysis

    NASA Astrophysics Data System (ADS)

    Panfili, Frédéric; Manceau, Alain; Sarret, Géraldine; Spadini, Lorenzo; Kirpichtchikova, Tatiana; Bert, Valérie; Laboudigue, Agnès; Marcus, Matthew A.; Ahamdach, Noureddine; Libert, Marie-Françoise

    2005-05-01

    The maintenance of waterways generates large amounts of dredged sediments, which are deposited on adjacent land surfaces. These sediments are often rich in metal contaminants and present a risk to the local environment. Understanding how the metals are immobilized at the molecular level is critical for formulating effective metal containment strategies such as phytoremediation. In the present work, the mineralogical transformations of Zn-containing phases induced by two graminaceous plants (A grostis tenuis and Festuca rubra) in a contaminated sediment ([Zn] = 4700 mg kg -1, [P 2O 5] = 7000 mg kg -1, pH = 7.8), untreated or amended with hydroxylapatite (AP) or Thomas basic slag (TS), were investigated after two yr of pot experiment by scanning electron microscopy coupled with energy-dispersive spectrometry (SEM-EDS), synchrotron-based X-ray microfluorescence (μ-SXRF), and powder and laterally resolved extended X-ray absorption fine structure (μ-EXAFS) spectroscopy. The number and nature of Zn species were evaluated by principal component (PCA) and least-squares fitting (LSF) analysis of the entire set of μ-EXAFS spectra, which included up to 32 individual spectra from regions of interest varying in chemical composition. Seven Zn species were identified at the micrometer scale: sphalerite, gahnite, franklinite, Zn-containing ferrihydrite and phosphate, (Zn-Al)-hydrotalcite, and Zn-substituted kerolite-like trioctahedral phyllosilicate. Bulk fractions of each species were quantified by LSF of the powder EXAFS spectra to linear combinations of the identified Zn species spectra. In the untreated and unvegetated sediment, Zn was distributed as ˜50% (mole ratio of total Zn) sphalerite, ˜40% Zn-ferrihydrite, and ˜10 to 20% (Zn-Al)-hydrotalcite plus Zn-phyllosilicate. In unvegetated but amended sediments (AP and TS), ZnS and Zn-ferrihydrite each decreased by 10 to 20% and were replaced by Zn-phosphate (˜30˜40%). In the presence of plants, ZnS was almost completely

  1. The growth of epitaxial iron oxides on platinum (111) as studied by X-ray photoelectron diffraction, scanning tunneling microscopy, and low energy electron diffraction

    SciTech Connect

    Kim, Yong -Joo

    1995-05-01

    Three complementary surface structure probes, x-ray photoelectron diffraction (XPD), scanning tunneling microscopy (STM), and low-energy electron diffraction (LEED) have been combined in a single instrument. This experimental system has been utilized to study the structure and growth mechanisms of iron oxide films on Pt(111); these films were formed by first depositing a single overlayer of Fe with a certain coverage in monolayers (ML`s), and then thermally oxidizing it in an oxygen atmosphere. For films up to ~1 ML in thickness, a bilayer of Fe and O similar to those in FeO(111) is found to form. In agreement with prior studies, STM and LEED show this to be an incommensurate oxide film forming a lateral superlattice with short- and long-range periodicities of ~3.1 Å and ~26.0 Å. XPD in addition shows a topmost oxygen layer to be relaxed inward by -0.6 Å compared to bulk FeO(111), and these are new structural conclusions. The oxygen stacking in the FeO(111) bilayer is dominated by one of two possible binding sites. For thicker iron oxide films from 1.25 ML to 3.0 ML, the growth mode is essentially Stranski-Krastanov: iron oxide islands form on top of the FeO(111) bilayer mentioned above. For iron oxide films of 3.0 ML thickness, x-ray photoelectron spectroscopy (XPS) yields an Fe 2p3/2 binding energy and an Fe:O stoichiometry consistent with the presence of Fe3O4. Our XPD data further prove this overlayer to be Fe3O4(111)-magnetite in two almost equally populated domains with a 180° rotation between them. The structural parameters for this Fe3O4 overlayer generally agree with those of a previous LEED study, except that we find a significant difference in the first Fe-O interplanar spacing. This work demonstrates the considerable benefits to be derived by using this set of complementary surface structure probes in such epitaxial growth studies.

  2. Contact microscopy with a soft x-ray laser

    SciTech Connect

    DiCicco, D.S.; Kim, D.; Rosser, R.J.; Skinner, C.H.; Suckewer, S.; Gupta, A.P.; Hirschberg, J.G.

    1989-03-01

    A soft x-ray laser of output energy 1-3 mJ at 19.2 nm has been used to record high resolution images of biological specimens. The contact images were recorded on photoresist which was later viewed in a scanning electron microscope. We also present a Composite Optical X- ray Laser Microscope ''COXRALM'' of novel design. 14 refs., 8 figs., 1 tab.

  3. X-ray dense cellular inclusions in the cells of the green alga Chlamydomonas reinhardtii as seen by soft-x-ray microscopy

    SciTech Connect

    Stead, A.D.; Ford, T.W.; Page, A.M.; Brown, J.T.; Meyer-Ilse, W.

    1997-04-01

    Soft x-rays, having a greater ability to penetrate biological material than electrons, have the potential for producing images of intact, living cells. In addition, by using the so-called {open_quotes}water window{close_quotes} area of the soft x-ray spectrum, a degree of natural contrast is introduced into the image due to differential absorption of the wavelengths by compounds with a high carbon content compared to those with a greater oxygen content. The variation in carbon concentration throughout a cell therefore generates an image which is dependent upon the carbon density within the specimen. Using soft x-ray contact microscopy the authors have previously examined the green alga Chlamydomonas reinhardtii, and the most prominent feature of the cells are the numerous x-ray absorbing spheres, But they were not seen by conventional transmission electron microscopy. Similar structures have also been reported by the Goettingen group using their cryo transmission x-ray microscope at BESSY. Despite the fact that these spheres appear to occupy up to 20% or more of the cell volume when seen by x-ray microscopy, they are not visible by transmission electron microscopy. Given the difficulties and criticisms associated with soft x-ray contact microscopy, the present study was aimed at confirming the existence of these cellular inclusions and learning more of their possible chemical composition.

  4. High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

    SciTech Connect

    Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Marchesini, Stephano; Neiman, Aaron M.; Turner, Joshua J.; Jacobsen, Chris

    2010-04-20

    X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane and freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.

  5. High-resolution x-ray diffraction microscopy of specifically labeled yeast cells

    DOE PAGES

    Nelson, Johanna; Huang, Xiaojing; Steinbrener, Jan; ...

    2010-04-20

    X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11-13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane andmore » freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.« less

  6. X-ray induced chemical reaction revealed by in-situ X-ray diffraction and scanning X-ray microscopy in 15 nm resolution (Conference Presentation)

    NASA Astrophysics Data System (ADS)

    Ge, Mingyuan; Liu, Wenjun; Bock, David; De Andrade, Vincent; Yan, Hanfei; Huang, Xiaojing; Marschilok, Amy; Takeuchi, Esther; Xin, Huolin; Chu, Yong S.

    2016-09-01

    The detection sensitivity of synchrotron-based X-ray techniques has been largely improved due to the ever increasing source brightness, which have significantly advanced ex-situ and in-situ research for energy materials, such as lithium-ion batteries. However, the strong beam-matter interaction arisen from the high beam flux can significantly modify the material structure. The parasitic beam-induced effect inevitably interferes with the intrinsic material property, which brings difficulties in interpreting experimental results, and therefore requires comprehensive evaluation. Here we present a quantitative in-situ study of the beam-effect on one electrode material Ag2VO2PO4 using four different X-ray probes with different radiation dose rate. The material system we reported exhibits interesting and reversible radiation-induced thermal and chemical reactions, which was further evaluated under electron microscopy to illustrate the underlying mechanism. The work we presented here will provide a guideline in using synchrotron X-rays to distinguish the materials' intrinsic behavior from extrinsic structure changed induced by X-rays, especially in the case of in-situ and operando study where the materials are under external field of either temperature or electric field.

  7. Structural studies of technetium-zirconium alloys by X-ray diffraction, high-resolution electron microscopy, and first-principles calculations.

    PubMed

    Poineau, Frederic; Hartmann, Thomas; Weck, Philippe F; Kim, Eunja; Silva, G W Chinthaka; Jarvinen, Gordon D; Czerwinski, Kenneth R

    2010-02-15

    The structural properties of Tc-Zr binary alloys were investigated using combined experimental and computational approaches. The Tc(2)Zr and Tc(6)Zr samples were characterized by X-ray diffraction analysis, scanning electron microscopy, electron probe microanalysis, and transmission electron microscopy. Our XRD results show that Tc(6)Zr crystallizes in the cubic alpha-Mn-type structure (I43m space group) with a variable stoichiometry of Tc(6.25-x)Zr (0 < x < 1.45), and Tc(2)Zr has a hexagonal crystal lattice with a MgZn(2)-type structure (P6(3)/mmc space group). Rietveld analysis of the powder XRD patterns and density functional calculations of the "Tc(6)Zr" phase show a linear increase of the lattice parameter when moving from Tc(6.25)Zr to Tc(4..80)Zr compositions, similar to previous observations in the Re-Zr system. This variation of the composition of "Tc(6)Zr" is explained by the substitution of Zr for Tc atoms in the 2a site of the alpha-Mn-type structure. These results suggest that the width of the "Tc(6)Zr" phase needs to be included when constructing the Tc-Zr phase diagram. The bonding character and stability of the various Tc-Zr phases were also investigated from first principles. Calculations indicate that valence and conduction bands near the Fermi level are dominated by electrons occupying the 4d orbital. In particular, the highest-lying molecular orbitals of the valence band of Tc(2)Zr are composed of d-d sigma bonds, oriented along the normal axis of the (110) plane and linking the Zr network to the Tc framework. Strong d-d bonds stabilizing the Tc framework in the hexagonal unit cell are also in the valence band. In the cubic structures of Tc-Zr phases, only Tc 4d orbitals are found to significantly contribute near the Fermi level.

  8. High spatial resolution soft-x-ray microscopy

    SciTech Connect

    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 to 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.

  9. Biological imaging by soft x-ray diffraction microscopy

    SciTech Connect

    Shapiro, D.; Thibault, P.; Beetz, T.; Elser, V.; Howells, M.; Jacobsen, C.; Kirz, J.; Lima, E.; Miao, H.; Neiman, A. M.; Sayre, D.

    2005-10-25

    We have used the method of x-ray diffraction microscopy to image the complex-valued exit wave of an intact and unstained yeast cell. The images of the freeze-dried cell, obtained by using 750-eV x-rays from different angular orientations, portray several of the cell's major internal components to 30-nm resolution. The good agreement among the independently recovered structures demonstrates the accuracy of the imaging technique. To obtain the best possible reconstructions, we have implemented procedures for handling noisy and incomplete diffraction data, and we propose a method for determining the reconstructed resolution. This work represents a previously uncharacterized application of x-ray diffraction microscopy to a specimen of this complexity and provides confidence in the feasibility of the ultimate goal of imaging biological specimens at 10-nm resolution in three dimensions.

  10. Biological imaging by soft x-ray diffraction microscopy

    DOE PAGES

    Shapiro, D.; Thibault, P.; Beetz, T.; ...

    2005-10-25

    We have used the method of x-ray diffraction microscopy to image the complex-valued exit wave of an intact and unstained yeast cell. The images of the freeze-dried cell, obtained by using 750-eV x-rays from different angular orientations, portray several of the cell's major internal components to 30-nm resolution. The good agreement among the independently recovered structures demonstrates the accuracy of the imaging technique. To obtain the best possible reconstructions, we have implemented procedures for handling noisy and incomplete diffraction data, and we propose a method for determining the reconstructed resolution. This work represents a previously uncharacterized application of x-ray diffractionmore » microscopy to a specimen of this complexity and provides confidence in the feasibility of the ultimate goal of imaging biological specimens at 10-nm resolution in three dimensions.« less

  11. Applications of Hard X-ray Full-Field Transmission X-ray Microscopy at SSRL

    NASA Astrophysics Data System (ADS)

    Liu, Y.; Andrews, J. C.; Meirer, F.; Mehta, A.; Gil, S. Carrasco; Sciau, P.; Mester, Z.; Pianetta, P.

    2011-09-01

    State-of-the-art hard x-ray full-field transmission x-ray microscopy (TXM) at beamline 6-2C of Stanford Synchrotron Radiation Lightsource has been applied to various research fields including biological, environmental, and material studies. With the capability of imaging a 32-micron field-of-view at 30-nm resolution using both absorption mode and Zernike phase contrast, the 3D morphology of yeast cells grown in gold-rich media was investigated. Quantitative evaluation of the absorption coefficient was performed for mercury nanoparticles in alfalfa roots exposed to mercury. Combining XANES and TXM, we also performed XANES-imaging on an ancient pottery sample from the Roman pottery workshop at LaGraufesenque (Aveyron).

  12. In Operando X-ray diffraction and transmission X-ray microscopy of lithium sulfur batteries.

    PubMed

    Nelson, Johanna; Misra, Sumohan; Yang, Yuan; Jackson, Ariel; Liu, Yijin; Wang, Hailiang; Dai, Hongjie; Andrews, Joy C; Cui, Yi; Toney, Michael F

    2012-04-11

    Rechargeable lithium-sulfur (Li-S) batteries hold great potential for high-performance energy storage systems because they have a high theoretical specific energy, low cost, and are eco-friendly. However, the structural and morphological changes during electrochemical reactions are still not well understood. In this Article, these changes in Li-S batteries are studied in operando by X-ray diffraction and transmission X-ray microscopy. We show recrystallization of sulfur by the end of the charge cycle is dependent on the preparation technique of the sulfur cathode. On the other hand, it was found that crystalline Li(2)S does not form at the end of discharge for all sulfur cathodes studied. Furthermore, during cycling the bulk of soluble polysulfides remains trapped within the cathode matrix. Our results differ from previous ex situ results. This highlights the importance of in operando studies and suggests possible strategies to improve cycle life.

  13. Applications of Hard X-ray Full-Field Transmission X-ray Microscopy at SSRL

    SciTech Connect

    Liu, Y.; Andrews, J. C.; Mehta, A.; Pianetta, P.; Meirer, F.; Gil, S. Carrasco; Sciau, P.; Mester, Z.

    2011-09-09

    State-of-the-art hard x-ray full-field transmission x-ray microscopy (TXM) at beamline 6-2C of Stanford Synchrotron Radiation Lightsource has been applied to various research fields including biological, environmental, and material studies. With the capability of imaging a 32-micron field-of-view at 30-nm resolution using both absorption mode and Zernike phase contrast, the 3D morphology of yeast cells grown in gold-rich media was investigated. Quantitative evaluation of the absorption coefficient was performed for mercury nanoparticles in alfalfa roots exposed to mercury. Combining XANES and TXM, we also performed XANES-imaging on an ancient pottery sample from the Roman pottery workshop at LaGraufesenque (Aveyron).

  14. Zernike phase contrast in scanning microscopy with X-rays

    PubMed Central

    Holzner, Christian; Feser, Michael; Vogt, Stefan; Hornberger, Benjamin; Baines, Stephen B.; Jacobsen, Chris

    2011-01-01

    Scanning X-ray microscopy focuses radiation to a small spot and probes the sample by raster scanning. It allows information to be obtained from secondary signals such as X-ray fluorescence, which yields an elemental mapping of the sample not available in full-field imaging. The analysis and interpretation from these secondary signals can be considerably enhanced if these data are coupled with structural information from transmission imaging. However, absorption often is negligible and phase contrast has not been easily available. Originally introduced with visible light, Zernike phase contrast1 is a well-established technique in full-field X-ray microscopes for visualization of weakly absorbing samples2–7. On the basis of reciprocity, we demonstrate the implementation of Zernike phase contrast in scanning X-ray microscopy, revealing structural detail simultaneously with hard-X-ray trace-element measurements. The method is straightforward to implement without significant influence on the resolution of the fluorescence images and delivers complementary information. We show images of biological specimens that clearly demonstrate the advantage of correlating morphology with elemental information. PMID:21544232

  15. Zernike phase contrast in scanning microscopy with X-rays.

    PubMed

    Holzner, Christian; Feser, Michael; Vogt, Stefan; Hornberger, Benjamin; Baines, Stephen B; Jacobsen, Chris

    2010-11-01

    Scanning X-ray microscopy focuses radiation to a small spot and probes the sample by raster scanning. It allows information to be obtained from secondary signals such as X-ray fluorescence, which yields an elemental mapping of the sample not available in full-field imaging. The analysis and interpretation from these secondary signals can be considerably enhanced if these data are coupled with structural information from transmission imaging. However, absorption often is negligible and phase contrast has not been easily available. Originally introduced with visible light, Zernike phase contrast(1) is a well-established technique in full-field X-ray microscopes for visualization of weakly absorbing samples(2-7). On the basis of reciprocity, we demonstrate the implementation of Zernike phase contrast in scanning X-ray microscopy, revealing structural detail simultaneously with hard-X-ray trace-element measurements. The method is straightforward to implement without significant influence on the resolution of the fluorescence images and delivers complementary information. We show images of biological specimens that clearly demonstrate the advantage of correlating morphology with elemental information.

  16. Orthogonal identification of gunshot residue with complementary detection principles of voltammetry, scanning electron microscopy, and energy-dispersive X-ray spectroscopy: sample, screen, and confirm.

    PubMed

    O'Mahony, Aoife M; Samek, Izabela A; Sattayasamitsathit, Sirilak; Wang, Joseph

    2014-08-19

    Field-deployable voltammetric screening coupled with complementary laboratory-based analysis to confirm the presence of gunshot residue (GSR) from the hands of a subject who has handled, loaded, or discharged a firearm is described. This protocol implements the orthogonal identification of the presence of GSR utilizing square-wave stripping voltammetry (SWSV) as a rapid screening tool along with scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) to confirm the presence of the characteristic morphology and metal composition of GSR particles. This is achieved through the judicious modification of the working electrode of a carbon screen-printed electrode (CSPE) with carbon tape (used in SEM analysis) to fix and retain a sample. A comparison between a subject who has handled and loaded a firearm and a subject who has had no contact with GSR shows the significant variations in voltammetric signals and the presence or absence of GSR-consistent particles and constituent metals. This initial electrochemical screening has no effect on the integrity of the metallic particles, and SEM/EDX analysis conducted prior to and postvoltammetry show no differences in analytical output. The carbon tape is instrumental in retaining the GSR sample after electrochemical analysis, supported by comparison with orthogonal detection at a bare CSPE. This protocol shows great promise as a two-tier detection system for the presence of GSR from the hands of a subject, whereby initial screening can be conducted rapidly onsite by minimally trained operators; confirmation can follow at the same substrate to substantiate the voltammetric results.

  17. Mercury intake by inflammatory phagocytes: in vivo cytology of mouse macrophages and neutrophils by X-ray elemental microanalysis coupled with scanning electron microscopy.

    PubMed

    Cunha, Elisabete M; Oliveira, Maria João R; Ferreira, Paula G; Aguas, Artur P

    2004-08-01

    Phagocytes remove and store mercury (Hg) that enters the body. Macrophages and granulocytes respond in opposite ways to Hg: macrophages loose cell viability, and neutrophils become protected from apoptosis. We have investigated the cytology of early intake of Hg by macrophages and neutrophils after a short period (2-4 min) of in vivo exposure to HgCl2. The two types of phagocytes were attracted either to a subcutaneous air pouch or to the peritoneal cavity of BALB/c mice by in situ BSA injection. BSA caused, 72 hours later, inflammatory exudates where neutrophils (air-pouch cavity) or macrophages (peritoneal cavity) were the predominant cell type. A lethal dose of HgCl2 (25 mg) was then injected in the two inflammatory cavities. The mice died 2-4 min later and the cell exudates were harvested and studied by scanning electron microscopy coupled with X-ray elemental microanalysis (SEM-XRM). More than half of the phagocytes showed ingested Hg; a higher percentage of macrophages (around 70%) than neutrophils (around 50%) were positive for the metal. Intracellular particles of Hg were spheroid and presented a small diameter (less than 20 nm). They could be seen in large numbers inside phagocytes (up to 20-30 Hg dots per cell); they were scattered throughout the cytoplasm of the cells. The ability of phagocytes to ingest Hg increased as the BSA-induced inflammation progressed. We conclude that (i) Hg is quickly ingested as small particles by phagocytes; (ii) endocytosis of Hg increases with the degree of activation of phagocytes; and (iii) phagocytes internalize Hg by pinocytosis.

  18. X-Ray diffraction and scanning electron microscopy-energy dispersive spectroscopic analysis of ceramõmetal interface at different firing temperatures

    PubMed Central

    Saini, Monika; Chandra, Suresh; Singh, Yashpal; Basu, Bikramjit; Tripathi, Arvind

    2010-01-01

    Objective: Porcelain chipping from porcelain fused to metal restoration has been Achilles heel till date. There has been advent of newer ceramics in past but but none of them has been a panacea for Porcelain fracture. An optimal firing is thus essential for the clinical success of the porcelain-fused to metal restoration. The aim of the present study was to evaluate ceramo-metal interface at different firing temperature using XRD and SEM-EDS analysis. Clinical implication of the study was to predict the optimal firing temperature at which porcelain should be fused with metal in order to possibly prevent the occasional failure of the porcelain fused to metal restorations. Materials and Methods: To meet the above-mentioned goal, porcelain was fused to metal at different firing temperatures (930–990°C) in vacuum. The microstructural observations of interface between porcelain and metal were evaluated using X-ray diffraction and scanning electron microscopy with energy dispersive spectroscopy. Results: Based on the experimental investigation of the interaction zone of porcelain fused to metal samples, it was observed that as the firing temperature was increased, the pores became less in number as well as the size of the pores decreased at the porcelain/metal interface upto 975°C but increased in size at 990°C. The least number of pores with least diameter were found in samples fired at 975°C. Several oxides like Cr2O3, NiO, and Al2O3 and intermetallic compounds (CrSi2, AlNi3) were also formed in the interaction zone. Conclusions It is suggested that the presence of pores may trigger the crack propagation along the interface, causing the failure of the porcelain fused to metal restoration during masticatory action. PMID:22114406

  19. Twin domain imaging in topological insulator Bi2Te3 and Bi2Se3 epitaxial thin films by scanning X-ray nanobeam microscopy and electron backscatter diffraction

    PubMed Central

    Harcuba, Petr; Veselý, Jozef; Lesnik, Andreas; Bauer, Guenther; Springholz, Gunther; Holý, Václav

    2017-01-01

    The twin distribution in topological insulators Bi2Te3 and Bi2Se3 was imaged by electron backscatter diffraction (EBSD) and scanning X-ray diffraction microscopy (SXRM). The crystal orientation at the surface, determined by EBSD, is correlated with the surface topography, which shows triangular pyramidal features with edges oriented in two different orientations rotated in the surface plane by 60°. The bulk crystal orientation is mapped out using SXRM by measuring the diffracted X-ray intensity of an asymmetric Bragg peak using a nano-focused X-ray beam scanned over the sample. By comparing bulk- and surface-sensitive measurements of the same area, buried twin domains not visible on the surface are identified. The lateral twin domain size is found to increase with the film thickness. PMID:28381969

  20. Compact water-window transmission X-ray microscopy.

    PubMed

    Berglund, M; Rymell, L; Peuker, M; Wilhein, T; Hertz, H M

    2000-03-01

    We demonstrate sub-100 nm resolution water-window soft X-ray full-field transmission microscopy with a compact system. The microscope operates at lambda = 3.37 nm and is based on a 100 Hz table-top regenerative debris-free droplet-target laser-plasma X-ray source in combination with normal-incidence multilayer condenser optics for sample illumination. High-spatial-resolution imaging is performed with a 7.3% efficiency nickel zone plate and a 1024 x 1024 pixel CCD detector. Images of dry test samples are recorded with exposure times of a few minutes and show features smaller than 60 nm.

  1. Near-edge X-ray refraction fine structure microscopy

    DOE PAGES

    Farmand, Maryam; Celestre, Richard; Denes, Peter; ...

    2017-02-06

    We demonstrate a method for obtaining increased spatial resolution and specificity in nanoscale chemical composition maps through the use of full refractive reference spectra in soft x-ray spectro-microscopy. Using soft x-ray ptychography, we measure both the absorption and refraction of x-rays through pristine reference materials as a function of photon energy and use these reference spectra as the basis for decomposing spatially resolved spectra from a heterogeneous sample, thereby quantifying the composition at high resolution. While conventional instruments are limited to absorption contrast, our novel refraction based method takes advantage of the strongly energy dependent scattering cross-section and can seemore » nearly five-fold improved spatial resolution on resonance.« less

  2. Hard x-ray scanning microscopy with coherent radiation: Beyond the resolution of conventional x-ray microscopes

    SciTech Connect

    Schropp, A.; Hoppe, R.; Patommel, J.; Samberg, D.; Seiboth, F.; Stephan, S.; Schroer, C. G.; Wellenreuther, G.; Falkenberg, G.

    2012-06-18

    We demonstrate x-ray scanning coherent diffraction microscopy (ptychography) with 10 nm spatial resolution, clearly exceeding the resolution limits of conventional hard x-ray microscopy. The spatial resolution in a ptychogram is shown to depend on the shape (structure factor) of a feature and can vary for different features in the object. In addition, the resolution and contrast are shown to increase with increasing coherent fluence. For an optimal ptychographic x-ray microscope, this implies a source with highest possible brilliance and an x-ray optic with a large numerical aperture to generate the optimal probe beam.

  3. Studies on x-ray and UV emissions in electron cyclotron resonance x-ray source

    SciTech Connect

    Baskaran, R.; Selvakumaran, T. S.

    2008-02-15

    A novel electron cyclotron resonance x-ray source is constructed based on the ECR technique. In this paper, the possibility of using the ECR x-ray source for producing UV rays by optimizing the plasma parameters is explored. X-ray and UV emissions from the ECR x-ray source are carried out for argon, nitrogen, and CO{sub 2} plasma. The x-ray spectral and dose measurements are carried with NaI(Tl) based spectrometer and dosimeter, respectively. For UV measurement, a quartz window arrangement is made at the exit port and the UV intensity is measured at 5 cm from the quartz plate using UV meter. The x-ray and UV emissions are carried out for different microwave power levels and gas pressures. The x-ray emission is observed in the pressure range {<=}10{sup -5} Torr, whereas the UV emission is found to be negligible for the gas pressures <10{sup -5} Torr and it starts increasing in the pressure range between 10{sup -5} and 10{sup -3} Torr. At high-pressure range, collision frequency of electron-atom is large which leads to the higher UV flux. At low pressure, the electron-atom collision frequency is low and hence the electrons reach high energy and by hitting the cavity wall produces higher x-ray flux. By choosing proper experimental conditions and plasma gas species, the same source can be used as either an x-ray source or an UV source.

  4. X-ray microscopy for neural circuit reconstruction

    NASA Astrophysics Data System (ADS)

    Mizutani, Haruo; Takeda, Yoshihiro; Momose, Atsushi; Takeuchi, Akihisa; Takagi, Toshihisa

    2009-09-01

    Neural circuits in the central nervous system build our various higher brain functions. However, little is known about mechanisms underlying neuronal information processing in the brain. Anatomical graph structures of real neural networks will provide us with fundamental views to elucidate them. We aim at developing a three-dimensional atlas of neural circuits using high resolution hard X-ray microscopy by synchrotron radiation. We stained neurons of a complete brain from a mouse by the Golgi-Cox method. The heavy metals used in our procedure enhanced X-ray absorption and phase contrast. 3D images of fibriform axons and dendrites of various neurons were reconstructed by back projection. X-ray microscopy with a Talbot interferometer demonstrated finer histological structures of pyramidal neurons in the hippocampus and the cerebral cortex. This observation probably serves as a foundation for achieving a mammalian Connectome Project (identifying complete wiring diagrams of the brain) with X-ray nano-tomography in the near future.

  5. PREFACE: 9th International Conference on X-Ray Microscopy

    NASA Astrophysics Data System (ADS)

    Quitmann, Christoph; David, Christian; Nolting, Frithjof; Pfeiffer, Franz; Stampanoni, Marco

    2009-09-01

    Conference logo This volume compiles the contributions to the International Conference on X-Ray Microscopy (XRM2008) held on 20-25 July 2008 in Zurich, Switzerland. The conference was the ninth in a series which started in Göttingen in 1984. Over the years the XRM conference series has served as a forum bringing together all relevant players working on the development of methods, building instrumentation, and applying x-ray microscopy to challenging issues in materials science, condensed matter research, environmental science and biology. XRM2008 was attended by about 300 participants who followed 44 oral presentations and presented 220 posters. Conference photograph Figure 1: Participants of the XRM2008 conference gathered in front of the main building of the ETH-Zurich. The conference showed that x-ray microscopy has become a mature field resting on three pillars. The first are workhorse instruments available even to non-specialist users. These exist at synchrotron sources world-wide as well as in laboratories. They allow the application of established microscopy methods to solve scientific projects in areas as diverse as soil science, the investigation of cometary dust particles, magnetic materials, and the analysis of ancient parchments. Examples of all of these projects can be found in this volume. These instruments have become so well understood that now they are also commercially available. The second pillar is the continued development of methods. Methods like stroboscopic imaging, wet cells or high and low temperature environments add versatility to the experiments. Methods like phase retrieval and ptychographic imaging allow the retrieval of information which hitero was thought to be inaccessible. The third pillar is the extension of such instruments and methods to new photon sources. With x-ray free electron lasers on the horizon the XRM community is working to transfer their know-how to these novel sources which will offer unprecedented brightness and

  6. Development of scanning electron and x-ray microscope

    SciTech Connect

    Matsumura, Tomokazu Hirano, Tomohiko Suyama, Motohiro

    2016-01-28

    We have developed a new type of microscope possessing a unique feature of observing both scanning electron and X-ray images under one unit. Unlike former X-ray microscopes using SEM [1, 2], this scanning electron and X-ray (SELX) microscope has a sample in vacuum, thus it enables one to observe a surface structure of a sample by SEM mode, to search the region of interest, and to observe an X-ray image which transmits the region. For the X-ray observation, we have been focusing on the soft X-ray region from 280 eV to 3 keV to observe some bio samples and soft materials. The resolutions of SEM and X-ray modes are 50 nm and 100 nm, respectively, at the electron energy of 7 keV.

  7. Viewing spin structures with soft x-ray microscopy

    SciTech Connect

    Fischer, Peter

    2010-06-01

    The spin of the electron and its associated magnetic moment marks the basic unit for magnetic properties of matter. Magnetism, in particular ferromagnetism and antiferromagnetism is described by a collective order of these spins, where the interaction between individual spins reflects a competition between exchange, anisotropy and dipolar energy terms. As a result the energetically favored ground state of a ferromagnetic system is a rather complex spin configuration, the magnetic domain structure. Magnetism is one of the eldest scientific phenomena, yet it is one of the most powerful and versatile utilized physical effects in modern technologies, such as in magnetic storage and sensor devices. To achieve highest storage density, the relevant length scales, such as the bit size in disk drives is now approaching the nanoscale and as such further developments have to deal with nanoscience phenomena. Advanced characterization tools are required to fully understand the underlying physical principles. Magnetic microscopes using polarized soft X-rays offer a close-up view into magnetism with unique features, these include elemental sensitivity due to X-ray magnetic dichroism effects as contrast mechanism, high spatial resolution provided by state-of-the-art X-ray optics and fast time resolution limited by the inherent time structure of current X-ray sources, which will be overcome with the introduction of ultrafast and high brilliant X-ray sources.

  8. Performing elemental microanalysis with high accuracy and high precision by scanning electron microscopy/silicon drift detector energy-dispersive X-ray spectrometry (SEM/SDD-EDS).

    PubMed

    Newbury, Dale E; Ritchie, Nicholas W M

    Electron-excited X-ray microanalysis performed in the scanning electron microscope with energy-dispersive X-ray spectrometry (EDS) is a core technique for characterization of the microstructure of materials. The recent advances in EDS performance with the silicon drift detector (SDD) enable accuracy and precision equivalent to that of the high spectral resolution wavelength-dispersive spectrometer employed on the electron probe microanalyzer platform. SDD-EDS throughput, resolution, and stability provide practical operating conditions for measurement of high-count spectra that form the basis for peak fitting procedures that recover the characteristic peak intensities even for elemental combination where severe peak overlaps occur, such PbS, MoS2, BaTiO3, SrWO4, and WSi2. Accurate analyses are also demonstrated for interferences involving large concentration ratios: a major constituent on a minor constituent (Ba at 0.4299 mass fraction on Ti at 0.0180) and a major constituent on a trace constituent (Ba at 0.2194 on Ce at 0.00407; Si at 0.1145 on Ta at 0.0041). Accurate analyses of low atomic number elements, C, N, O, and F, are demonstrated. Measurement of trace constituents with limits of detection below 0.001 mass fraction (1000 ppm) is possible within a practical measurement time of 500 s.

  9. Transmission and emission x-ray microscopy: operation modes, contrast mechanisms and applications.

    PubMed

    Kaulich, Burkhard; Thibault, Pierre; Gianoncelli, Alessandra; Kiskinova, Maya

    2011-03-02

    Advances in microscopy techniques based on x-rays have opened unprecedented opportunities in terms of spatial resolution, combined with chemical and morphology sensitivity, to analyze solid, soft and liquid matter. The advent of ultrabright third and fourth generation photon sources and the continuous development of x-ray optics and detectors has pushed the limits of imaging and spectroscopic analysis to structures as small as a few tens of nanometers. Specific interactions of x-rays with matter provide elemental and chemical sensitivity that have made x-ray spectromicroscopy techniques a very attractive tool, complementary to other microscopies, for characterization in all actual research fields. The x-ray penetration power meets the demand to examine samples too thick for electron microscopes implementing 3D imaging and recently also 4D imaging which adds time resolution as well. Implementation of a variety of phase contrast techniques enhances the structural sensitivity, especially for the hard x-ray regime. Implementation of lensless or diffraction imaging helps to enhance the lateral resolution of x-ray imaging to the wavelength dependent diffraction limit.

  10. Evolution of titania nanotubes-supported WO{sub x} species by in situ thermo-Raman spectroscopy, X-ray diffraction and high resolution transmission electron microscopy

    SciTech Connect

    Cortes-Jacome, M.A.; Angeles-Chavez, C.; Morales, M.; Lopez-Salinas, E.; Toledo-Antonio, J.A.

    2007-10-15

    Structural evolution of WO{sub x} species on the surface of titania nanotubes was followed by in situ thermo-Raman spectroscopy. A total of 15 wt% of W atoms were loaded on the surface of a hydroxylated titania nanotubes by impregnation with ammonium metatungstate solution and then, the sample was thermally treated in a Linkam cell at different temperatures in nitrogen flow. The band characteristic of the W=O bond was observed at 962 cm{sup -1} in the dried sample, which vanished between 300 and 700 deg. C, and reappear again after annealing at 800 deg. C, along with a broad band centered at 935 cm{sup -1}, attributed to the v{sub 1} vibration of W=O in tetrahedral coordination. At 900 and 1000 deg. C, the broad band decomposed into four bands at 923, 934, 940 and 950 cm{sup -1}, corresponding to the symmetric and asymmetric vibration of W=O bonds in Na{sub 2}WO{sub 4} and Na{sub 2}W{sub 2}O{sub 7} phases as determined by X-ray diffraction and High resolution transmission electron microscopy (HRTEM). The structure of the nanotubular support was kept at temperatures below 450 deg. C, thereafter, it transformed into anatase being stabilized at temperatures as high as 900 deg. C. At 1000 deg. C, anatase phase partially converted into rutile. After annealing at 1000 deg. C, a core-shell model material was obtained, with a shell of ca. 5 nm thickness, composed of sodium tungstate nanoclusters, and a core composed mainly of rutile TiO{sub 2} phase. - Graphical abstract: Titania nanotubes loaded with 15 wt% W atoms were characterized from room temperature (rt) to 1000 deg. C by thermo-Raman spectroscopy in N{sub 2}. At 1000 deg. C, a core-shell model material was obtained, with a shell thickness of ca. 5 nm composed by nanoclusters of sodium tungstate, and a core composed mainly of rutile TiO{sub 2} phase.

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

    PubMed

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

    2017-08-18

    We have developed a new experimental platform for in situ scanning transmission electron microscope (STEM) energy dispersive X-ray spectroscopy (EDS) which allows real time, nanoscale, elemental and structural changes to be studied at elevated temperature (up to 1000 °C) and pressure (up to 1 atm). Here we demonstrate the first application of this approach to understand complex structural changes occurring during reduction of a bimetallic catalyst, PdCu supported on TiO2 , synthesized by wet impregnation. We reveal a heterogeneous evolution of nanoparticle size, distribution, and composition with large differences in reduction behavior for the two metals. We show that the data obtained is complementary to in situ STEM electron energy loss spectroscopy (EELS) and when combined with in situ X-ray absorption spectroscopy (XAS) allows correlation of bulk chemical state with nanoscale changes in elemental distribution during reduction, facilitating new understanding of the catalytic behavior for this important class of materials. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

  12. Elemental imaging of cartilage by scanning x-ray microscopy

    SciTech Connect

    Buckley, C.J.; Foster, G.F.; Burge, R.E. ); Ali, S.Y.; Scotchford, C.A. , Royal National Orthopaedic Hospital, Stanmore, Middlesex ); Kirz, J. ); Rivers, M.L. )

    1992-01-01

    Elemental imaging via scanning transmission x-ray microscopy (STXM) and scanning fluorescence x-ray microscopy (SFXM) has been used to image calcium deposits in cartilage. In the case of STXM, 0.1 {mu}m thick sections were imaged to investigate the proximity of calcium deposits in relation to chondrocyte cells. The resolution available was 0.5 {mu}m, and field widths of up to 25 {mu}m were used at this resolution. The resolution available in SFXM was 10 {mu}m, and field widths of up to 2 mm were used at this resolution on 5-{mu}m thick specimens. Together these techniques were used to map calcium deposits at the cellular level, and at the full tissue size level.

  13. X-ray fluorescence microscopy of olfactory receptor neurons

    NASA Astrophysics Data System (ADS)

    Dučić, T.; Breunig, E.; Schild, D.; Herbst, J.; Nováková, E.; Susini, J.; Tucoulu, R.; Salditt, T.

    2009-09-01

    We report a x-ray fluorescence microscopy study of cells and tissues from the olfactory system of Xenopus laevis. In this experiment we focus on sample preparation and experimental issues, and present first results of fluorescence maps of the elemental distribution of Cl, K, Ca, P, S and Na both in individual isolated neural cells and in cross-sections of the same tissue.

  14. Calcified-tissue investigations using synchrotron x-ray microscopy

    SciTech Connect

    Jones, K.W.; Spanne, P.; Schidlovsky, G.; Dejun, X. ); Bockman, R.S. . Medical Coll.); Rabinowitz, M.B. ); Hammond, P.B.; Bornschein, R.L. ); Hoeltzel, D.A. )

    1990-10-01

    Synchrotron x-ray microscopy (SXRM) in both emission and absorption modes has been used to examine elemental distributions in specimens of rat tibia, human deciduous teeth, and an orthopedic implant phantom. The work was performed with a spatial resolution of 8 {mu}m for the emission work and 25 {mu}m for the absorption work. The results illustrate the usefulness of SXRM for measurements of different types of calcified tissue. 3 figs.

  15. Stability of a Bifunctional Cu-Based Core@Zeolite Shell Catalyst for Dimethyl Ether Synthesis Under Redox Conditions Studied by Environmental Transmission Electron Microscopy and In Situ X-Ray Ptychography.

    PubMed

    Baier, Sina; Damsgaard, Christian D; Klumpp, Michael; Reinhardt, Juliane; Sheppard, Thomas; Balogh, Zoltan; Kasama, Takeshi; Benzi, Federico; Wagner, Jakob B; Schwieger, Wilhelm; Schroer, Christian G; Grunwaldt, Jan-Dierk

    2017-06-01

    When using bifunctional core@shell catalysts, the stability of both the shell and core-shell interface is crucial for catalytic applications. In the present study, we elucidate the stability of a CuO/ZnO/Al2O3@ZSM-5 core@shell material, used for one-stage synthesis of dimethyl ether from synthesis gas. The catalyst stability was studied in a hierarchical manner by complementary environmental transmission electron microscopy (ETEM), scanning electron microscopy (SEM) and in situ hard X-ray ptychography with a specially designed in situ cell. Both reductive activation and reoxidation were applied. The core-shell interface was found to be stable during reducing and oxidizing treatment at 250°C as observed by ETEM and in situ X-ray ptychography, although strong changes occurred in the core on a 10 nm scale due to the reduction of copper oxide to metallic copper particles. At 350°C, in situ X-ray ptychography indicated the occurrence of structural changes also on the µm scale, i.e. the core material and parts of the shell undergo restructuring. Nevertheless, the crucial core-shell interface required for full bifunctionality appeared to remain stable. This study demonstrates the potential of these correlative in situ microscopy techniques for hierarchically designed catalysts.

  16. A comparison of muscle thin filament models obtained from electron microscopy reconstructions and low-angle X-ray fibre diagrams from non-overlap muscle.

    PubMed

    Poole, Katrina J V; Lorenz, Michael; Evans, Gwyndaf; Rosenbaum, Gerd; Pirani, Alnoor; Craig, Roger; Tobacman, Larry S; Lehman, William; Holmes, Kenneth C

    2006-08-01

    The regulation of striated muscle contraction involves changes in the interactions of troponin and tropomyosin with actin thin filaments. In resting muscle, myosin-binding sites on actin are thought to be blocked by the coiled-coil protein tropomyosin. During muscle activation, Ca2+ binding to troponin alters the tropomyosin position on actin, resulting in cyclic actin-myosin interactions that accompany muscle contraction. Evidence for this steric regulation by troponin-tropomyosin comes from X-ray data [Haselgrove, J.C., 1972. X-ray evidence for a conformational change in the actin-containing filaments of verterbrate striated muscle. Cold Spring Habor Symp. Quant. Biol. 37, 341-352; Huxley, H.E., 1972. Structural changes in actin and myosin-containing filaments during contraction. Cold Spring Habor Symp. Quant. Biol. 37, 361-376; Parry, D.A., Squire, J.M., 1973. Structural role of tropomyosin in muscle regulation: analysis of the X-ray diffraction patterns from relaxed and contracting muscles. J. Mol. Biol. 75, 33-55] and electron microscope (EM) data [Spudich, J.A., Huxley, H.E., Finch, J., 1972. Regulation of skeletal muscle contraction. II. Structural studies of the interaction of the tropomyosin-troponin complex with actin. J. Mol. Biol. 72, 619-632; O'Brien, E.J., Gillis, J.M., Couch, J., 1975. Symmetry and molecular arrangement in paracrystals of reconstituted muscle thin filaments. J. Mol. Biol. 99, 461-475; Lehman, W., Craig, R., Vibert, P., 1994. Ca2+-induced tropomyosin movement in Limulus thin filaments revealed by three-dimensional reconstruction. Nature 368, 65-67] each with its own particular strengths and limitations. Here we bring together some of the latest information from EM analysis of single thin filaments from Pirani et al. [Pirani, A., Xu, C., Hatch, V., Craig, R., Tobacman, L.S., Lehman, W. (2005). Single particle analysis of relaxed and activated muscle thin filaments. J. Mol. Biol. 346, 761-772], with synchrotron X-ray data from non

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

    NASA Astrophysics Data System (ADS)

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

    2016-01-01

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

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

    SciTech Connect

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

    2016-01-28

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

  19. Ultrastructural and elemental imaging of biological specimens by soft x-ray contact microscopy

    SciTech Connect

    Panessa, B.J.; Hoffman, P. . Dept. of Orthopedics); Warren, J.B. ); Feder, R.; Sayre, D. . Thomas J. Watson Research Center)

    1980-01-01

    Soft X-ray contact microscopy offers a means of visualizing unstained as well as stained biological materials at better than 6 nm resolution. Soft X-ray imaging depends on differential absorption of incident soft (1--10nm wavelength) X-rays by the endogenous elements within a specimen. The advantages of using soft X-rays for imaging are: (1) reduced specimen damage during exposure; (2) ability to image hydrated specimens at atmospheric pressure; (3) ability to image specimens ranging in thickness from less than 40 nm to as much as 10{mu}m; and (4) ability to map the elemental composition of the specimen through observation of the differential absorption of properly chosen incident x-ray wavelengths. This paper explains the principles of image formation and demonstrates the use of soft X-ray contact microscopy with biological samples which could not readily be imaged in their natural form using conventional electron microscopy methods. Data are also presented on the recognition of compositional features in histochemically treated articular joint tissues. 30 refs., 15 figs.

  20. Striped domains of coarse-grained magnetite observed by X-ray photoemission electron microscopy as a source of the high remanence of granites in the Vredefort dome

    NASA Astrophysics Data System (ADS)

    Kubo, Hiroto; Nakamura, Norihiro; Kotsugi, Masato; Ohkochi, Takuo; Terada, Kentaro; Fukuda, Kohei

    2015-06-01

    The characteristics of a coarse-grained high-remanence magnetite obtained from shocked Vredefort granite were investigated by X-ray magnetic circular dichroism (XMCD) analysis and X-ray absorption spectroscopy (XAS). The study utilized a spectroscopic photoelectron low-energy electron emission microscope (SPELEEM) and was conducted in the SPring-8 large-synchrotron radiation facility. It is generally believed that the strong and stable bulk remanence of Vredefort granites is due to the presence of minerals that have been strongly magnetized by either an impact-generated magnetic field or terrestrial lightning strikes. Although coarse-grained magnetite is traditionally characterized by weak coercivity and remanence, the specimen used in the present study exhibited high coercivity and an intense remanent magnetization. The presence of hematite lamellae observed on the partially oxidized magnetite specimen indicated an array of striped domains, intensifying a remanence and coercivity. We also conducted XAS and XMCD analyses on a natural lodestone permanent magnet produced by lightning strikes; while maghemite was found to be present, no magnetic domain structures were observed. Considering that the nucleation of hematite lamellae on magnetite/maghemite grains is due to high-temperature oxidation, we attribute the intense remanent magnetization and magnetic hardening of Vredefort granites to post-impact hydrothermal activity.

  1. X-ray, scanning electron microscopy and electrical properties of synthetic fresnoite (Ba2TiSi2O8) ceramics

    NASA Astrophysics Data System (ADS)

    Roy, M.; Barbar, S. K.; Dave, P.; Jangid, S.; Bala, Indu

    2010-09-01

    Polycrystalline ceramic samples of fresnoite (Ba2TiSi2O8 or BTS) have been prepared by a standard solid-state reaction method using high-purity oxides and carbonates. For one set of compounds, in stoichiometric ratio BaCO3, TiO2 and SiO2 were melted at 1300°C and then sintered into pellet form, whereas the other set of compounds have been prepared without melting and sintered into pellet form at 1250°C. The formation of the single-phase compound and its structural parameters were investigated by X-ray diffraction followed by Rietveld refinement and scanning electron microscopic (SEM) techniques. A better agreement between the observed and calculated X-ray diffraction patterns was obtained by performing the Rietveld refinement with a structural model using the non-centrosymmetric space group P4bm. A better agreement between observed and calculated d-values shows that the lattice parameters calculated using the Rietveld refinement analysis are better than that of the earlier report so far. The activation energies of both compounds were calculated by measuring its dc electrical conductivities. The results are discussed in detail.

  2. Stacking disorder in silicon carbide supported cobalt crystallites: an X-ray diffraction, electron diffraction and high resolution electron microscopy study.

    PubMed

    du Plessis, H E; de Villiers, J P R; Tuling, A; Olivier, E J

    2016-11-21

    Supported cobalt Fischer-Tropsch catalysts are characteristically nanoparticulate and the reduced SiC supported catalyst was found to contain both HCP and FCC polymorphs. This is reflected in the powder XRD patterns and generally there is a poor fit between the experimental and calculated diffractograms. This was ascribed to small crystallite sizes and the occurrence of disorder, manifested as peak broadening and peak shifts. Selected area electron diffraction data of suitably oriented cobalt catalyst grains on silicon carbide supports show non-periodic disorder in the zone axis orientations that contain the common (001) (HCP) and (111) (FCC) reciprocal lattice planes. Both FCC and HCP polymorphs are present in the same grains and these show disorder mainly in the HCP component. The disorder is further examined using high angle annular dark field (HAADF) scanning transmission electron microscopy at atomic resolution and the stacking sequences elucidated. Random sequences of mainly FCC are interrupted by HCP sequences and twin surfaces with reverse stacking sequences are also present. This study highlights the presence of significant disorder in cobalt catalyst grains confirmed by HAADF microscopy.

  3. Laboratory source based full-field x-ray microscopy at 9 keV

    SciTech Connect

    Fella, C.; Balles, A.; Wiest, W.; Zabler, S.; Hanke, R.

    2016-01-28

    In the past decade, hard x-ray transmission microscopy experienced tremendous developments. With the avail-ability of efficient Fresnel zone plates, even set-ups utilizing laboratory sources were developed [1]. In order to improve the performance of these x-ray microscopes, novel approaches to fabricate optical elements [2] and brighter x-ray tubes [3] are promising candidates. We are currently building a laboratory transmission x-ray microscope for 9.25 keV, using an electron impact liquid-metal-jet anode source. Up to now, the further elements of our setup are: a polycapillary condenser, a tungsten zone plate, and a scintillator which is optically coupled to a CMOS camera. However, further variations in terms of optical elements are intended. Here we present the current status of our work, as well as first experimental results.

  4. High-resolution ab initio three-dimensional x-ray diffraction microscopy

    DOE PAGES

    Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; ...

    2006-01-01

    Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and largest scattering angles recorded. We demonstrate x-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatialmore » resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.« less

  5. High-resolution ab initio Three-dimensional X-ray Diffraction Microscopy

    SciTech Connect

    Chapman, H N; Barty, A; Marchesini, S; Noy, A; Cui, C; Howells, M R; Rosen, R; He, H; Spence, J H; Weierstall, U; Beetz, T; Jacobsen, C; Shapiro, D

    2005-08-19

    Coherent X-ray diffraction microscopy is a method of imaging non-periodic isolated objects at resolutions only limited, in principle, by the largest scattering angles recorded. We demonstrate X-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the 3D diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a non-periodic object. We also construct 2D images of thick objects with infinite depth of focus (without loss of transverse spatial resolution). These methods can be used to image biological and materials science samples at high resolution using X-ray undulator radiation, and establishes the techniques to be used in atomic-resolution ultrafast imaging at X-ray free-electron laser sources.

  6. High-resolution ab initio three-dimensional x-ray diffraction microscopy

    SciTech Connect

    Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; Noy, Aleksandr; Hau-Riege, Stefan P.; Cui, Congwu; Howells, Malcolm R.; Rosen, Rachel; He, Haifeng; Spence, John C. H.; Weierstall, Uwe; Beetz, Tobias; Jacobsen, Chris; Shapiro, David

    2006-01-01

    Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and largest scattering angles recorded. We demonstrate x-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatial resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.

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

    SciTech Connect

    Jones, Michael W. M.; Phillips, Nicholas W.; van Riessen, Grant A.; Abbey, Brian; Vine, David J.; Nashed, Youssef S. G.; Mudie, Stephen T.; Afshar, Nader; Kirkham, Robin; Chen, Bo; Balaur, Eugeniu; de Jonge, Martin D.

    2016-08-11

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

  8. Direct imaging of both ferroelectric and antiferromagnetic domains in multiferroic BiFeO{sub 3} single crystal using x-ray photoemission electron microscopy

    SciTech Connect

    Moubah, R.; Colson, D.; Viret, M.; Elzo, M.; Jaouen, N.; Belkhou, R.

    2012-01-23

    In this work, we propose to study the magnetic and ferroelectric configurations in ferroelectric multidomain BiFeO{sub 3} single crystals. Using x-ray (magnetic) linear dichroism in a photoemission electron microscope (X-PEEM), we are able to directly image both the antiferromagnetic and ferroelectric domains. We find that inside one single ferroelectric domain several antiferromagnetic domains coexist. This is different from what was observed on epitaxial thin films, where the ferroelectric domains perfectly match the antiferromagnetic ones, but also from previous neutron measurements on ferroelectric monodomain single-crystals for which one single antiferromagnetic domain was identified. This underlines the fundamental differences between thin films, bulk samples, and single versus ferroelectric multidomain samples.

  9. Direct imaging of both ferroelectric and antiferromagnetic domains in multiferroic BiFeO3 single crystal using x-ray photoemission electron microscopy

    NASA Astrophysics Data System (ADS)

    Moubah, R.; Elzo, M.; El Moussaoui, S.; Colson, D.; Jaouen, N.; Belkhou, R.; Viret, M.

    2012-01-01

    In this work, we propose to study the magnetic and ferroelectric configurations in ferroelectric multidomain BiFeO3 single crystals. Using x-ray (magnetic) linear dichroism in a photoemission electron microscope (X-PEEM), we are able to directly image both the antiferromagnetic and ferroelectric domains. We find that inside one single ferroelectric domain several antiferromagnetic domains coexist. This is different from what was observed on epitaxial thin films, where the ferroelectric domains perfectly match the antiferromagnetic ones, but also from previous neutron measurements on ferroelectric monodomain single-crystals for which one single antiferromagnetic domain was identified. This underlines the fundamental differences between thin films, bulk samples, and single versus ferroelectric multidomain samples.

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

    PubMed

    Deng, Junjing; Vine, David J; Chen, Si; Jin, Qiaoling; Nashed, Youssef S G; Peterka, Tom; Vogt, Stefan; Jacobsen, Chris

    2017-03-27

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

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

    DOE PAGES

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

    2017-03-27

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

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

    PubMed

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

    2013-04-22

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

  13. Nanostructure characterization by a combined x-ray absorption/scanning force microscopy system.

    PubMed

    Pilet, Nicolas; Raabe, Joerg; Stevenson, Stephanie E; Romer, Sara; Bernard, Laetitia; McNeill, Christopher R; Fink, Rainer H; Hug, Hans J; Quitmann, Christoph

    2012-11-30

    A combined x-ray transmission and scanning force microscope setup (NanoXAS) recently installed at a dedicated beamline of the Swiss Light Source combines complementary experimental techniques to access chemical and physical sample properties with nanometer scale resolution. While scanning force microscopy probes physical properties such as sample topography, local mechanical properties, adhesion, electric and magnetic properties on lateral scales even down to atomic resolution, scanning transmission x-ray microscopy offers direct access to the local chemical composition, electronic structure and magnetization. Here we present three studies which underline the advantages of complementary access to nanoscale properties in prototype thin film samples.

  14. Characterization of toners and inkjets by laser ablation spectrochemical methods and Scanning Electron Microscopy-Energy Dispersive X-ray Spectroscopy

    NASA Astrophysics Data System (ADS)

    Trejos, Tatiana; Corzo, Ruthmara; Subedi, Kiran; Almirall, José

    2014-02-01

    Detection and sourcing of counterfeit currency, examination of counterfeit security documents and determination of authenticity of medical records are examples of common forensic document investigations. In these cases, the physical and chemical composition of the ink entries can provide important information for the assessment of the authenticity of the document or for making inferences about common source. Previous results reported by our group have demonstrated that elemental analysis, using either Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS) or Laser Ablation Induced Breakdown Spectroscopy (LIBS), provides an effective, practical and robust technique for the discrimination of document substrates and writing inks with minimal damage to the document. In this study, laser-based methods and Scanning Electron Microscopy-Energy Dispersive X-Ray Spectroscopy (SEM-EDS) methods were developed, optimized and validated for the forensic analysis of more complex inks such as toners and inkjets, to determine if their elemental composition can differentiate documents printed from different sources and to associate documents that originated from the same printing source. Comparison of the performance of each of these methods is presented, including the analytical figures of merit, discrimination capability and error rates. Different calibration strategies resulting in semi-quantitative and qualitative analysis, comparison methods (match criteria) and data analysis and interpretation tools were also developed. A total of 27 black laser toners originating from different manufacturing sources and/or batches were examined to evaluate the discrimination capability of each method. The results suggest that SEM-EDS offers relatively poor discrimination capability for this set (~ 70.7% discrimination of all the possible comparison pairs or a 29.3% type II error rate). Nonetheless, SEM-EDS can still be used as a complementary method of analysis since it has

  15. Forensic analysis of soil and sediment traces by scanning electron microscopy and energy-dispersive X-ray analysis: an experimental investigation.

    PubMed

    Pye, Kenneth; Croft, Debra

    2007-01-05

    This paper reports the results of a series of experiments carried out to determine the precision of soil trace comparisons based on elemental peak height ratios determined by energy-dispersive X-ray analysis (EDXRA) in a variable pressure scanning electron microscope (VP-SEM). Experiments were conducted on 'bulk' soil aggregates, ground powders prepared from the <150 microm soil fractions and on smears of both the bulk soil and <150 microm material placed on cotton cloth. X-ray count data were obtained using area scans and spot analyses at different magnifications. The effects on elemental peak height ratios of varying the SEM chamber pressure, beam spot size, emission current and accelerating voltage were also examined. The peak height ratios for oxygen, silicon, aluminium, potassium, calcium and iron were found to show little variation as a function of chamber pressure, spot size and emission current over the ranges examined, but a strong dependency on accelerating voltage was observed. Within-sample variation in results, expressed by the percentage coefficient of variation, was found to be lowest for area scan analyses of the ground <150 microm fractions and greatest for the spot analyses of the bulk soil aggregates and the <150 microm fractions. We conclude that comparison of elemental peak height ratios determined by EDXRA can be a useful tool for rapid screening of soil samples, especially when combined with investigation of other attributes of the soil traces such as colour, fabric and the composition, shapes and surface textures of individual particles or aggregates within the soil traces. If sufficient material is available and can be readily separated without contamination or loss, higher resolution and more precise elemental data should be obtained by methods such as inductively coupled plasma atomic-emission spectrometry (ICP-AES) or mass-spectrometry (ICP-MS).

  16. X-ray microscopy and imaging of Escherichia coli, LPS and DNA.

    PubMed

    Rajyaguru, J M; Kado, M; Torres, D; Richardson, M; Muszynski, M J

    1997-11-01

    Ultrastructural examination by transmission and scanning electron microscopy involves a series of specialized preparation steps which may introduce artefacts in the micrographs. X-ray microscopy can take instant images of specimens but is mostly restricted to a few synchrotron X-ray sources. We have utilized a bench-top nanosecond laser-plasma to produce a single-shot source of nanosecond X-rays tuned for maximum contrast with carbon-rich material. To examine the ultrastructure by absorption profiles, we utilized a laser-produced plasma generated by a single-shot laser (1.06 microns wavelength, 5 x 10(12) W cm-2 intensity) focused on to a silicon target as an X-ray source for high-resolution X-ray microscopy. This approach eliminates the specimen preparation steps. Whole hydrated cells of Escherichia coli and purified preparations of lipopolysaccharide (LPS) and chromosomal DNA (cDNA) were streaked onto poly(methyl methacrylate) (PMMA)-coated grids (resist). This resist was exposed to X-rays under vacuum at a distance of 2.5 cm from the target disc. The silicon plasma produced by a 10-ns burst of laser energy (at 20J) radiates strong emission lines in the region of 300 eV. The X-rays penetrate the sample and their absorption profile is transferred on to the resist where PMMA acts as a negative to generate an image. By atomic force microscopy imaging of this photoresist we have visualized layers around cells of E.coli, darker areas inside the cell probably corresponding to cDNA, and preliminary images of LPS and DNA molecules. This technique has resolution at the 100 A level, produces images similar to the space-filling models of macromolecules and may be of great value in the study of the ultrastructure of hydrated live biological specimens.

  17. X-ray microscopy using reflection targets based on SEM with tungsten filament

    NASA Astrophysics Data System (ADS)

    Liu, Junbiao; Ma, Yutian; Zhao, Weixia; Niu, Geng; Chu, Mingzhang; Yin, Bohua; Han, Li; Liu, Baodong

    2016-10-01

    X-ray MicroandNano imaging is developed based on the conventional x-ray tomography, it can not only provide nondestructive testing with higher resolution measurement, but also be used to examine the material or the structure with low atomic number and low density. The source with micro-focal spot size is one of the key components of x-ray MicroandNano imaging. The focused electron beam from SEM bombarding the metal target can generate x-ray with ultra-small size. It is convenient to set up x-ray microscopy based on SEM for laboratory use. This paper describes a new x-ray microscopy using reflection targets based on FEI Quanta600 SEM with tungsten filament. The flat panel detector is placed outside of the vacuum chamber with 300μm thickness Be-window to isolate vacuum from the air. A stage with 3 DOFs is added to adjust the positions of the target, the SEM's sample stage is used to move sample. And the shape of target is designed as cone with 60° half cone angle to get the maximum x-ray dosage. The attenuation coefficient of Bewindow for x-ray is about 25%. Finally, the line pair card is used to evaluate the resolution and the result shows that the resolution of the system can receive less than 750nm, when the acceleration voltage is 30keV, the beam current is 160nA, the SEM working distance is 5mm and the acquisition time of the detector is 60s.

  18. Density gradient free electron collisionally excited x-ray laser

    DOEpatents

    Campbell, E.M.; Rosen, M.D.

    1984-11-29

    An operational x-ray laser is provided that amplifies 3p-3s transition x-ray radiation along an approximately linear path. The x-ray laser is driven by a high power optical laser. The driving line focused optical laser beam illuminates a free-standing thin foil that may be associated with a substrate for improved structural integrity. This illumination produces a generally cylindrically shaped plasma having an essentially uniform electron density and temperature, that exists over a long period of time, and provides the x-ray laser gain medium. The x-ray laser may be driven by more than one optical laser beam. The x-ray laser has been successfully demonstrated to function in a series of experimental tests.

  19. Density gradient free electron collisionally excited X-ray laser

    DOEpatents

    Campbell, Edward M.; Rosen, Mordecai D.

    1989-01-01

    An operational X-ray laser (30) is provided that amplifies 3p-3s transition X-ray radiation along an approximately linear path. The X-ray laser (30) is driven by a high power optical laser. The driving line focused optical laser beam (32) illuminates a free-standing thin foil (34) that may be associated with a substrate (36) for improved structural integrity. This illumination produces a generally cylindrically shaped plasma having an essentially uniform electron density and temperature, that exists over a long period of time, and provides the X-ray laser gain medium. The X-ray laser (30) may be driven by more than one optical laser beam (32, 44). The X-ray laser (30) has been successfully demonstrated to function in a series of experimental tests.

  20. Soft X-ray Microscopy of Green Cements

    SciTech Connect

    Monteiro, P. J. M.; Mancio, M.; Chae, R.; Ha, J.; Kirchheim, A. P.; Fischer, P.; Tyliszczak, T.

    2011-09-09

    The present status of the cement and concrete industry is not sustainable. The production of Portland cement is responsible for 7% of the CO{sub 2} emissions in the world and existing reinforced concrete infrastructure is deteriorating at a fast pace. The change in the existing technology requires new developments in our understanding of the nanostructure of hydration products and the complex deterioration reactions. We have been developing an elaborate research program to advance the existing cement and concrete science by characterizing its nanostructure by synchrotron radiation. A new generation of green cements is being studied using high-resolution soft x-ray microscopy at the nano-level.

  1. X-ray microscopy of soft and hard human tissues

    SciTech Connect

    Müller, Bert Schulz, Georg Deyhle, Hans Stalder, Anja K. Ilgenstein, Bernd Holme, Margaret N. Hieber, Simone E.; Beckmann, Felix

    2016-01-28

    The simultaneous post mortem visualization of soft and hard tissues using absorption-based CT remains a challenge. If the photon energy is optimized for the visualization of hard tissue, the surrounding soft tissue components are almost X-ray transparent. Therefore, the combination with other modalities such as phase-contrast CT, magnetic resonance microscopy, and histology is essential to detect the anatomical features. The combination of the 2D and 3D data sets using sophisticated segmentation and registration tools allows for conclusions about otherwise inaccessible anatomical features essential for improved patient treatments.

  2. X-ray microscopy of soft and hard human tissues

    NASA Astrophysics Data System (ADS)

    Müller, Bert; Schulz, Georg; Deyhle, Hans; Stalder, Anja K.; Ilgenstein, Bernd; Holme, Margaret N.; Weitkamp, Timm; Beckmann, Felix; Hieber, Simone E.

    2016-01-01

    The simultaneous post mortem visualization of soft and hard tissues using absorption-based CT remains a challenge. If the photon energy is optimized for the visualization of hard tissue, the surrounding soft tissue components are almost X-ray transparent. Therefore, the combination with other modalities such as phase-contrast CT, magnetic resonance microscopy, and histology is essential to detect the anatomical features. The combination of the 2D and 3D data sets using sophisticated segmentation and registration tools allows for conclusions about otherwise inaccessible anatomical features essential for improved patient treatments.

  3. Electronic and geometric properties of Au nanoparticles on Highly Ordered Pyrolytic Graphite (HOPG) studied using X-ray Photoelectron Spectroscopy (XPS) and Scanning Tunneling Microscopy (STM).

    PubMed

    Lopez-Salido, Ignacio; Lim, Dong Chan; Dietsche, Rainer; Bertram, Nils; Kim, Young Dok

    2006-01-26

    Au nanoparticles grown on mildly sputtered Highly Ordered Pyrolytic Graphite (HOPG) surfaces were studied using Scanning Tunneling Microscopy (STM) and X-ray Photoelectron Spectroscopy (XPS). The results were compared with those of Ag nanoparticles on the same substrate. By varying the defect densities of HOPG and the Au coverages, one can create Au nanoparticles in various sizes. At high Au coverages, the structures of the Au films significantly deviate from the ideal truncated octahedral form: the existence of many steps between different Au atomic layers can be observed, most likely due to a high activation barrier of the diffusion of Au atoms across the step edges. This implies that the particle growth at room temperature is strongly limited by kinetic factors. Hexagonal shapes of Au structures could be identified, indicating preferential growth of Au nanostructures along the (111) direction normal to the surface. In the case of Au, XPS studies reveal a weaker core level shift with decreasing particle size compared to the 3d level in similarly sized Ag particles. Also taking into account the Auger analysis of the Ag particles, the core level shifts of the metal nanoparticles on HOPG can be understood in terms of the metal/substrate charge transfer. Ag is (partially) positively charged, whereas Au negatively charged on HOPG. It is demonstrated that XPS can be a useful tool to study metal-support interactions, which plays an important role for heterogeneous catalysis, for example.

  4. Electron beam welder X-rays its own welds

    NASA Technical Reports Server (NTRS)

    Roden, W. A.

    1967-01-01

    Beam of an electron beam welder X rays its own welds, enabling rapid weld quality checks to be made without removing the work from the vacuum chamber. A tungsten target produces X rays when hit by the beam. They are directed at the weld specimen and recorded on polaroid film.

  5. X-Ray-Diffraction Tests Of Irradiated Electronic Devices: II

    NASA Technical Reports Server (NTRS)

    Shaw, David C.; Lowry, Lynn E.; Barnes, Charles E.

    1993-01-01

    Report describes research on use of x-ray diffraction to measure stresses in metal conductors of complementary metal oxide/semiconductor (CMOS) integrated circuits exposed to ionizing radiation. Expanding upon report summarized in "X-Ray-Diffraction Tests Of Irradiated Electronic Devices: I" (NPO-18803), presenting data further suggesting relationship between electrical performances of circuits and stresses and strains in metal conductors.

  6. X-Ray-Diffraction Tests Of Irradiated Electronic Devices: II

    NASA Technical Reports Server (NTRS)

    Shaw, David C.; Lowry, Lynn E.; Barnes, Charles E.

    1993-01-01

    Report describes research on use of x-ray diffraction to measure stresses in metal conductors of complementary metal oxide/semiconductor (CMOS) integrated circuits exposed to ionizing radiation. Expanding upon report summarized in "X-Ray-Diffraction Tests Of Irradiated Electronic Devices: I" (NPO-18803), presenting data further suggesting relationship between electrical performances of circuits and stresses and strains in metal conductors.

  7. X-ray tube with magnetic electron steering

    DOEpatents

    Reed, Kim W.; Turman, Bobby N.; Kaye, Ronald J.; Schneider, Larry X.

    2000-01-01

    An X-ray tube uses a magnetic field to steer electrons. The magnetic field urges electrons toward the anode, increasing the proportion of electrons emitted from the cathode that reach desired portions of the anode and consequently contribute to X-ray production. The magnetic field also urges electrons reflected from the anode back to the anode, further increasing the efficiency of the tube.

  8. The extraction of gold nanoparticles from oat and wheat biomasses using sodium citrate and cetyltrimethylammonium bromide, studied by x-ray absorption spectroscopy, high-resolution transmission electron microscopy, and UV-visible spectroscopy.

    PubMed

    Armendariz, Veronica; Parsons, Jason G; Lopez, Martha L; Peralta-Videa, Jose R; Jose-Yacaman, Miguel; Gardea-Torresdey, Jorge L

    2009-03-11

    Gold (Au) nanoparticles can be produced through the interaction of Au(III) ions with oat and wheat biomasses. This paper describes a procedure to recover gold nanoparticles from oat and wheat biomasses using cetyltrimethylammonium bromide or sodium citrate. Extracts were analyzed using UV-visible spectroscopy, high-resolution transmission electron microscopy (HRTEM), and x-ray absorption spectroscopy. The HRTEM data demonstrated that smaller nanoparticles are extracted first, followed by larger nanoparticles. In the fourth extraction, coating of chelating agents is visible on the extracted nanoparticles.

  9. Examination of Libby, Montana, Fill Material for Background Levels of Amphibole from the Rainy Creek Complex Using Scanning Electron Microscopy and X-Ray Microanalysis

    USGS Publications Warehouse

    Adams, David T.; Langer, William H.; Hoefen, Todd M.; Van Gosen, Bradley S.; Meeker, Gregory P.

    2010-01-01

    Natural background levels of Libby-type amphibole in the sediment of the Libby valley in Montana have not, up to this point, been determined. The purpose of this report is to provide the preliminary findings of a study designed by both the U.S. Geological Survey and the U.S. Environmental Protection Agency and performed by the U.S. Geological Survey. The study worked to constrain the natural background levels of fibrous amphiboles potentially derived from the nearby Rainy Creek Complex. The material selected for this study was sampled from three localities, two of which are active open-pit sand and gravel mines. Seventy samples were collected in total and examined using a scanning electron microscope equipped with an energy dispersive x-ray spectrometer. All samples contained varying amounts of feldspars, ilmenite, magnetite, quartz, clay minerals, pyroxene minerals, and non-fibrous amphiboles such as tremolite, actinolite, and magnesiohornblende. Of the 70 samples collected, only three had detectable levels of fibrous amphiboles compatible with those found in the rainy creek complex. The maximum concentration, identified here, of the amphiboles potentially from the Rainy Creek Complex is 0.083 percent by weight.

  10. Imaging at high spatial resolution: Soft x-ray microscopy to 15nm

    SciTech Connect

    Attwood, D.; Chao, W.; Anderson, E.; Liddle, J.A.; Harteneck, B.; Fischer, P.; Schneider, G.; Le Gros, M.; Larabell, C.

    2006-04-05

    Soft x-ray microscopy has now achieved 15 nm spatial resolution with new zone plates and bending magnet radiation. Combined with elemental sensitivity and flexible sample environment (applied magnetic or electric fields, wet samples, windows, overcoatings) this emerges as a valuable tool for nanoscience and nanotechnology, complimenting common electron and scanning tip microscopies. In this presentation we describe recent advances in spatial resolution, expectations for the near future, and applications to magnetic materials, bio-tomography, etc.

  11. Laser Electron Generator of the X-Ray Radiation

    NASA Astrophysics Data System (ADS)

    Artyukov, I. A.; Bessonov, E. G.; Vinogradov, A. V.; Gorbunkov, M. V.; Maslova, Yu. Ya.; Popov, N. L.; Postnov, A. A.; Uspenski, Yu. A.; Feshchenko, R. M.; Shabalin, Yu. V.; Slovokhotov, Yu. L.; Zubavichus, Ya. V.; Ishanov, B. S.; Poseryaev, A. V.; Shvedunov, V. I.; Kostrukov, P. V.; Tunkin, V. G.

    The possibility of the creation and the application prospects of the laser-electron X-ray generator based on the Thompson scattering of the laser radiation on a bunch of relativistic electrons are considered. Such a generator fills the existing gap between X-ray tubes and synchrotron sources, which is several orders of magnitude in terms of the brightness, average intensity, size and also in the construction and exploitation costs. The layout of beam-lines and experimental stations intended for the applications of the X-ray laser-electron generator to the investigation of the elemental composition and material structure and biological objects is discussed.

  12. Low Energy X-Ray and Electron Interactions within Matter.

    DTIC Science & Technology

    1980-03-01

    0-C3962 HAWAII] UNIV HONOLULU DEPT OF PHYSICS AND AST/RONiOMY FmI SelfLOW ENERGY X-RAY AND ELECTRON INTERACTIONS WITHIN MATTER.1U) 14M a L HEM Ai -79...U UNCLASSIFIED AFMWTI olL E iiEEEEEsoE II,,,,hEEIN Eh~hEhh~hhhmmEEmhEEAhE Xbo R-TE. 8oo194 DV , LOW ENERGY X-RAY AND ELECTRON INTERACTIONS WITHIN...ACCESSION NO 3. RECiPIENT’S CATALOG NUMBER TITLE (and SublIII.) 5. TYPE OF REPORT & PERIOD COVERE? LOW ENERGY X-RAY AND ELECTRON INTERACTIONS // Interim A

  13. X-ray microscopy using grazing-incidence reflections optics

    SciTech Connect

    Price, R.H.

    1983-06-30

    The role of Kirkpatrick-Baez microscopes as the workhorse of the x-ray imaging devices is discussed. This role is being extended with the development of a 22X magnification Kirkpatrick-Baez x-ray microscope with multilayer x-ray mirrors. These mirrors can operate at large angles, high x-ray energies, and have a narrow, well defined x-ray energy bandpass. This will make them useful for numerous experiments. However, where a large solid angle is needed, the Woelter microscope will still be necessary and the technology needed to build them will be useful for many other types of x-ray optics.

  14. X-ray microscopy using grazing-incidence reflection optics

    SciTech Connect

    Price, R.H.

    1981-08-06

    The Kirkpatrick-Baez microscopes are described along with their role as the workhorse of the x-ray imaging devices. This role is being extended with the development of a 22X magnification Kirkpatrick-Baez x-ray microscope with multilayer x-ray mirrors. These mirrors can operate at large angles, high x-ray energies, and have a narrow, well defined x-ray energy bandpass. This will make them useful for numerous experiments. However, where a large solid angle is needed, the Woelter microscope will still be necessary and the technology needed to build them will be useful for many other types of x-ray optics.

  15. A New Method for Investigation of the Hair Shaft: Hard X-Ray Microscopy with a 90-nm Spatial Resolution

    PubMed Central

    Jeon, Soo-Young; Goo, Ja Woong; Hong, Seung Phil; Oh, Tak Heon; Youn, Hwa Shik

    2008-01-01

    Various methods have been used to investigate the hair shaft. In the ultrastructural hair field, scanning and transmission electron microscopies are widely used investigative methods, but they have some technical limitations. Recently, X-ray microscopes with sub-micron spatial resolution have emerged as useful instruments because they offer a unique opportunity to observe the interior of an undamaged sample in greater detail. In this report, we examined damaged hair shaft tips using hard X-ray microscopy with a 90 nm spatial resolution. The results of this study suggest that hard X-ray microscopy is an alternative investigative method for hair morphology studies. PMID:18452275

  16. X-ray holographic microscopy by means of photoresist recording and atomic-force microscope readout

    SciTech Connect

    Lindaas, S.; Howells, M.; Jacobsen, C.; Kalinovsky, A.

    1996-09-01

    We have reconstructed in-line (or Gabor) x-ray holograms at 40{endash}50-nm resolution from a complex biological specimen. The holograms were recorded as a relief pattern on photoresist with use of 1.89-nm, soft x rays from the X1A undulator beam line at the National Synchrotron Light Source at Brookhaven National Laboratory. We have improved the resolution and the fidelity and simplified the experiment compared with earlier work by employing a special atomic-force microscope to examine and digitize the holograms. Following digitization the holograms were reconstructed numerically, allowing both the absorptive and phase-shifting properties of the reconstructed object to be mapped. A comparison of the reconstructed images with images obtained from visible light and transmission electron microscopes has been made to confirm the validity of the x-ray holographic technique. The method offers promise as a technique for soft-x-ray microscopy and diffraction tomography of dry and frozen hydrated specimens and for microscopy with pulsed x-ray sources. {copyright} {ital 1996 Optical Society of America.}

  17. Glass Monocapillary X-ray Optics And Their Applications In X-ray Microscopy

    NASA Astrophysics Data System (ADS)

    Zeng, X.; Feser, M.; Huang, E.; Lyon, A.; Yun, W.

    2010-04-01

    Elliptical, parabolic and Wolter type glass monocapillaries were fabricated for use as x-ray condensers in the energy range of 250 eV to 20 keV. On a routine basis a diameter error of +/-0.4 μm and straightness error of 0.8 μm (peak to valley) can be reached. The final test of condensers was performed at-wavelength by imaging the far field x-ray reflection intensity distribution using a laboratory microfocus x-ray source. For medium length condensers with a total length <80 mm, a total slope error of 40 μrad rms was obtained. The applications in full-field x-ray microscopes and the future effort in developing capillary Wolter mirrors based on this technology are reported.

  18. Structure of low-density nanoporous dielectrics revealed by low-vacuum electron microscopy and small-angle x-ray scattering

    SciTech Connect

    Kucheyev, S O; Toth, M; Baumann, T F; Hamza, A V; Ilavsky, J; Knowles, W R; Thiel, B L; Tileli, V; van Buuren, T; Wang, Y M; Willey, T M

    2006-06-05

    We use low-vacuum scanning electron microscopy to image directly the ligament and pore size and shape distributions of representative aerogels over a wide range of length scales ({approx} 10{sup 0}-10{sup 5} nm). The images are used for unambiguous, real-space interpretation of small-angle scattering data for these complex nanoporous systems.

  19. Development of X-ray Microscopy at IPOE

    SciTech Connect

    Zhu, J.; Mu, B.; Huang, Q.; Huang, C.; Yi, S.; Zhang, Z.; Wang, F.; Wang, Z.; Chen, L.

    2011-09-09

    In order to meet the different requirements of applications in synchrotron radiation and plasma diagnosis in China, focusing and imaging optics based on Kirkpatrick-Baez (KB) mirrors, compound refractive lenses (CRLs), and multilayer Laue lenses (MLLs) were studied in our lab. A one-dimensional KB microscope using mirrors with a dual-periodic multilayer coating was developed. The multilayer mirror can reflect both 4.75 keV (Ti K-line) and 8.05 keV (Cu K-line) simultaneously, which makes alignment easier. For hard x-ray microscopy, CRL was studied. Using a SU-8 resist planar parabolic CRL, a focal line of 28.8-{mu}m width was obtained. To focus hard x-rays to nanometer levels efficiently, an MLL was fabricated using a WSi{sub 2}/Si multilayer. The MLL consists of 324 alternating WSi{sub 2} and Si layers with a total thickness of 7.9 {mu}m. (Recently, a much thicker multilayer has been deposited with a layer number of n = 1582 and a total thickness of 27 {mu}m.) After deposition, the sample was sliced and polished into an approximate ideal aspect ratio (depth of the zone plate to outmost layer thickness); the measured results show an intact structure remains, and the surface roughness of the cross section is about 0.4 nm after grinding and polishing processes.

  20. Synchrotron X-ray tomographic microscopy of fossil embryos.

    PubMed

    Donoghue, Philip C J; Bengtson, Stefan; Dong, Xi-ping; Gostling, Neil J; Huldtgren, Therese; Cunningham, John A; Yin, Chongyu; Yue, Zhao; Peng, Fan; Stampanoni, Marco

    2006-08-10

    Fossilized embryos from the late Neoproterozoic and earliest Phanerozoic have caused much excitement because they preserve the earliest stages of embryology of animals that represent the initial diversification of metazoans. However, the potential of this material has not been fully realized because of reliance on traditional, non-destructive methods that allow analysis of exposed surfaces only, and destructive methods that preserve only a single two-dimensional view of the interior of the specimen. Here, we have applied synchrotron-radiation X-ray tomographic microscopy (SRXTM), obtaining complete three-dimensional recordings at submicrometre resolution. The embryos are preserved by early diagenetic impregnation and encrustation with calcium phosphate, and differences in X-ray attenuation provide information about the distribution of these two diagenetic phases. Three-dimensional visualization of blastomere arrangement and diagenetic cement in cleavage embryos resolves outstanding questions about their nature, including the identity of the columnar blastomeres. The anterior and posterior anatomy of embryos of the bilaterian worm-like Markuelia confirms its position as a scalidophoran, providing new insights into body-plan assembly among constituent phyla. The structure of the developing germ band in another bilaterian, Pseudooides, indicates a unique mode of germ-band development. SRXTM provides a method of non-invasive analysis that rivals the resolution achieved even by destructive methods, probing the very limits of fossilization and providing insight into embryology during the emergence of metazoan phyla.

  1. Development of X-ray Microscopy at IPOE

    NASA Astrophysics Data System (ADS)

    Zhu, J.; Mu, B.; Huang, Q.; Huang, C.; Yi, S.; Zhang, Z.; Wang, F.; Wang, Z.; Chen, L.

    2011-09-01

    In order to meet the different requirements of applications in synchrotron radiation and plasma diagnosis in China, focusing and imaging optics based on Kirkpatrick-Baez (KB) mirrors, compound refractive lenses (CRLs), and multilayer Laue lenses (MLLs) were studied in our lab. A one-dimensional KB microscope using mirrors with a dual-periodic multilayer coating was developed. The multilayer mirror can reflect both 4.75 keV (Ti K-line) and 8.05 keV (Cu K-line) simultaneously, which makes alignment easier. For hard x-ray microscopy, CRL was studied. Using a SU-8 resist planar parabolic CRL, a focal line of 28.8-μm width was obtained. To focus hard x-rays to nanometer levels efficiently, an MLL was fabricated using a WSi2/Si multilayer. The MLL consists of 324 alternating WSi2 and Si layers with a total thickness of 7.9 μm. (Recently, a much thicker multilayer has been deposited with a layer number of n = 1582 and a total thickness of 27 μm.) After deposition, the sample was sliced and polished into an approximate ideal aspect ratio (depth of the zone plate to outmost layer thickness); the measured results show an intact structure remains, and the surface roughness of the cross section is about 0.4 nm after grinding and polishing processes.

  2. Femtosecond X-ray magnetic circular dichroism absorption spectroscopy at an X-ray free electron laser

    SciTech Connect

    Higley, Daniel J. Yuan, Edwin; Hirsch, Konstantin; Dakovski, Georgi L.; Jal, Emmanuelle; Lutman, Alberto A.; Coslovich, Giacomo; Hart, Philip; Hoffmann, Matthias C.; Mitra, Ankush; Moeller, Stefan; Ohldag, Hendrik; Seaberg, Matthew; Stöhr, Joachim; Nuhn, Heinz-Dieter; Reid, Alex H.; Dürr, Hermann A.; Schlotter, William F.; Liu, Tianmin; MacArthur, James P.; and others

    2016-03-15

    X-ray magnetic circular dichroism spectroscopy using an X-ray free electron laser is demonstrated with spectra over the Fe L{sub 3,2}-edges. The high brightness of the X-ray free electron laser combined with high accuracy detection of incident and transmitted X-rays enables ultrafast X-ray magnetic circular dichroism studies of unprecedented sensitivity. This new capability is applied to a study of all-optical magnetic switching dynamics of Fe and Gd magnetic sublattices in a GdFeCo thin film above its magnetization compensation temperature.

  3. Atmospheric electron-induced x-ray spectrometer development

    NASA Technical Reports Server (NTRS)

    Wilcox, Jaroslava Z.; Urgiles, Eduardo; Toda, Risaku; Crisp, Joy

    2005-01-01

    This paper extends the work reported at the IEEE Aerospace conference in 2001 and 2003 where the concept and progress in the development of the so called atmospheric Electron X-ray Spectrometer (AEXS) has been described.

  4. Scanning and transmission electron microscopy and X-ray analysisof leaf salt glands of Limoniastrum guyonianum Boiss. under NaCl salinity.

    PubMed

    Zouhaier, Barhoumi; Abdallah, Atia; Najla, Trabelsi; Wahbi, Djebali; Wided, Chaïbi; Aouatef, Ben Ammar; Chedly, Abdelly; Abderazzak, Smaoui

    2015-11-01

    Leaf salt glands of Limoniastrum guyonianum were examined by scanning and transmission electron microscopes and energy dispersive X-ray analysis (EDAX) system, after growing for three months on sandy soil with or without 300 mM NaCl. Results showed that salt glands were irregularly scattered on both leaf sides and sunk under the epidermal level. Salt excretion occurred in both conditions and is mainly composed of calcium and magnesium in control plants, and essentially sodium and chloride in plants subjected to salt treatment. A salt gland is comprised of collecting, accumulating, and central compartments, and is made up of total thirty-two cells. The collecting cells were characterized by large central vacuoles. Accumulating cells contain numerous, large, and unshaped vacuoles and rudimentary chloroplasts. The central compartment was comprised of four basal cells and each one is surmounted by an apical cell. The basal cells are granulated, containing large nucleus, numerous mitochondria, endoplasmic reticulum, ribosomes, polyribosomes, and small vacuoles or vesicles. Equally, the apical cells are rich in organelles. Application of 300 mM NaCl to the culture medium increased vacuoles number and size, and organelles density especially the mitochondria which suggests energy requirement for ions transport. The reduction in size and number of vacuoles toward the interior of salt glands of treated plants and the fusion of the smallest ones with the plasma membrane substantiate the implication of such vacuoles in salt excretion process. The current study which is the first report on L. guyonianum salt gland has provided an in-depth understanding on structure-function relationship in the multicellular salt glands. Copyright © 2015 Elsevier Ltd. All rights reserved.

  5. Scanning Electron Microscopy and Energy-Dispersive X-Ray Microanalysis of Set CEM Cement after Application of Different Bleaching Agents.

    PubMed

    Samiei, Mohammad; Janani, Maryam; Vahdati, Amin; Alemzadeh, Yalda; Bahari, Mahmoud

    2017-01-01

    The present study evaluated the element distribution in completely set calcium-enriched mixture (CEM) cement after application of 35% carbamide peroxide, 40% hydrogen peroxide and sodium perborate as commercial bleaching agents using an energy-dispersive x-ray microanalysis (EDX) system. The surface structure was also observed using the scanning electron microscope (SEM). Twenty completely set CEM cement samples, measuring 4×4 mm(2), were prepared in the present in vitro study and randomly divided into 4 groups based on the preparation technique as follows: the control group; 35% carbamide peroxide group in contact for 30-60 min for 4 times; 40% hydrogen peroxide group with contact time of 15-20 min for 3 times; and sodium perborate group, where the powder and liquid were mixed and placed on CEM cement surface 4 times. Data were analyzed at a significance level of 0.05 through the one Way ANOVA and Tukey's post hoc tests. EDX showed similar element distribution of oxygen, sodium, calcium and carbon in CEM cement with the use of carbamide peroxide and hydroxide peroxide; however, the distribution of silicon was different (P<0.05). In addition, these bleaching agents resulted in significantly higher levels of oxygen and carbon (P<0.05) and a lower level of calcium (P<0.05) compared to the control group. SEM of the control group showed plate-like and globular structure. Sodium perborate was similar to control group due to its weak oxidizing properties. Globular structures and numerous woodpecker holes were observed on the even surface on the carbamide peroxide group. The mean elemental distribution of completely set CEM cement was different when exposed to sodium perborate, carbamide peroxide and hydrogen peroxide.

  6. Time-resolved molecular dynamics of bacteriophage HK97 capsid maturation interpreted by electron cryo-microscopy and X-ray crystallography.

    PubMed

    Wikoff, William R; Conway, James F; Tang, Jinghua; Lee, Kelly K; Gan, Lu; Cheng, Naiqian; Duda, Robert L; Hendrix, Roger W; Steven, Alasdair C; Johnson, John E

    2006-03-01

    The bacteriophage HK97 capsid is a molecular machine that exhibits large-scale conformational rearrangements of its 420 identical protein subunits during capsid maturation. Immature empty capsids, termed Prohead II, assemble in vivo in an Escherichia coli expression system. Maturation of these particles may be induced in vitro, converting them into Head II capsids that are indistinguishable in conformation from the capsid of an infectious phage particle. One method of in vitro maturation requires acidification to drive the reaction through two expansion intermediates (EI-I, EI-II) to its penultimate particle state (EI-III), which has 86% more internal volume than Prohead II. Neutralization of EI-III produces the fully mature capsid, Head II. The three expansion intermediates and the acid expansion pathway were characterized by cryo-EM analysis and 3D reconstruction. We now report that, although large-scale structural changes are involved, the electron density maps for these intermediate states are readily interpreted in terms of quasi-atomic models based on subunit structures determined by prior crystallographic analysis of Head II. Progression through the expansion intermediate states primarily represents rigid-body rotations and translations of the subunits, accompanied by refolding of two small regions, the N-terminal arm and a beta-hairpin called the E-loop. Movies made with these pseudo-atomic coordinates and the Head II X-ray coordinates illuminate various aspects of the maturation pathway in the course of which the pattern of inter-subunit interactions is sequentially transformed while the integrity of the capsid is maintained.

  7. Scanning Electron Microscopy and Energy-Dispersive X-Ray Microanalysis of Set CEM Cement after Application of Different Bleaching Agents

    PubMed Central

    Samiei, Mohammad; Janani, Maryam; Vahdati, Amin; Alemzadeh, Yalda; Bahari, Mahmoud

    2017-01-01

    Introduction: The present study evaluated the element distribution in completely set calcium-enriched mixture (CEM) cement after application of 35% carbamide peroxide, 40% hydrogen peroxide and sodium perborate as commercial bleaching agents using an energy-dispersive x-ray microanalysis (EDX) system. The surface structure was also observed using the scanning electron microscope (SEM). Methods and Materials: Twenty completely set CEM cement samples, measuring 4×4 mm2, were prepared in the present in vitro study and randomly divided into 4 groups based on the preparation technique as follows: the control group; 35% carbamide peroxide group in contact for 30-60 min for 4 times; 40% hydrogen peroxide group with contact time of 15-20 min for 3 times; and sodium perborate group, where the powder and liquid were mixed and placed on CEM cement surface 4 times. Data were analyzed at a significance level of 0.05 through the one Way ANOVA and Tukey’s post hoc tests. Results: EDX showed similar element distribution of oxygen, sodium, calcium and carbon in CEM cement with the use of carbamide peroxide and hydroxide peroxide; however, the distribution of silicon was different (P<0.05). In addition, these bleaching agents resulted in significantly higher levels of oxygen and carbon (P<0.05) and a lower level of calcium (P<0.05) compared to the control group. SEM of the control group showed plate-like and globular structure. Sodium perborate was similar to control group due to its weak oxidizing properties. Globular structures and numerous woodpecker holes were observed on the even surface on the carbamide peroxide group. Conclusion: The mean elemental distribution of completely set CEM cement was different when exposed to sodium perborate, carbamide peroxide and hydrogen peroxide. PMID:28512484

  8. X-Ray Fluorescence Microscopy for Investigation of Archival Tissues

    PubMed Central

    Paunesku, T.; Wanzer, M. B.; Kirillova, E. N.; Muksinova, K. N.; Revina, V. S.; Romanov, S. A.; Lyubchansky, E. R.; Grosche, B.; Birschwilks, M.; Vogt, S.; Finney, L.; Woloschak, G. E.

    2013-01-01

    Several recent efforts in radiation biology community worldwide have amassed records and archival tissues from animals exposed to different radionuclides and external beam irradiation. In most cases, these samples come from life-long studies on large animal populations conducted in national laboratories and equivalent institutions throughout Europe, North America, and Japan. While many of these tissues were used for histopathological analyses, much more information may still be obtained from these samples. A new technique suitable for imaging of these tissues is X-Ray Fluorescence Microscopy (XFM). Following development of third generation synchrotrons, XFM has emerged as an ideal technique for study of metal content, speciation, and localization in cells, tissues and organs. Here we review some of the recent XFM literature pertinent to tissue sample studies and present examples of XFM data obtained from tissue sections of beagle dog samples which show that the quality of archival tissues allows XFM investigation. PMID:22951477

  9. High-resolution compact X-ray microscopy.

    PubMed

    Takman, P A C; Stollberg, H; Johansson, G A; Holmberg, A; Lindblom, M; Hertz, H M

    2007-05-01

    We demonstrate compact full-field soft X-ray transmission microscopy with sub 60-nm resolution operating at lambda= 2.48 nm. The microscope is based on a 100-Hz regenerative liquid-nitrogen-jet laser-plasma source in combination with a condenser zone plate and a micro-zone plate objective for high-resolution imaging onto a 2048 x 2048 pixel CCD detector. The sample holder is mounted in a helium atmosphere and allows imaging of both dry and wet specimens. The microscope design enables fast sample switching and the sample can be pre-aligned using a visible-light microscope. High-quality images can be acquired with exposure times of less than 5 min. We demonstrate the performance of the microscope using both dry and wet samples.

  10. Development of miniaturized electron probe X-ray microanalyzer.

    PubMed

    Imashuku, Susumu; Imanishi, Akira; Kawai, Jun

    2011-11-15

    A miniaturized electron probe X-ray microanalyzer (EPMA) with a small chamber including the electron source and the sample stage was realized using a pyroelectric crystal as an electron source. The EPMA we propose is the smallest reported so far. Performance of the EPMA was evaluated by investigating energy of obtained continuous X-rays and lower detection limits of transition metals (titanium, iron, and nickel). End point energy (Duane-Hunt limit) of continuous X-rays of 45 keV was obtained. However, it is expected that the EPMA can analyze characteristic X-rays with energy less than 20 keV. The EPMA was able to measure titanium, iron, and nickel wires whose projected areas were more than 0.03 mm(2).

  11. High concentration of phosphorus is a distinctive feature of myelin. An X-ray elemental microanalysis study using freeze-fracture scanning electron microscopy of rat sciatic nerve.

    PubMed

    Oliveira, Maria João; Águas, Artur P

    2015-07-01

    We have used rat sciatic nerves submitted to freezing and freeze-fracture to determine the elemental composition of small domains of the peripheral nerve studied at high resolution by scanning electron microscopy. We found that myelin of Schwann cells is unique in its high content in phosphorus (P) that was more than 10 times higher than P measured in any other cells. This high concentration in P makes myelin chemistry suitable of monitoring at the subcellular level using the herein described methodology.

  12. X-ray optics for scanning fluorescence microscopy and other applications

    SciTech Connect

    Ryon, R.W.; Warburton, W.K.

    1992-05-01

    Scanning x-ray fluorescence microscopy is analogous to scanning electron microscopy. Maps of chemical element distribution are produced by scanning with a very small x-ray beam. Goal is to perform such scanning microscopy with resolution in the range of <1 to 10 {mu}m, using standard laboratory x-ray tubes. We are investigating mirror optics in the Kirkpatrick-Baez (K-B) configuration. K-B optics uses two curved mirrors mounted orthogonally along the optical axis. The first mirror provides vertical focus, the second mirror provides horizontal focus. We have used two types of mirrors: synthetic multilayers and crystals. Multilayer mirrors are used with lower energy radiation such as Cu K{alpha}. At higher energies such as Ag K{alpha}, silicon wafers are used in order to increase the incidence angles and thereby the photon collection efficiency. In order to increase the surface area of multilayers which reflects x-rays at the Bragg angle, we have designed mirrors with the spacing between layers graded along the optic axis in order to compensate for the changing angle of incidence. Likewise, to achieve a large reflecting surface with silicon, the wafers are placed on a specially designed lever arm which is bent into a log spiral by applying force at one end. In this way, the same diffracting angle is maintained over the entire surface of the wafer, providing a large solid angle for photon collection.

  13. Calibration of High-Resolution X-Ray Tomography With Atomic Force Microscopy

    PubMed Central

    Kalukin, Andrew R.; Winn, Barry; Wang, Yuxin; Jacobsen, Chris; Levine, Zachary H.; Fu, Joseph

    2000-01-01

    For two-dimensional x-ray imaging of thin films, the technique of scanning transmission x-ray microscopy (STXM) has achieved images with feature sizes as small as 40 nm in recent years. However, calibration of three-dimensional tomographic images that are produced with STXM data at this scale has not yet been described in the scientific literature, and the calibration procedure has novel problems that have not been encountered by x-ray tomography carried out at a larger scale. In x-ray microtomography, for example, one always has the option of using optical imaging on a section of the object to verify the x-ray projection measurements; with STXM, on the other hand, the sample features are too small to be resolved by light at optical wavelengths. This fact implies that one must rely on procedures with higher resolution, such as atomic force microscopy (AFM), for the calibration. Such procedures, however, generally depend on a highly destructive sectioning of the sample, and are difficult to interpret because they give surface information rather than depth information. In this article, a procedure for calibration is described that overcomes these limitations and achieves a calibration of an STXM tomography image with an AFM image and a scanning electron microscopy image of the same object. A Ge star-shaped pattern was imaged at a synchrotron with a scanning transmission x-ray microscope. Nineteen high-resolution projection images of 200 × 200 pixels were tomographically reconstructed into a three-dimensional image. Features in two-dimensional images as small as 40 nm and features as small as 80 nm in the three-dimensional reconstruction were resolved. Transverse length scales based on atomic force microscopy, scanning electron microscopy, x-ray transmission and tomographic reconstruction agreed to within 10 nm. Toward the center of the sample, the pattern thickness calculated from projection images was (51 ± 15) nm vs (80 ± 52) nm for tomographic reconstruction

  14. The X-ray Fluorescence Microscopy Beamline at the Australian Synchrotron

    SciTech Connect

    Paterson, D.; Jonge, M. D. de; Howard, D. L.; Lewis, W.; McKinlay, J.; Starritt, A.; Kusel, M.; Ryan, C. G.; Kirkham, R.; Moorhead, G.; Siddons, D. P.

    2011-09-09

    A hard x-ray micro-nanoprobe has commenced operation at the Australian Synchrotron providing versatile x-ray fluorescence microscopy across an incident energy range from 4 to 25 keV. Two x-ray probes are used to collect {mu}-XRF and {mu}-XANES for elemental and chemical microanalysis: a Kirkpatrick-Baez mirror microprobe for micron resolution studies and a Fresnel zone plate nanoprobe capable of 60-nm resolution. Some unique aspects of the beamline design and operation are discussed. An advanced energy dispersive x-ray fluorescence detection scheme named Maia has been developed for the beamline, which enables ultrafast x-ray fluorescence microscopy.

  15. Fluctuation x-ray microscopy for measuring medium-range order.

    SciTech Connect

    Fan, L.; McNulty, I.; Paterson, D.; Treacy, M. M. J.; Gibson, J. M.; Arizona State Univ.

    2005-01-01

    Many x-ray techniques exist to probe long- and short-range order in matter, in real space by imaging and in reciprocal space by diffraction and scattering. However, measuring medium-range order (MRO) in disordered materials is a long-standing problem. Based on fluctuation electron microscopy, which was applied successfully to the understanding of MRO in amorphous materials, we have developed fluctuation x-ray microscopy (FXM). This novel approach offers quantitative insight into medium-range correlations in materials at nanometer and larger length scales. It examines spatially resolved fluctuations in the intensity of a series of x-ray speckle patterns. The speckle variance depends on higher order correlations that are more sensitive to MRO. Systematically measuring the speckle variance as function of the momentum transfer and x-ray illumination size produces a fluctuation map that contains information about the degree of MRO and the correlation length. This approach can be used for the exploration of MRO and subtle spatial structural changes in a wide range of disordered materials from soft condensed matter to nanowire arrays, semiconductor quantum dot arrays and magnetic materials. It will also help us to understand the mechanisms of order-disorder transitions and may lead to control of ordering, which is important in developing ordered structures tailored for particular applications. A theory for FXM and preliminary experimental results from polystyrene latex spheres are discussed in this paper.

  16. Pinch plasma source for x-ray microscopy with nanosecond exposure time.

    PubMed

    Lebert, R; Neff, W; Rothweiler, D

    1996-01-01

    The strong demand for bright, compact, and inexpensive sources for x-ray microscopy has stimulated the development of flash x-ray sources. In this paper, the requirements for such a source are analyzed under boundary conditions given by the concept of an imaging x-ray microscope using mirror condenser and Fresnel zone plates for high-resolution imaging. It is found that the Lyman-α (1s-2p) line of hydrogen-like nitrogen (N VII) at λ = 2.48 nm emitted from a nonequilibrium plasma of about 200 eV temperature and 1020 cm-3 electron density is best suited. These conditions are achieved in medium-current pinch-plasma devices. Using detailed numerical simulation of the physical processes of such a device, optimization criteria for the integrated spectral brightness (ISB) are found. Measurements of the ISB confirm these optimization criteria. The results show that the spectral emission characteristics of an optimized pinch plasma souce are compatible with the demands of the mentioned x-ray microscopy concept. These emission characteristics are compared with laser-produced plasma sources. Using the optimized source with an ISB exceeding 0.6 μJ/(μm2 sr) in a 10-20 ns pulse, wet biological samples are imaged with about 0.1 μm lateral resolution.

  17. Feasibility of coherent X-ray production by X-ray pumping. [inverting electron population in lithium

    NASA Technical Reports Server (NTRS)

    Csonka, P. L.; Crasemann, B.

    1974-01-01

    It is suggested that coherent X-rays can be produced by inverting the electron population in a suitable target, such as Li, through irradiation with X-rays generated by fast electrons traversing an electromagnetic field (as in a storage ring). Conditions to be satisfied by target and radiation parameters are stated, and examples given.

  18. Application of x-ray nano-particulate markers for the visualization of intermediate layers and interfaces using scanning electron microscopy

    NASA Astrophysics Data System (ADS)

    Bessudnova, Nadezda O.; Bilenko, David I.; Zakharevich, Andrey M.

    2012-03-01

    In this study the methodology of biological sample preparation for dental research using SEM/EDX has been elaborated. (1)The original cutting equipment supplied with 3D user-controlled sample fixation and an adjustable cooling system has been designed and evaluated. (2) A new approach to the root dentine drying procedure has been developed to preserve structure peculiarities of root dentine. (3) A novel adhesive system with embedded X-Ray nanoparticulate markers has been designed. (4)The technique allowing for visualization of bonding resins, interfaces and intermediate layers between tooth hard tissues and restorative materials of endodontically treated teeth using the X-ray nano-particulate markers has been developed and approved. These methods and approaches were used to compare the objective depth of penetration of adhesive systems of different generations in root dentine. It has been shown that the depth of penetration in dentine is less for adhesive systems of generation VI in comparison with bonding resins of generation V, which is in agreement with theoretical evidence. The depth of penetration depends on the correlation between the direction of dentinal tubules, bonding resin delivery and gravity.

  19. Application of x-ray nano-particulate markers for the visualization of intermediate layers and interfaces using scanning electron microscopy

    NASA Astrophysics Data System (ADS)

    Bessudnova, Nadezda O.; Bilenko, David I.; Zakharevich, Andrey M.

    2011-10-01

    In this study the methodology of biological sample preparation for dental research using SEM/EDX has been elaborated. (1)The original cutting equipment supplied with 3D user-controlled sample fixation and an adjustable cooling system has been designed and evaluated. (2) A new approach to the root dentine drying procedure has been developed to preserve structure peculiarities of root dentine. (3) A novel adhesive system with embedded X-Ray nanoparticulate markers has been designed. (4)The technique allowing for visualization of bonding resins, interfaces and intermediate layers between tooth hard tissues and restorative materials of endodontically treated teeth using the X-ray nano-particulate markers has been developed and approved. These methods and approaches were used to compare the objective depth of penetration of adhesive systems of different generations in root dentine. It has been shown that the depth of penetration in dentine is less for adhesive systems of generation VI in comparison with bonding resins of generation V, which is in agreement with theoretical evidence. The depth of penetration depends on the correlation between the direction of dentinal tubules, bonding resin delivery and gravity.

  20. Quantitative Imaging of Single Unstained Magnetotactic Bacteria by Coherent X-ray Diffraction Microscopy.

    PubMed

    Fan, Jiadong; Sun, Zhibin; Zhang, Jian; Huang, Qingjie; Yao, Shengkun; Zong, Yunbing; Kohmura, Yoshiki; Ishikawa, Tetsuya; Liu, Hong; Jiang, Huaidong

    2015-06-16

    Novel coherent diffraction microscopy provides a powerful lensless imaging method to obtain a better understanding of the microorganism at the nanoscale. Here we demonstrated quantitative imaging of intact unstained magnetotactic bacteria using coherent X-ray diffraction microscopy combined with an iterative phase retrieval algorithm. Although the signal-to-noise ratio of the X-ray diffraction pattern from single magnetotactic bacterium is weak due to low-scattering ability of biomaterials, an 18.6 nm half-period resolution of reconstructed image was achieved by using a hybrid input-output phase retrieval algorithm. On the basis of the quantitative reconstructed images, the morphology and some intracellular structures, such as nucleoid, polyβ-hydroxybutyrate granules, and magnetosomes, were identified, which were also confirmed by scanning electron microscopy and energy dispersive spectroscopy. With the benefit from the quantifiability of coherent diffraction imaging, for the first time to our knowledge, an average density of magnetotactic bacteria was calculated to be ∼1.19 g/cm(3). This technique has a wide range of applications, especially in quantitative imaging of low-scattering biomaterials and multicomponent materials at nanoscale resolution. Combined with the cryogenic technique or X-ray free electron lasers, the method could image cells in a hydrated condition, which helps to maintain their natural structure.

  1. Exotic X-ray Sources from Intermediate Energy Electron Beams

    SciTech Connect

    Chouffani, K.; Wells, D.; Harmon, F.; Jones, J.L.; Lancaster, G.

    2003-08-26

    High intensity x-ray beams are used in a wide variety of applications in solid-state physics, medicine, biology and material sciences. Synchrotron radiation (SR) is currently the primary, high-quality x-ray source that satisfies both brilliance and tunability. The high cost, large size and low x-ray energies of SR facilities, however, are serious limitations. Alternatively, 'novel' x-ray sources are now possible due to new small linear accelerator (LINAC) technology, such as improved beam emittance, low background, sub-Picosecond beam pulses, high beam stability and higher repetition rate. These sources all stem from processes that produce Radiation from relativistic Electron beams in (crystalline) Periodic Structures (REPS), or the periodic 'structure' of laser light. REPS x-ray sources are serious candidates for bright, compact, portable, monochromatic, and tunable x-ray sources with varying degrees of polarization and coherence. Despite the discovery and early research into these sources over the past 25 years, these sources are still in their infancy. Experimental and theoretical research are still urgently needed to answer fundamental questions about the practical and ultimate limits of their brightness, mono-chromaticity etc. We present experimental results and theoretical comparisons for three exotic REPS sources. These are Laser-Compton Scattering (LCS), Channeling Radiation (CR) and Parametric X-Radiation (PXR)

  2. Scanning electron microscopy (SEM) and X-ray dispersive spectrometry evaluation of direct laser metal sintering surface and human bone interface: a case series.

    PubMed

    Mangano, Carlo; Piattelli, Adriano; Raspanti, Mario; Mangano, Francesco; Cassoni, Alessandra; Iezzi, Giovanna; Shibli, Jamil Awad

    2011-01-01

    Recent studies have shown that direct laser metal sintering (DLMS) produces structures with complex geometry and consequently that allow better osteoconductive properties. The aim of this patient report was to evaluate the early bone response to DLMS implant surface retrieved from human jaws. Four experimental DLMS implants were inserted in the posterior mandible of four patients during conventional dental implant surgery. After 8 weeks, the micro-implants and the surrounding tissue were removed and prepared for scanning electron microscopy (SEM) and histomorphometric analysis to evaluate the bone-implant interface. The SEM and EDX evaluations showed a newly formed tissue composed of calcium and phosphorus. The bone-to-implant contact presented a mean of 60.5 ± 11.6%. Within the limits of this patient report, data suggest that the DLMS surfaces presented a close contact with the human bone after a healing period of 8 weeks.

  3. An x-ray photoemission electron microscopy study of the formation of Ti-Al phases in 4 mol% TiCl3 catalyzed NaAlH4 during high energy ball milling

    NASA Astrophysics Data System (ADS)

    Dobbins, Tabbetha; Abrecht, Mike; Uprety, Youaraj; Moore, Kristan

    2009-05-01

    This study reports reaction pathways to form TiAlx metallic complexes during the high energy ball milling of 4 mol% TiCl3 with NaAlH4 powders determined using local structure analysis of Tix+ and Alx+ species. Using x-ray photoemission electron microscopy (XPEEM) and x-ray diffraction (XRD), the oxidation state of Alx+ and Tix+ and the crystalline compounds existing in equilibrium with NaAlH4 were tracked for samples milled for times of 0 (i.e. mixing), 5, and 25 min. XPEEM analysis of the Al K edge after 5 min of milling reveals that Al remains in the 3+ oxidation state (i.e. in NaAlH4) around Ti0-rich regions of the sample. After 25 min of high energy milling, Ti0 has reacted with Al3+ (in nearby NaAlH4) to form TiAlx complexes. This study reports the pathway for TiAlx complex formation during milling of 4 mol% TiCl3 catalyzed NaAlH4 to be as follows: (1) Ti3+ reduces to Ti0 (with Al3+ near Ti0 regions) and (2) Ti0 reacts with Al3+ in NaAlH4 to form TiAlx complexes.

  4. Microbial biofilm study by synchrotron X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Pennafirme, S.; Lima, I.; Bitencourt, J. A.; Crapez, M. A. C.; Lopes, R. T.

    2015-11-01

    Microbial biofilm has already being used to remove metals and other pollutants from wastewater. In this sense, our proposal was to isolate and cultivate bacteria consortia from mangrove's sediment resistant to Zn (II) and Cu (II) at 50 mg L-1 and to observe, through synchrotron X-ray fluorescence microscopy (microXRF), whether the biofilm sequestered the metal. The biofilm area analyzed was 1 mm2 and a 2D map was generated (pixel size 20×20 μm2, counting time 5 s/point). The biofilm formation and retention followed the sequence Zn>Cu. Bacterial consortium zinc resistant formed dense biofilm and retained 63.83% of zinc, while the bacterial consortium copper resistant retained 3.21% of copper, with lower biofilm formation. Dehydrogenase activity of Zn resistant bacterial consortium was not negatively affect by 50 mg ml-1 zinc input, whereas copper resistant bacterial consortium showed a significant decrease on dehydrogenase activity (50 mg mL-1 of Cu input). In conclusion, biofilm may protect bacterial cells, acting as barrier against metal toxicity. The bacterial consortia Zn resistant, composed by Nitratireductor spp. and Pseudomonas spp formed dense biofilm and sequestered metal from water, decreasing the metal bioavailability. These bacterial consortia can be used in bioreactors and in bioremediation programs.

  5. Low dose hard x-ray contact microscopy assisted by a photoelectric conversion layer

    SciTech Connect

    Gomella, Andrew; Martin, Eric W.; Lynch, Susanna K.; Wen, Han; Morgan, Nicole Y.

    2013-04-15

    Hard x-ray contact microscopy provides images of dense samples at resolutions of tens of nanometers. However, the required beam intensity can only be delivered by synchrotron sources. We report on the use of a gold photoelectric conversion layer to lower the exposure dose by a factor of 40 to 50, allowing hard x-ray contact microscopy to be performed with a compact x-ray tube. We demonstrate the method in imaging the transmission pattern of a type of hard x-ray grating that cannot be fitted into conventional x-ray microscopes due to its size and shape. Generally the method is easy to implement and can record images of samples in the hard x-ray region over a large area in a single exposure, without some of the geometric constraints associated with x-ray microscopes based on zone-plate or other magnifying optics.

  6. Low dose hard x-ray contact microscopy assisted by a photoelectric conversion layer

    PubMed Central

    Gomella, Andrew; Martin, Eric W.; Lynch, Susanna K.; Morgan, Nicole Y.; Wen, Han

    2013-01-01

    Hard x-ray contact microscopy provides images of dense samples at resolutions of tens of nanometers. However, the required beam intensity can only be delivered by synchrotron sources. We report on the use of a gold photoelectric conversion layer to lower the exposure dose by a factor of 40 to 50, allowing hard x-ray contact microscopy to be performed with a compact x-ray tube. We demonstrate the method in imaging the transmission pattern of a type of hard x-ray grating that cannot be fitted into conventional x-ray microscopes due to its size and shape. Generally the method is easy to implement and can record images of samples in the hard x-ray region over a large area in a single exposure, without some of the geometric constraints associated with x-ray microscopes based on zone-plate or other magnifying optics. PMID:23837131

  7. The identification of the pigments used to paint statues of Feixiange Cliff in China in late 19th century by micro-Raman spectroscopy and scanning electron microscopy/energy dispersive X-ray analysis

    NASA Astrophysics Data System (ADS)

    Jin, Pu-jun; Huang, Wei; Jianhua-Wang; Zhao, Gang; Wang, Xiao-ling

    2010-11-01

    The application of micro-Raman spectroscopy (μ-RS) and scanning electron microscopy (SEM)/energy dispersive X-ray spectrometer (EDS) to the research of pigments collected from Statues of Feixiange Cliff No. 67 and No. 69 niche of Tang Dynasty in China is reported. Five kinds of pigments were found in the experimental data, including black (carbon), white (gypsum + quartz), blue (lapis lazuli) and green (Paris green + Barium sulphate). After synthesized in 1814, Paris green was reported for a large import as a light and bright green pigment to paint architectures in China from the late 19th century. The analyzed blue pigment demonstrated the similar Raman spectra to the Lâjvardina blue glazed ceramics, which indicated lapis lazuli was an artificial product. This confirmed the painting of Feixiange Cliff in the early Republic of China as the historical record, and also reveals that some pigments were imported from abroad.

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

    PubMed

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

    2005-09-01

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

  9. Application of scanning electron microscopy to x-ray analysis of frozen- hydrated sections. III. Elemental content of cells in the rat renal papillary tip

    PubMed Central

    1981-01-01

    The electrolyte and water content of cellular and interstitial compartments in the renal papilla of the rat was determined by x-ray microanalysis of frozen-hydrated tissue sections. Papillae from rats on ad libitum water were rapidly frozen in a slush of Freon 12, and sectioned in a cryomicrotome at -30 to -40 degrees C. Frozen 0.5- micrometer sections were mounted on carbon-coated nylon film over a Be grid, transferred cold to the scanning microscope, and maintained at - 175 degrees C during analysis. The scanning transmission mode was used for imaging. Structural preservation was of good quality and allowed identification of tissue compartments. Tissue mass (solutes + water) was determined by continuum radiation from regions of interest. After drying in the SEM, elemental composition of morphologically defined compartments (solutes) was determined by analysis of specific x-rays, and total dry mass by continuum. Na, K, Cl, and H2O contents in collecting-duct cells (CDC), papillary epithelial cells (PEC), and interstitial cells (IC) and space were measured. Cells had lower water content (mean 58.7%) than interstitium (77.5%). Intracellular K concentrations (millimoles per kilogram wet weight) were unremarkable (79-156 mm/kg wet weight); P was markedly higher in cells than in interstitium. S was the same in all compartments. Intracellular Na levels were extremely high (CDC, 344 +/- 127 SD mm/kg wet weight; PEC, 287 +/- 105; IC, 898 +/- 194). Mean interstitial Na was 590 +/- 119 mm/kg wet weight. CI values paralleled those for Na. If this Na is unbound, then these data suggest that renal papillary interstitial cells adapt to their hyperosmotic environment by a Na-uptake process. PMID:7204493

  10. Determination of elemental distribution in green micro-algae using synchrotron radiation nano X-ray fluorescence (SR-nXRF) and electron microscopy techniques--subcellular localization and quantitative imaging of silver and cobalt uptake by Coccomyxa actinabiotis.

    PubMed

    Leonardo, T; Farhi, E; Boisson, A-M; Vial, J; Cloetens, P; Bohic, S; Rivasseau, C

    2014-02-01

    The newly discovered unicellular micro-alga Coccomyxa actinabiotis proves to be highly radio-tolerant and strongly concentrates radionuclides, as well as large amounts of toxic metals. This study helps in the understanding of the mechanisms involved in the accumulation and detoxification of silver and cobalt. Elemental distribution inside Coccomyxa actinabiotis cells was determined using synchrotron nano X-ray fluorescence spectroscopy at the ID22 nano fluorescence imaging beamline of the European Synchrotron Radiation Facility. The high resolution and high sensitivity of this technique enabled the assessment of elemental associations and exclusions in subcellular micro-algae compartments. A quantitative treatment of the scans was implemented to yield absolute concentrations of each endogenous and exogenous element with a spatial resolution of 100 nm and compared to the macroscopic content in cobalt and silver determined using inductively coupled plasma-mass spectrometry. The nano X-ray fluorescence imaging was complemented by transmission electron microscopy coupled to X-ray microanalysis (TEM-EDS), yielding differential silver distribution in the cell wall, cytosol, nucleus, chloroplast and mitochondria with unique resolution. The analysis of endogenous elements in control cells revealed that iron had a unique distribution; zinc, potassium, manganese, molybdenum, and phosphate had their maxima co-localized in the same area; and sulfur, copper and chlorine were almost homogeneously distributed among the whole cell. The subcellular distribution and quantification of cobalt and silver in micro-alga, assessed after controlled exposure to various concentrations, revealed that exogenous metals were mainly sequestered inside the cell rather than on mucilage or the cell wall, with preferential compartmentalization. Cobalt was homogeneously distributed outside of the chloroplast. Silver was localized in the cytosol at low concentration and in the whole cell excluding the

  11. Streaked x-ray microscopy of laser-fusion targets

    SciTech Connect

    Price, R.H.; Campbell, E.M.; Rosen, M.D.; Auerbach, J.M.; Phillion, D.W.; Whitlock, R.R.; Obenshain, S.P.; McLean, E.A.; Ripin, B.H.

    1982-08-01

    An ultrafast soft x-ray streak camera has been coupled to a Wolter axisymmetric x-ray microscope. This system was used to observe the dynamics of laser fusion targets both in self emission and backlit by laser produced x-ray sources. Spatial resolution was 7 ..mu..m and temporal resolution was 20 ps. Data is presented showing the ablative acceleration of foils to velocities near 10/sup 7/ cm/sec and the collision of an accelerated foil with a second foil, observed using 3 keV streaked x-ray backlighting. Good agreement was found between hydrocode simulations, simple models of the ablative acceleration and the observed velocities of the carbon foils.

  12. Simultaneous cryo X-ray ptychographic and fluorescence microscopy of green algae.

    PubMed

    Deng, Junjing; Vine, David J; Chen, Si; Nashed, Youssef S G; Jin, Qiaoling; Phillips, Nicholas W; Peterka, Tom; Ross, Rob; Vogt, Stefan; Jacobsen, Chris J

    2015-02-24

    Trace metals play important roles in normal and in disease-causing biological functions. X-ray fluorescence microscopy reveals trace elements with no dependence on binding affinities (unlike with visible light fluorophores) and with improved sensitivity relative to electron probes. However, X-ray fluorescence is not very sensitive for showing the light elements that comprise the majority of cellular material. Here we show that X-ray ptychography can be combined with fluorescence to image both cellular structure and trace element distribution in frozen-hydrated cells at cryogenic temperatures, with high structural and chemical fidelity. Ptychographic reconstruction algorithms deliver phase and absorption contrast images at a resolution beyond that of the illuminating lens or beam size. Using 5.2-keV X-rays, we have obtained sub-30-nm resolution structural images and ∼90-nm-resolution fluorescence images of several elements in frozen-hydrated green algae. This combined approach offers a way to study the role of trace elements in their structural context.

  13. Simultaneous cryo X-ray ptychographic and fluorescence microscopy of green algae

    PubMed Central

    Deng, Junjing; Vine, David J.; Chen, Si; Nashed, Youssef S. G.; Jin, Qiaoling; Phillips, Nicholas W.; Peterka, Tom; Ross, Rob; Vogt, Stefan; Jacobsen, Chris J.

    2015-01-01

    Trace metals play important roles in normal and in disease-causing biological functions. X-ray fluorescence microscopy reveals trace elements with no dependence on binding affinities (unlike with visible light fluorophores) and with improved sensitivity relative to electron probes. However, X-ray fluorescence is not very sensitive for showing the light elements that comprise the majority of cellular material. Here we show that X-ray ptychography can be combined with fluorescence to image both cellular structure and trace element distribution in frozen-hydrated cells at cryogenic temperatures, with high structural and chemical fidelity. Ptychographic reconstruction algorithms deliver phase and absorption contrast images at a resolution beyond that of the illuminating lens or beam size. Using 5.2-keV X-rays, we have obtained sub–30-nm resolution structural images and ∼90-nm–resolution fluorescence images of several elements in frozen-hydrated green algae. This combined approach offers a way to study the role of trace elements in their structural context. PMID:25675478

  14. Simultaneous cryo X-ray ptychographic and fluorescence microscopy of green algae

    DOE PAGES

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

    2015-02-24

    Trace metals play important roles in normal and in disease-causing biological functions. X-ray fluorescence microscopy reveals trace elements with no dependence on binding affinities (unlike with visible light fluorophores) and with improved sensitivity relative to electron probes. However, X-ray fluorescence is not very sensitive for showing the light elements that comprise the majority of cellular material. Here we show that X-ray ptychography can be combined with fluorescence to image both cellular structure and trace element distribution in frozen-hydrated cells at cryogenic temperatures, with high structural and chemical fidelity. Ptychographic reconstruction algorithms deliver phase and absorption contrast images at a resolutionmore » beyond that of the illuminating lens or beam size. Using 5.2-keV X-rays, we have obtained sub-30-nm resolution structural images and ~90-nm-resolution fluorescence images of several elements in frozen-hydrated green algae. Finally, this combined approach offers a way to study the role of trace elements in their structural context.« less

  15. Study of Interactions Between Microbes and Minerals by Scanning Transmission X-Ray Microscopy (STXM)

    NASA Astrophysics Data System (ADS)

    Benzerara, K.; Tyliszczak, T.; Brown, G. E.

    2007-02-01

    Scanning Transmission X-ray Microscopy (STXM) and Transmission Electron Microscopy (TEM) were combined to characterize various samples of geomicrobiological interest down to the nanometer scale. An approach based on energy-filtered imaging was used to examine microbe-mineral interactions and the resulting biominerals, as well as biosignatures in simplified laboratory samples. This approach was then applied to natural samples, including natural biofilms entombed in calcium carbonate precipitates and bioweathered silicates and facilitated location of bacterial cells and provided unique insights about their biogeochemical interactions with minerals at the 30-40 nm scale.

  16. Characterisation of internal morphologies in electrospun fibers by X-ray tomographic microscopy

    NASA Astrophysics Data System (ADS)

    Nygaard, Jens Vinge; Uyar, Tamer; Chen, Menglin; Cloetens, Peter; Kingshott, Peter; Besenbacher, Flemming

    2011-09-01

    Electrospun fabrics for use in, for example, tissue engineering, wound dressings, textiles, filters and membranes have attracted a lot of attention due to their morphological nanoscale architectures which enhance their physical properties. A thorough detailed internal morphological study has been performed on electrospun polystyrene (PS) fibers produced from dimethylformamide (DMF) solutions. Investigations by transmission electron microscopy (TEM) and thorough studies for the first time by synchrotron based X-ray tomographic microscopy (XTM) revealed that the individual electrospun PS fibers and beads have a graded density and in some cases even an internal porous structure.

  17. Study of Interactions Between Microbes and Minerals by Scanning Transmission X-Ray Microscopy (STXM)

    SciTech Connect

    Benzerara, K.; Tyliszczak, T.; Brown, G.E., Jr.; /Stanford U., Geo. Environ. Sci. /SLAC, SSRL

    2007-01-03

    Scanning Transmission X-ray Microscopy (STXM) and Transmission Electron Microscopy (TEM) were combined to characterize various samples of geomicrobiological interest down to the nanometer scale. An approach based on energy-filtered imaging was used to examine microbe-mineral interactions and the resulting biominerals, as well as biosignatures in simplified laboratory samples. This approach was then applied to natural samples, including natural biofilms entombed in calcium carbonate precipitates and bioweathered silicates and facilitated location of bacterial cells and provided unique insights about their biogeochemical interactions with minerals at the 30-40 nm scale.

  18. Probing Transient Electron Dynamics Using Ultrafast X Rays

    NASA Astrophysics Data System (ADS)

    Bucksbaum, Philip

    2016-05-01

    Linear x-ray absorption in atoms or molecules creates highly excited multi-electron quantum systems, which relax rapidly by fluorescence or Auger emission. These relaxation rates are usually less than a few femtoseconds in duration, and so they can reveal transient elecronic states in molecules as they undergo photo-induced transformations. I will show recent results from femtosecond x-ray experiments that display this phenomenon. There are efforts underway to push the temporal resolving power of ultrafast x-ray pulses into the attosecond regime, using stronger fields to initiate nonlinear absorption processes such as transient stimulated electronic Raman scattering. I will discuss current progress and future prospects for research in this area. This research is supported through Stanford PULSE Institute, SLAC National Accelerator Lab by the U.S. Department of Energy, Office of Basic Energy Sciences, Atomic, Molecular, and Optical Science Program.

  19. X-ray mapping in electron-beam instruments.

    PubMed

    Friel, John J; Lyman, Charles E

    2006-02-01

    This review traces the development of X-ray mapping from its beginning 50 years ago through current analysis procedures that can reveal otherwise obscure elemental distributions and associations. X-ray mapping or compositional imaging of elemental distributions is one of the major capabilities of electron beam microanalysis because it frees the operator from the necessity of making decisions about which image features contain elements of interest. Elements in unexpected locations, or in unexpected association with other elements, may be found easily without operator bias as to where to locate the electron probe for data collection. X-ray mapping in the SEM or EPMA may be applied to bulk specimens at a spatial resolution of about 1 microm. X-ray mapping of thin specimens in the TEM or STEM may be accomplished at a spatial resolution ranging from 2 to 100 nm, depending on specimen thickness and the microscope. Although mapping has traditionally been considered a qualitative technique, recent developments demonstrate the quantitative capabilities of X-ray mapping techniques. Moreover, the long-desired ability to collect and store an entire spectrum at every pixel is now a reality, and methods for mining these data are rapidly being developed.

  20. Optical Shaping of X-Ray Free-Electron Lasers

    NASA Astrophysics Data System (ADS)

    Marinelli, A.; Coffee, R.; Vetter, S.; Hering, P.; West, G. N.; Gilevich, S.; Lutman, A. A.; Li, S.; Maxwell, T.; Galayda, J.; Fry, A.; Huang, Z.

    2016-06-01

    In this Letter we report the experimental demonstration of a new temporal shaping technique for x-ray free-electron lasers (FELs). This technique is based on the use of a spectrally shaped infrared (IR) laser and allows optical control of the x-ray generation process. By accurately manipulating the spectral amplitude and phase of the IR laser, we can selectively modify the electron bunch longitudinal emittance thus controlling the duration of the resulting x-ray pulse down to the femtosecond time scale. Unlike other methods currently in use, optical shaping is directly applicable to the next generation of high-average power x-ray FELs such as the Linac Coherent Light Source-II or the European X-FEL, and it enables pulse shaping of FELs at the highest repetition rates. Furthermore, this laser-shaping technique paves the way for flexible tailoring of complex multicolor FEL pulse patterns required for nonlinear multidimensional x-ray spectroscopy as well as novel multicolor diffraction imaging schemes.

  1. The History of X-ray Free-Electron Lasers

    SciTech Connect

    Pellegrini, C.; /UCLA /SLAC

    2012-06-28

    The successful lasing at the SLAC National Accelerator Laboratory of the Linear Coherent Light Source (LCLS), the first X-ray free-electron laser (X-ray FEL), in the wavelength range 1.5 to 15 {angstrom}, pulse duration of 60 to few femtoseconds, number of coherent photons per pulse from 10{sup 13} to 10{sup 11}, is a landmark event in the development of coherent electromagnetic radiation sources. Until now electrons traversing an undulator magnet in a synchrotron radiation storage ring provided the best X-ray sources. The LCLS has set a new standard, with a peak X-ray brightness higher by ten orders of magnitudes and pulse duration shorter by three orders of magnitudes. LCLS opens a new window in the exploration of matter at the atomic and molecular scales of length and time. Taking a motion picture of chemical processes in a few femtoseconds or less, unraveling the structure and dynamics of complex molecular systems, like proteins, are some of the exciting experiments made possible by LCLS and the other X-ray FELs now being built in Europe and Asia. In this paper, we describe the history of the many theoretical, experimental and technological discoveries and innovations, starting from the 1960s and 1970s, leading to the development of LCLS.

  2. Correlative VIS-fluorescence and soft X-ray cryo-microscopy/tomography of adherent cells

    PubMed Central

    Hagen, Christoph; Guttmann, Peter; Klupp, Barbara; Werner, Stephan; Rehbein, Stefan; Mettenleiter, Thomas C.; Schneider, Gerd; Grünewald, Kay

    2012-01-01

    Soft X-ray cryo-microscopy/tomography of vitreous samples is becoming a valuable tool in structural cell biology. Within the ‘water-window’ wavelength region (2.34–4.37 nm), it provides absorption contrast images with high signal to noise ratio and resolution of a few tens of nanometer. Soft X-rays with wavelengths close to the K-absorption edge of oxygen penetrate biological samples with thicknesses in the micrometer range. Here, we report on the application of a recently established extension of the transmission soft X-ray cryo-microscope (HZB TXM) at the beamline U41-XM of the BESSY II electron storage ring by an in-column epi-fluorescence and reflected light cryo-microscope. We demonstrate the new capability for correlative fluorescence and soft X-ray cryo-microscopy/tomography of this instrument along a typical life science experimental approach – the correlation of a fluorophore-tagged protein (pUL34-GFP of pseudorabies virus, PrV, the nuclear membrane-anchored component of the nuclear egress complex of the Herpesviridae which interacts with viral pUL31) in PrV pUL34-GFP/pUL31 coexpressing mammalian cells, with virus-induced vesicular structures in the nucleus, expanding the nucleoplasmic reticulum. Taken together, our results demonstrate new possibilities to study the role of specific proteins in substructures of adherent cells, especially of the nucleus in toto, accessible to electron microscopy in thinned samples only. PMID:22210307

  3. Final Report on Small Particle Speciation for Forensics Analysis by Soft X-ray Scanning Transmission X-ray Microscopy

    SciTech Connect

    Pacold, J. I.; Altman, A. B.; Donald, S B; Dai, Z.; Davisson, M. L.; Holliday, K S; Knight, K. B.; Kristo, M. J.; Minasian, S. G.; Nelson, A J; Tyliszczak, T; Booth, C. H.; Shuh, D. K.

    2016-09-30

    Materials of interest for nuclear forensic science are often highly heterogeneous, containing complex mixtures of actinide compounds in a wide variety of matrices. Scanning transmission X-ray microscopy (STXM) is ideally suited to study such materials, as it can be used to chemically image specimens by acquiring X-ray absorption near-edge spectroscopy (XANES) data with 25 nm spatial resolution. In particular, STXM in the soft X-ray synchrotron radiation regime (approximately 120 – 2000 eV) can collect spectroscopic information from the actinides and light elements in a single experiment. Thus, STXM combines the chemical sensitivity of X-ray absorption spectroscopy with high spatial resolution in a single non-destructive characterization method. This report describes the application of STXM to a broad range of nuclear materials. Where possible, the spectroscopic images obtained by STXM are compared with information derived from other analytical methods, and used to make inferences about the process history of each material. STXM measurements can yield information including the morphology of a sample, “elemental maps” showing the spatial distribution of major chemical constituents, and XANES spectra from localized regions of a sample, which may show spatial variations in chemical composition.

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

    SciTech Connect

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

    2014-09-15

    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.

  5. 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.

  6. 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.

  7. Metal Particle Growth During Glucose Hydrogenation over Ru/SiO2 Evaluated by X-ray Absorption Spectroscopy and Electron Microscopy

    SciTech Connect

    Maris,E.; Ketchie, W.; Oleshko, V.; Davis, R.

    2006-01-01

    Biorenewable resources such as carbohydrates are considered alternative feedstocks for oxygenated chemicals. This work investigates the stability of silica-supported Ru catalysts in the aqueous phase conversion of glucose to sorbitol. In situ X-ray absorption spectroscopy at the Ru K edge revealed that air-exposed silica-supported Ru was in an oxidized state but was subsequently reduced in aqueous solutions saturated with 40 bar H{sub 2} at 373 K. Furthermore, exposure to aqueous phase conditions resulted in the sintering of Ru particles on the silica surface. However, the presence of glucose in the aqueous phase stabilized the growth of the Ru particles. Batchwise hydrogenation of glucose at 373 K and 80 bar H{sub 2} over a Ru/SiO{sub 2} (2.67 wt %) catalyst is nearly 100% selective to sugar alcohol with an average turnover frequency of 0.21 {+-} 0.04 s{sup -1}. The hydrogenation reaction was not mass transfer limited according to the Madon-Boudart criterion.

  8. Scanning electron microscopy with energy dispersive X-ray spectrophotometry analysis of reciprocating and continuous rotary nickel-titanium instruments following root canal retreatment.

    PubMed

    Kalyoncuoğlu, Elif; Keskin, Cangül; Uzun, İsmail; Bengü, Aydın S; Guler, Buğra

    2016-01-01

    This study aimed to evaluate superficial defects and the composition of Reciproc R25 and ProTaper Retreatment file systems (Dentsply Maillefer, Ballaigues, Switzerland) used for retreatment. A total of 100 maxillary incisor teeth were randomly divided into the following two groups: Reciproc R25 (n = 25) and ProTaper Retreatment instrument (n = 75) groups. The nickel-titanium (Ni-Ti) compositions of the files before and after use were analyzed using energy dispersive X-ray spectrophotometry (EDX). Chi-square, Mann-Whitney U, and Kruskal-Wallis tests were used to analyze the data. ProTaper Retreatment instrument group showed a significantly higher number of defects than the Reciproc group (P < 0.05). No instrument fracture was detected. The presence of debris was observed in both groups before use, although the level was significantly higher in the ProTaper Retreatment group, which consisted of metals (P < 0.05). There was no significant difference between new and used instruments with regard to Ni-Ti composition (P < 0.05). EDX analysis showed that both the Reciproc and ProTaper Retreatment instruments had a Ni-Ti composition that was within the standards specified by the American Society of Testing and Materials. This study confirmed the use of both the Reciproc R25 file and ProTaper Retreatment file system for root canal filling removal in straight root canals as a safe procedure. (J Oral Sci 58, 401-406, 2016).

  9. Ultrastructural imaging and molecular modeling of live bacteria using soft x-ray contact microscopy with nanoseconds laser plasma radiation

    SciTech Connect

    Kado, M.; Richardson, M.C.; Gabel, K.; Torres, D.; Rajyaguru, J.; Muszynski, M.J.

    1995-12-31

    Detection for clinical diagnosis and study of microbial cell is performed by a combination of low magnification optical microscopy and direct and indirect labeling techniques. Visual ultrastructural studies on subcellular organelles are possible with variations of electron microscopy (thin section, scanning and freeze fracture), although specimen preparation steps such as fixation, dehydration, resin embedding, ultra-thin sectioning, coating and staining are very specialized, extensive and may introduce artifacts in the original sample. The development of high resolution x-ray microscopy is a new technique well suited to observe the intact structure of a biological specimen at high resolution without any artifacts. Here, x ray images of the various live bacteria, such as Staphylococcus and Streptococcus, and micromolecule such as chromosomal DNA from Escherichia coli, and Lipopolysaccharide from Burkholderia cepacia, are obtained with soft x-ray contact microscopy. A compact tabletop type glass laser system is used to produce x rays from Al, Si, and Au targets. The PMMA photoresists are used to record x-ray images. An AFM (atomic force microscope) is used to reproduce the x-ray images from the developed photoresists. The performance of the 50 nm spatial resolutions are achieved and images are able to be discussed on the biological view.

  10. Combined X-ray Microfluorescence and Atomic Force Microscopy Studies of Mg Distribution in Whole Cells

    SciTech Connect

    Lagomarsino, S.; Farruggia, G.; Trapani, V.; Mastrototaro, L.; Wolf, F.; Cedola, A.; Fratini, M.; Notargiacomo, A.; Bukreeva, I.; McNulty, I.; Vogt, S.; Kim, S.; Legnini, D.; Maier, J. A. M.

    2011-09-09

    We present in this paper a novel methodology that combines scanning x-ray fluorescencee microscopy and atomic force microscopy. The combination of these two techniques allows the determination of a concentration map of Mg in whole (not sectioned) cells.

  11. Soft X-ray Zone Plate Microscopy to 10 nm Resolution with XM-1 at the ALS

    SciTech Connect

    Chao Weilun; Attwood, David T.; Anderson, Erik H.; Harteneck, Bruce D.; Liddle, J. Alexander

    2007-01-19

    Soft x-ray zone plate microscopy provides a unique combination of capabilities that complement those of electron and scanning probe microscopies. Tremendous efforts are taken worldwide to achieve sub-10 nm resolution, which will permit extension of x-ray microscopy to a broader range of nanosciences and nanotechnologies. In this paper, the overlay nanofabrication technique is described, which permits zone width of 15 nm and below to be fabricated. The fabrication results of 12 nm zone plates, and the stacking of identical zone patterns for higher aspect ratio, are discussed.

  12. X-ray photoelectron and X-ray Auger electron spectroscopy studies of heavy ion irradiated C 60 films

    NASA Astrophysics Data System (ADS)

    Kumar, Amit; Singh, F.; Govind; Shivaprasad, S. M.; Avasthi, D. K.; Pivin, J. C.

    2008-09-01

    The influence of 200 MeV Au ion irradiation on the surface properties of polycrystalline fullerene films has been investigated. The X-ray photoelectron and X-ray Auger electron spectroscopies are employed to study the ion-induced modification of the fullerene, near the surface region. The shift of C 1s core level and decrease in intensity of shake-up satellite were used to investigate the structural changes (like sp 2 to sp 3 conversion) and reduction of π electrons, respectively, under heavy ion irradiation. Further, X-ray Auger electron spectroscopy was employed to investigate hybridization conversion qualitatively as a function of ion fluence.

  13. Deducing Electron Properties from Hard X-Ray Observations

    NASA Technical Reports Server (NTRS)

    Kontar, E. P.; Brown, J. C.; Emslie, A. G.; Hajdas, W.; Holman, G. D.; Hurford, G. J.; Kasparova, J.; Mallik, P. C. V.; Massone, A. M.; McConnell, M. L.; Piana, M.; Prato, M.; Schmahl, E. J.; Suarez-Garcia, E.

    2011-01-01

    X-radiation from energetic electrons is the prime diagnostic of flare-accelerated electrons. The observed X-ray flux (and polarization state) is fundamentally a convolution of the cross-section for the hard X-ray emission process(es) in question with the electron distribution function, which is in turn a function of energy, direction, spatial location and time. To address the problems of particle propagation and acceleration one needs to infer as much information as possible on this electron distribution function, through a deconvolution of this fundamental relationship. This review presents recent progress toward this goal using spectroscopic, imaging and polarization measurements, primarily from the Reuven Ramaty High Energy Solar Spectroscopic Imager (RHESSI). Previous conclusions regarding the energy, angular (pitch angle) and spatial distributions of energetic electrons in solar flares are critically reviewed. We discuss the role and the observational evidence of several radiation processes: free-free electron-ion, free-free electron-electron, free-bound electron-ion, photoelectric absorption and Compton backscatter (albedo), using both spectroscopic and imaging techniques. This unprecedented quality of data allows for the first time inference of the angular distributions of the X-ray-emitting electrons and improved model-independent inference of electron energy spectra and emission measures of thermal plasma. Moreover, imaging spectroscopy has revealed hitherto unknown details of solar flare morphology and detailed spectroscopy of coronal, footpoint and extended sources in flaring regions. Additional attempts to measure hard X-ray polarization were not sufficient to put constraints on the degree of anisotropy of electrons, but point to the importance of obtaining good quality polarization data in the future.

  14. Deducing Electron Properties from Hard X-Ray Observations

    NASA Technical Reports Server (NTRS)

    Kontar, E. P.; Brown, J. C.; Emslie, A. G.; Hajdas, W.; Holman, G. D.; Hurford, G. J.; Kasparova, J.; Mallik, P. C. V.; Massone, A. M.; McConnell, M. L.; hide

    2011-01-01

    X-radiation from energetic electrons is the prime diagnostic of flare-accelerated electrons. The observed X-ray flux (and polarization state) is fundamentally a convolution of the cross-section for the hard X-ray emission process(es) in question with the electron distribution function, which is in turn a function of energy, direction, spatial location and time. To address the problems of particle propagation and acceleration one needs to infer as much information as possible on this electron distribution function, through a deconvolution of this fundamental relationship. This review presents recent progress toward this goal using spectroscopic, imaging and polarization measurements, primarily from the Reuven Ramaty High Energy Solar Spectroscopic Imager (RHESSI). Previous conclusions regarding the energy, angular (pitch angle) and spatial distributions of energetic electrons in solar flares are critically reviewed. We discuss the role and the observational evidence of several radiation processes: free-free electron-ion, free-free electron-electron, free-bound electron-ion, photoelectric absorption and Compton backscatter (albedo), using both spectroscopic and imaging techniques. This unprecedented quality of data allows for the first time inference of the angular distributions of the X-ray-emitting electrons and improved model-independent inference of electron energy spectra and emission measures of thermal plasma. Moreover, imaging spectroscopy has revealed hitherto unknown details of solar flare morphology and detailed spectroscopy of coronal, footpoint and extended sources in flaring regions. Additional attempts to measure hard X-ray polarization were not sufficient to put constraints on the degree of anisotropy of electrons, but point to the importance of obtaining good quality polarization data in the future.

  15. Phase contrast hard x-ray microscopy with submicron resolution

    SciTech Connect

    Lagomarsino, S.; Cedola, A.; Cloetens, P.; Di Fonzo, S.; Jark, W.; Soullie, G.; Riekel, C.

    1997-11-01

    In this letter we present a hard x-ray phase contrast microscope based on the divergent and coherent beam exiting an x-ray waveguide. It uses lensless geometrical projection to magnify spatial variations in optical path length more than 700 times. Images of a nylon fiber and a gold test pattern were obtained with a resolution of 0.14 {mu}m in one direction. Exposure times as short as 0.1 s gave already visible contrast, opening the way to high resolution, real time studies. {copyright} {ital 1997 American Institute of Physics.}

  16. The physics of x-ray free-electron lasers

    NASA Astrophysics Data System (ADS)

    Pellegrini, C.; Marinelli, A.; Reiche, S.

    2016-01-01

    X-ray free-electron lasers (x-ray FELs) give us for the first time the possibility to explore structures and dynamical processes of atomic and molecular systems at the angstrom-femtosecond space and time scales. They generate coherent photon pulses with time duration of a few to 100 fs, peak power of 10 to 100 GW, over a wavelength range extending from about 100 nm to less than 1 Å. Using these novel and unique capabilities new scientific results are being obtained in atomic and molecular sciences, in areas of physics, chemistry, and biology. This paper reviews the physical principles, the theoretical models, and the numerical codes on which x-ray FELs are based, starting from a single electron spontaneous undulator radiation to the FEL collective instability of a high density electron beam, strongly enhancing the electromagnetic radiation field intensity and its coherence properties. A short review is presented of the main experimental properties of x-ray FELs, and the results are discussed of the most recent research to improve their longitudinal coherence properties, increase the peak power, and generate multicolor spectra.

  17. Design of an x-ray free electron laser undulator

    SciTech Connect

    Carr, R.

    1997-09-01

    An undulator designed to be used for an x-ray free electron laser has to meet a set of stringent requirements. With no optical cavity, an x-ray FeL operates in the single pass Self Amplified Spontaneous Emission (SASE) mode; an electron macropulse is microbunched by an undulator and the radiation it creates. The microbunched pulse emits spontaneous radiation and coherent FEL radiation, whose power may reach saturation in a sufficiently long and perfect undulator. The pulse must have low emittance and high current, and its trajectory in the undulator must keep the radiation and the pulse together with a very high degree of overlap. The authors shall consider the case of the Linear Coherent Light Source (LCLS) FEL project at SLAC, which is intended to create 1.5 {angstrom} x-rays using an electron beam with 15 GeV energy, 1.5{pi} mm-mrad normalized emittance, 3,400 A peak current, and 280 fsec FWHM bunch duration. They find that this 65 {micro}m rms diameter beam must overlap its radiation with a walk/off of no more than 5 {micro}m for efficient gain. This places severe limitations on the magnetic field errors and other mechanical tolerances. The following is a discussion of the undulator design, specifications, alignment, engineering, and beam position monitoring they plan to implement for the LCLS X-ray FEL.

  18. ELECTRON INJECTORS FOR NEXT GENERATION X-RAY SOURCES.

    SciTech Connect

    BLUEM,H.; BEN-ZVI,I.; SRINIVASAN-RAO,T.; ET AL.

    2004-08-02

    Next generation x-ray sources require very high-brightness electron beams that are typically at or beyond the present state-of-the-art, and thus place stringent and demanding requirements upon the electron injector parameters. No one electron source concept is suitable for all the diverse applications envisaged, which have operating characteristics ranging from high-average-current, quasi-CW, to high-peak-current, single-pulse electron beams. Advanced Energy Systems, in collaboration with various partners, is developing several electron injector concepts for these x-ray source applications. The performance and design characteristics of five specific RF injectors, spanning ''L'' to ''X''-band, normal-conducting to superconducting, and low repetition rate to CW, which are presently in various stages of design, construction or testing, is described. We also discuss the status and schedule of each with respect to testing.

  19. Magnetic soft x-ray microscopy-imaging fast spin dynamics inmagnetic nanostructures

    SciTech Connect

    Fischer, Peter; Kim, Dong-Hyun; Mesler, Brooke L.; Chao, Weilun; Sakdinawat, Anne E.; Anderson, Erik H.

    2007-06-01

    Magnetic soft X-ray microscopy combines 15nm spatial resolution with 70ps time resolution and elemental sensitivity. Fresnel zone plates are used as X-ray optics and X-ray magnetic circular dichroism serves as magnetic contrast mechanism. Thus scientifically interesting and technologically relevant low dimensional nanomagnetic systems can be imaged at fundamental length and ultrafast time scales in a unique way. Studies include magnetization reversal in magnetic multilayers, nanopatterned systems, vortex dynamics in nanoelements and spin current induced phenomena.

  20. Quantitative x-ray differential-interference-contrast microscopy with independently adjustable bias and shear

    SciTech Connect

    Nakamura, Takashi; Chang Chang

    2011-04-15

    We present a quantitative x-ray phase imaging method that can be readily implemented on existing x-ray microscopy facilities. This technique utilizes Fresnel zone plates both as imaging optical elements for magnification and as second-order grating structures for phase-shifting interferometry. By making high-resolution quantitative x-ray phase information widely available, we expect this work to have significant impact on nanoscale biological and material studies.

  1. Searching ultimate nanometrology for AlOx thickness in magnetic tunnel junction by analytical electron microscopy and X-ray reflectometry.

    PubMed

    Song, Se Ahn; Hirano, Tatsumi; Park, Jong Bong; Kaji, Kazutoshi; Kim, Ki Hong; Terada, Shohei

    2005-10-01

    Practical analyses of the structures of ultrathin multilayers in tunneling magneto resistance (TMR) and Magnetic Random Access Memory (MRAM) devices have been a challenging task because layers are very thin, just 1-2 nm thick. Particularly, the thinness (approximately 1 nm) and chemical properties of the AlOx barrier layer are critical to its magnetic tunneling property. We focused on evaluating the current TEM analytical methods by measuring the thickness and composition of an AlOx layer using several TEM instruments, that is, a round robin test, and cross-checked the thickness results with an X-ray reflectometry (XRR) method. The thickness measured by using HRTEM, HAADF-STEM, and zero-loss images was 1.1 nm, which agreed with the results from the XRR method. On the other hand, TEM-EELS measurements showed 1.8 nm for an oxygen 2D-EELS image and 3.0 nm for an oxygen spatially resolved EELS image, whereas the STEM-EDS line profile showed 2.5 nm in thickness. However, after improving the TEM-EELS measurements by acquiring time-resolved images, the measured thickness of the AlOx layer was improved from 1.8 nm to 1.4 nm for the oxygen 2D-EELS image and from 3.0 nm to 2.0 nm for the spatially resolved EELS image, respectively. Also the observed thickness from the EDS line profile was improved to 1.4 nm after more careful optimization of the experimental parameters. We found that EELS and EDS of one-dimensional line scans or two-dimensional elemental mapping gave a larger AlOx thickness even though much care was taken. The reasons for larger measured values can be found from several factors such as sample drift, beam damage, probe size, beam delocalization, and multiple scattering for the EDS images, and chromatic aberration, diffraction limit due to the aperture, delocalization, alignment between layered direction in samples, and energy dispersion direction in the EELS instrument for EELS images. In the case of STEM-EDS mapping with focused nanoprobes, it is always

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

    NASA Astrophysics Data System (ADS)

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

    2017-03-01

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

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

    PubMed

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

    2017-03-21

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

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

    PubMed Central

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

    2017-01-01

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

  5. Surface characterization of poly(N-isopropylacrylamide) grafted tissue culture polystyrene by electron beam irradiation, using atomic force microscopy, and X-ray photoelectron spectroscopy.

    PubMed

    Akiyama, Yoshikatsu; Kushida, Ai; Yamato, Masayuki; Kikuchi, Akihiko; Okano, Teruo

    2007-03-01

    To understand features of polymers grafted by electron beam (EB) irradiation method, we investigated topology of poly(N-isopropylacrylamide) (PIPAAm) grafted tissue culture polystyrene (TCPS) (PIPAAm-TCPS) prepared by EB irradiation, using atomic force microscopy (AFM) in air and under aqueous conditions. Furthermore, surfaces properties of PIPAAm-TCPS surfaces before and after cell culture were also examined for evaluation of functionality of the surface as biomaterials, using XPS analysis. Three types of PIPAAm-TCPSs with different graft densities (1.0+/-0.1, 1.6+/-0.1, and 2.0+/-0.1 microg/cm2 of the grafted) were obtained (abbreviated as 11PIPAAm-, 16PIPAAm-, and 20PIPAAm-TCPS) by using different initial monomer concentration (20, 55, and 65 wt%). Contact angles (costheta value) of the surfaces increased with an increase in density of the grafted polymer. AFM observation in air clearly revealed that original TCPS surface possesses scratched and grooved topology (ca. 10 nm height of the scratch), while PIPAAm-TCPSs surfaces exhibited nanoordered PIPAAm particle-like domains. The size of the particles also increased proportionally initial IPAAm monomer concentration. The 11PIPAAm-and 16PIPAAm-TCPS surfaces having ca. 10-30 nm and ca. 40-50 nm size of the particles also displayed scratched and grooved topology featured in basal TCPS. However, the larger sizes of the particles (ca. 40-100 nm) formed on 20PIPAAm-TCPS surfaces adequately conceals the topological feature of the basal TCPS surfaces. The AFM images indicate that the graft polymer is as ultra thin as the scratch and grooves featured on basal TCPS are discernible, and the grafted PIPAAm layer become thicker with an increase of the monomer concentration. For 16PIPAAm-TCPS surfaces, the nanoordered particles were also observable in aqueous conditions at 20 degrees C and 37 degrees C. Comparison between the images obtained at 20 degrees C and 37 degrees C suggest that the domains are not likely to exhibit

  6. Progress and prospects in soft x-ray holographic microscopy

    SciTech Connect

    Howells, M.R.; Jacobsen, C.; Kirz, J.; McQuaid, K.; Rothman, S.S.

    1987-12-01

    We report some of the latest developments in x-ray holography experiments and make some speculations about the limits of performance of the approaches currently in use. We also make some suggestions about where the technique can (and cannot) go in the future. 32 refs., 5 figs., 1 tab.

  7. A Novel Integrating Solid State Detector With Segmentation For Scanning Transmission Soft X-ray Microscopy

    NASA Astrophysics Data System (ADS)

    Feser, Michael; Jacobsen, Chris; Degeronimo, Gianluigi; Rehak, Pavel; Holl, Peter; Strueder, Lothar

    2003-03-01

    Scanning transmission x-ray microscopy (STXM) with soft x-rays has unique detector requirements, which are not readily met by commercially available detectors. For implementation of dark-field and phase contrast imaging modes a segmented detector is needed with the high signal to noise ratio of a counting detector and a high detective quantum efficiency. Since the market for STXM is very small, the development of specialized detector systems relies on the collaboration with detector specialists at research facilities. We report on the successful development of a segmented silicon detector for STXM, which has been carried out in collaboration between the x-ray microscopy research group at SUNY Stony Brook, the instrumentation division at Brookhaven National Laboratory and silicon x-ray detector specialists in Germany. This project illustrates the effectiveness of such arrangements and justifies the support of future efforts in developing dedicated detectors for synchrotron radiation experiments bringing together detector experts and experimenters. The developed detector features eight separate circular segments matched to the STXM geometry. Fast charge integrating electronics have been developed to match the short pixel dwell times in a synchrotron based scanning microscope (in the ms range for the NSLS). The noise level of 5 photons RMS per integration per channel (at 520 eV photon energy) and a 1500 photon capacity (corresponding to the well depth in a CCD detector) is well matched to the characteristics of the experiment. Combining the detector signals in an appropriate way, different imaging modes (i.e. bright field, dark field or phase contrast) can be selected. We discuss recent developments on simultaneous quantitative phase and amplitude contrast imaging using this segmented detector in conjunction with a Fourier filter reconstruction technique.

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

    SciTech Connect

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

    2016-10-04

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

  9. Direct imaging electron microscopy (EM) methods in modern structural biology: overview and comparison with X-ray crystallography and single-particle cryo-EM reconstruction in the studies of large macromolecules.

    PubMed

    Miyaguchi, Katsuyuki

    2014-10-01

    Determining the structure of macromolecules is important for understanding their function. The fine structure of large macromolecules is currently studied primarily by X-ray crystallography and single-particle cryo-electron microscopy (EM) reconstruction. Before the development of these techniques, macromolecular structure was often examined by negative-staining, rotary-shadowing and freeze-etching EM, which are categorised here as 'direct imaging EM methods'. In this review, the results are summarised by each of the above techniques and compared with respect to four macromolecules: the ryanodine receptor, cadherin, rhodopsin and the ribosome-translocon complex (RTC). The results of structural analysis of the ryanodine receptor and cadherin are consistent between each technique. The results obtained for rhodopsin vary to some extent within each technique and between the different techniques. Finally, the results for RTC are inconsistent between direct imaging EM and other analytical techniques, especially with respect to the space within RTC, the reasons for which are discussed. Then, the role of direct imaging EM methods in modern structural biology is discussed. Direct imaging methods should support and verify the results obtained by other analytical methods capable of solving three-dimensional molecular architecture, and they should still be used as a primary tool for studying macromolecule structure in vivo. © 2014 Société Française des Microscopies and Société de Biologie Cellulaire de France. Published by John Wiley & Sons Ltd.

  10. Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

    DOE PAGES

    Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; ...

    2009-11-01

    We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

  11. X-ray stereo microscopy for investigation of dynamics in soil

    SciTech Connect

    Gleber, S.-C.; Sedlmair, J.; Bertilson, M.; von Hofsten, O.; Heim,S.; Guttmann, P.; Hertz, H.; Fischer, P.; Thieme, J.

    2008-09-16

    The presented combination of stereo imaging and elemental mapping with soft X-ray microscopy reveals the spatial arrangement of naturally aqueous colloidal systems, e.g. iron oxides in soil colloid clusters. Changes in the spatial arrangement can be induced by manipulating the sample mounted to the X-ray microscope and thus be investigated directly.

  12. A compact x-ray free electron laser

    SciTech Connect

    Barletta, W.; Attac, M.; Cline, D.B.; Kolonko, J.; Wang, X.; Bhowmik, A.; Bobbs, B.; Cover, R.A.; Dixon, F.P.; Rakowsky, G.; Gallardo, J.; Pellegrini, C.; Westenskow, G.

    1988-09-09

    We present a design concept and simulation of the performance of a compact x-ray, free electron laser driven by ultra-high gradient rf-linacs. The accelerator design is based on recent advances in high gradient technology by a LLNL/SLAC/LBL collaboration and on the development of bright, high current electron sources by BNL and LANL. The GeV electron beams generated with such accelerators can be concerted to soft x-rays in the range from 2--10 nm by passage through short period, high fields strength wigglers as are being designed at Rocketdyne. Linear light sources of this type can produce trains of picosecond (or shorter) pulses of extremely high spectral brilliance suitable for flash holography of biological specimens in vivo and for studies of fast chemical reactions. 12 refs., 8 figs., 4 tabs.

  13. A compact X-ray free electron laser

    NASA Astrophysics Data System (ADS)

    Barletta, W.; Atac, M.; Cline, D. B.; Kolonko, J.; Wang, X.; Bhowmik, A.; Bobbs, B.; Cover, R. A.; Dixon, F. P.; Rakowsky, G.

    1988-09-01

    A design concept and simulation of the performance of a compact X-ray, free electron laser driven by ultra-high gradient RF-linacs is presented. The accelerator design is based on recent advances in high gradient technology by a LLNL/SLAC/LBL collaboration and on the development of bright, high current electron sources by BNL and LANL. The GeV electron beams generated with such accelerators can be converted to soft X-rays in the range from 2 to 10 nm by passage through short period, high fields strength wigglers as are being designed at Rocketdyne. Linear light sources of this type can produce trains of picosecond (or shorter) pulses of extremely high spectral brilliance suitable for flash holography of biological specimens in vivo and for studies of fast chemical reactions.

  14. High resolution X-ray CT for advanced electronics packaging

    NASA Astrophysics Data System (ADS)

    Oppermann, M.; Zerna, T.

    2017-02-01

    Advanced electronics packaging is a challenge for non-destructive Testing (NDT). More, smaller and mostly hidden interconnects dominate modern electronics components and systems. To solve the demands of customers to get products with a high functionality by low volume, weight and price (e.g. mobile phones, personal medical monitoring systems) often the designers use System-in-Package solutions (SiP). The non-destructive testing of such devices is a big challenge. So our paper will impart fundamentals and applications for non-destructive evaluation of inner structures of electronics packaging for quality assurance and reliability investigations with a focus on X-ray methods, especially on high resolution X-ray computed tomography (CT).

  15. Generation of apodized X-ray illumination and its application to scanning and diffraction microscopy.

    PubMed

    Khakurel, Krishna P; Kimura, Takashi; Nakamori, Hiroki; Goto, Takumi; Matsuyama, Satoshi; Sasaki, Tomoya; Takei, Masashi; Kohmura, Yoshiki; Ishikawa, Tetsuya; Yamauchi, Kazuto; Nishino, Yoshinori

    2017-01-01

    X-ray science has greatly benefited from the progress in X-ray optics. Advances in the design and the manufacturing techniques of X-ray optics are key to the success of various microscopic and spectroscopic techniques practiced today. Here the generation of apodized X-ray illumination using a two-stage deformable Kirkpatrick-Baez mirror system is presented. Such apodized illumination is marked by the suppression of the side-lobe intensities of the focused beam. Thus generated apodized illumination was employed to improve the image quality in scanning X-ray fluorescence microscopy. Imaging of a non-isolated object by coherent X-ray diffractive imaging with apodized illumination in a non-scanning mode is also presented.

  16. Transmission X-ray microscopy for full-field nano-imaging of biomaterials

    PubMed Central

    ANDREWS, JOY C; MEIRER, FLORIAN; LIU, YIJIN; MESTER, ZOLTAN; PIANETTA, PIERO

    2010-01-01

    Imaging of cellular structure and extended tissue in biological materials requires nanometer resolution and good sample penetration, which can be provided by current full-field transmission X-ray microscopic techniques in the soft and hard X-ray regions. The various capabilities of full-field transmission X-ray microscopy (TXM) include 3D tomography, Zernike phase contrast, quantification of absorption, and chemical identification via X-ray fluorescence and X-ray absorption near edge structure (XANES) imaging. These techniques are discussed and compared in light of results from imaging of biological materials including microorganisms, bone and mineralized tissue and plants, with a focus on hard X-ray TXM at ≤ 40 nm resolution. PMID:20734414

  17. Anti-contamination device for cryogenic soft X-ray diffraction microscopy

    DOE PAGES

    Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; ...

    2011-05-01

    Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens.

  18. Anti-contamination device for cryogenic soft X-ray diffraction microscopy

    PubMed Central

    Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; Turner, Joshua; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Jacobsen, Chris

    2011-01-01

    Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens. PMID:21547016

  19. Application of X-ray synchrotron microscopy instrumentation in biology

    SciTech Connect

    Gasperini, F. M.; Pereira, G. R.; Granjeiro, J. M.; Calasans-Maia, M. D.; Rossi, A. M.; Perez, C. A.; Lopes, R. T.; Lima, I.

    2011-07-01

    X-ray micro-fluorescence imaging technique has been used as a significant tool in order to investigate minerals contents in some kinds of materials. The aim of this study was to evaluate the elemental distribution of calcium and zinc in bone substitute materials (nano-hydroxyapatite spheres) and cortical bones through X-Ray Micro-fluorescence analysis with the increment of Synchrotron Radiation in order to evaluate the characteristics of the newly formed bone and its interface, the preexisting bone and biomaterials by the arrangement of collagen fibers and its birefringence. The elemental mapping was carried out at Brazilian Synchrotron Light Laboratory, Campinas - Sao Paulo, Brazil working at D09-XRF beam line. Based on this study, the results suggest that hydroxyapatite-based biomaterials are biocompatible, promote osteo-conduction and favored bone repair. (authors)

  20. Structural characterization of Al0.55Ga0.45N epitaxial layer determined by high resolution x-ray diffraction and transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Xu, Qing-Jun; Liu, Bin; Zhang, Shi-Ying; Tao, Tao; Xie, Zi-Li; Xiu, Xiang-Qian; Chen, Dun-Jun; Chen, Peng; Han, Ping; Zhang, Rong; Zheng, You-Dou

    2017-04-01

    Not Available Project supported by the National Key Research and Development Project of China (Grant No. 2016YFB0400100), the Hi-tech Research Project of China (Grant Nos. 2014AA032605 and 2015AA033305), the National Natural Science Foundation of China (Grant Nos. 61274003, 61422401, 51461135002, and 61334009), the Natural Science Foundation of Jiangsu Province, China (Grant Nos. BY2013077, BK20141320, and BE2015111), the Project of Green Young and Golden Phenix of Yangzhou City, the Postdoctoral Sustentation Fund of Jiangsu Province, China (Grant No. 1501143B), the Project of Shandong Provinceial Higher Educational Science and Technology Program, China (Grant No. J13LN08), the Solid State Lighting and Energy-saving Electronics Collaborative Innovation Center, Priority Academic Program Development of Jiangsu Higher Education Institutions (PAPD), and Research Funds from NJU-Yangzhou Institute of Opto-electronics.

  1. X-ray holographic microscopy with zone plates applied to biological samples in the water window using 3rd harmonic radiation from the free-electron laser FLASH.

    PubMed

    Gorniak, T; Heine, R; Mancuso, A P; Staier, F; Christophis, C; Pettitt, M E; Sakdinawat, A; Treusch, R; Guerassimova, N; Feldhaus, J; Gutt, C; Grübel, G; Eisebitt, S; Beyer, A; Gölzhäuser, A; Weckert, E; Grunze, M; Vartanyants, I A; Rosenhahn, A

    2011-06-06

    The imaging of hydrated biological samples - especially in the energy window of 284-540 eV, where water does not obscure the signal of soft organic matter and biologically relevant elements - is of tremendous interest for life sciences. Free-electron lasers can provide highly intense and coherent pulses, which allow single pulse imaging to overcome resolution limits set by radiation damage. One current challenge is to match both the desired energy and the intensity of the light source. We present the first images of dehydrated biological material acquired with 3rd harmonic radiation from FLASH by digital in-line zone plate holography as one step towards the vision of imaging hydrated biological material with photons in the water window. We also demonstrate the first application of ultrathin molecular sheets as suitable substrates for future free-electron laser experiments with biological samples in the form of a rat fibroblast cell and marine biofouling bacteria Cobetia marina.

  2. Near Edge X-Ray Absorption Fine Structure Spectroscopy with X-Ray Free-Electron Lasers

    SciTech Connect

    Bernstein, D.P.; Acremann, Y.; Scherz, A.; Burkhardt, M.; Stohr, J.; Beye, M.; Schlotter, W.F.; Beeck, T.; Sorgenfrei, F.; Pietzsch, A.; Wurth, W.; Fohlisch, A.; /Hamburg U.

    2009-12-11

    We demonstrate the feasibility of Near Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy on solids by means of femtosecond soft x-ray pulses from a free-electron laser (FEL). Our experiments, carried out at the Free-Electron Laser at Hamburg (FLASH), used a special sample geometry, spectrographic energy dispersion, single shot position-sensitive detection and a data normalization procedure that eliminates the severe fluctuations of the incident intensity in space and photon energy. As an example we recorded the {sup 3}D{sub 1} N{sub 4,5}-edge absorption resonance of La{sup 3+}-ions in LaMnO{sub 3}. Our study opens the door for x-ray absorption measurements on future x-ray FEL facilities.

  3. Evidence for beamed electrons in a limb X-ray flare observed by Hard X-Ray Imaging Spectrometer (HXIS)

    NASA Technical Reports Server (NTRS)

    Haug, Eberhard; Elwert, Gerhard

    1986-01-01

    The limb flare of November 18, 1980, 14:51 UT, was investigated on the basis of X-ray images taken by the Hard X-ray Imaging Spectrometer (HXIS) and of X-ray spectra from the Hard X-Ray Burst Spectrometer (HXRBS) aboard the Solar Maximum Mission (SMM). The impulsive burst was also recorded at microwave frequencies between 2 and 20 GHz whereas no optical flare and no radio event at frequencies below 1 GHz were reported. The flare occurred directly at the SW limb of the solar disk. Taking advantage of the spatial resolution of HXIS images, the time evolution of the X-radiation originating from relatively small source regions can be studied. Using Monte Carlo computations of the energy distribution of energetic electrons traversing the solar plasma, the bremsstrahlung spectra produced by the electrons were derived.

  4. Stochastic stimulated electronic x-ray Raman spectroscopy

    PubMed Central

    Kimberg, Victor; Rohringer, Nina

    2016-01-01

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

  5. High efficiency, multiterawatt x-ray free electron lasers

    NASA Astrophysics Data System (ADS)

    Emma, C.; Fang, K.; Wu, J.; Pellegrini, C.

    2016-02-01

    In this paper we present undulator magnet tapering methods for obtaining high efficiency and multiterawatt peak powers in x-ray free electron lasers (XFELs), a key requirement for enabling 3D atomic resolution single molecule imaging and nonlinear x-ray science. The peak power and efficiency of tapered XFELs is sensitive to time dependent effects, like synchrotron sideband growth. To analyze this dependence in detail we perform a comparative numerical optimization for the undulator magnetic field tapering profile including and intentionally disabling these effects. We show that the solution for the magnetic field taper profile obtained from time independent optimization does not yield the highest extraction efficiency when time dependent effects are included. Our comparative optimization is performed for a novel undulator designed specifically to obtain TW power x-ray pulses in the shortest distance: superconducting, helical, with short period and built-in strong focusing. This design reduces the length of the breaks between modules, decreasing diffraction effects, and allows using a stronger transverse electron focusing. Both effects reduce the gain length and the overall undulator length. We determine that after a fully time dependent optimization of a 100 m long Linac coherent light source-like XFEL we can obtain a maximum efficiency of 7%, corresponding to 3.7 TW peak radiation power. Possible methods to suppress the synchrotron sidebands, and further enhance the FEL peak power, up to about 6 TW by increasing the seed power and reducing the electron beam energy spread, are also discussed.

  6. Measurements of Electron Diffusion via Hard X-ray Detection

    NASA Astrophysics Data System (ADS)

    Clayton, D. J.; O'Connell, R.; Burke, D. R.; Chapman, B. E.; Goetz, J. A.; Kaufman, M. C.; Gobbin, M.; Marrelli, L.; Martin, P.; Piovesan, P.; Harvey, R. W.

    2006-10-01

    An upgraded array of hard x-ray (HXR) detectors has been implemented on MST to measure electron particle diffusion in globally improved confinement pulsed parallel current drive (PPCD) plasmas and locally improved confinement quasi-single- helicity (QSH) plasmas. Each of these plasmas confines runaway electrons that emit HXRs. The diagnostic is a multichord array of CdZnTe detectors sensitive to 10-300 keV x-rays. Recently added lead shielding blocks x-rays from outside collimated lines of sight. The Fokker-Planck code CQL3D, now with HXR flux from the entire array as a constraint, is used to compute the diffusion coefficient as a function of radius during PPCD. In QSH plasmas, where one mode dominates the core tearing mode spectrum, HXRs are observed when a dominant island emerges, and the HXR flux oscillates in phase with the rotation of this island. Modeling with the ORBIT code shows that runaway electrons are better confined inside the island than in the exterior stochastic region.

  7. Characterization of AN Electron-Cyclotron - Mirror Plasma as a Soft X-Ray Source for X-Ray Lithography

    NASA Astrophysics Data System (ADS)

    Goodman, Timothy Paul

    There exists an international race to reduce the linewidths of integrated circuits to the sub-micron level. The results of this race are likely to have a strong impact on both the economic and military independence of this country as our society relies more and more heavily on highly sophisticated electronic equipment in our daily lives and in the defense of the country. One of the leading technologies in attaining sub-micron linewidths is x-ray lithography. Results from the ECRIAXS computer code have suggested that a laboratory-sized electron-cyclotron-resonance -heated mirror plasma may be a viable source for x-ray lithography. This work attempts to investigate this suggestion. A foil-filtered x-ray PIN diode and an x-ray pinhole camera have been used to measure x-ray intensities from krypton and neon plasma. The spatially resolved spectral density of the negatives from the x-ray pinhole camera has been measured. A film modeling code (FILM) has been written which predicts the film response. The code includes the integrated spectral response of the film to plasma x-ray emission that has been filtered by a beryllium foil filter. The PIN diode also yields electron temperatures for the plasmas (T_{rm e} ~ 1.3-4.0 keV). The intensity measurements are compared to computations from the ECRIAXS code. The measurements of the spectrally integrated x-ray intensity are supplemented by the measurement of plasma parameters that can be directly compared with some of the ECRIAXS code outputs. It has been found that the plasma densities that are predicted by the code (e.g. 1.75 times 10^{12 } cm^{-3}) are significantly higher than the experimental measurements (e.g. 4.5 times 10^ {11} cm^{-3} ). Modifications to the code can explain some of the discrepancies; however, the results are reliable only to within an order of magnitude.

  8. Studying Nanoscale Magnetism and its Dynamics with Soft X-ray Microscopy

    SciTech Connect

    Mccall, Monnikue M; Fischer, Peter

    2008-05-01

    Magnetic soft X-ray microscopy allows for imaging magnetic structures at a spatial resolution down to 15nm and a time resolution in the sub-100ps regime. Inherent elemental specificity can be used to image the magnetic response of individual components such as layers in multilayered systems. This review highlights current achievements and discusses the future potential of magnetic soft X-ray microscopy at fsec X-ray sources where snapshot images of ultrafast spin dynamics with a spatial resolution below 10nm will become feasible.

  9. Imaging translocation and transformation of bioavailable selenium by Stanleya pinnata with X-ray microscopy.

    PubMed

    Amos, Wren; Webb, Samuel; Liu, Yijin; Andrews, Joy C; LeDuc, Danika L

    2012-09-01

    Selenium hyperaccumulator Stanleya pinnata, Colorado ecotype, was supplied with water-soluble and biologically available selenate or selenite. Selenium distribution and tissue speciation were established using X-ray microscopy (micro-X-ray fluorescence and transmission X-ray microscopy) in two dimensions and three dimensions. The results indicate that S. pinnata tolerates, accumulates, and volatilizes significant concentrations of selenium when the inorganic form supplied is selenite and may possess novel metabolic capacity to differentiate, metabolize, and detoxify selenite concentrations surpassing field concentrations. The results also indicate that S. pinnata is a feasible candidate to detoxify selenium-polluted soil sites, especially locations with topsoil polluted with soluble and biologically available selenite.

  10. Correcting lateral chromatic aberrations in non-monochromatic X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Falch, Ken Vidar; Detlefs, Carsten; Di Michiel, Marco; Snigireva, Irina; Snigirev, Anatoly; Mathiesen, Ragnvald H.

    2016-08-01

    Lateral chromatic aberration in microscopy based on refractive optics may be reduced significantly by adjustments to the illumination scheme. By taking advantage of a broadened bandwidth illumination, the proposed scheme could open for x-ray microscopy with spatial resolution in the range 150-200 nm at millisecond frame rates. The scheme is readily implemented and is achievable using only standard refractive x-ray lenses, which has the advantage of high efficiency. It also maximizes the transmission and removes the spatial filtering effects associated with absorption in x-ray lenses.

  11. The atomic structural dynamics of γ-Al2O3 supported Ir-Pt nanocluster catalysts prepared from a bimetallic molecular precursor: a study using aberration-corrected electron microscopy and X-ray absorption spectroscopy.

    PubMed

    Small, Matthew W; Sanchez, Sergio I; Menard, Laurent D; Kang, Joo H; Frenkel, Anatoly I; Nuzzo, Ralph G

    2011-03-16

    This study describes a prototypical, bimetallic heterogeneous catalyst: compositionally well-defined Ir-Pt nanoclusters with sizes in the range of 1-2 nm supported on γ-Al(2)O(3). Deposition of the molecular bimetallic cluster [Ir(3)Pt(3)(μ-CO)(3)(CO)(3)(η-C(5)Me(5))(3)] on γ-Al(2)O(3), and its subsequent reduction with hydrogen, provides highly dispersed supported bimetallic Ir-Pt nanoparticles. Using spherical aberration-corrected scanning transmission electron microscopy (C(s)-STEM) and theoretical modeling of synchrotron-based X-ray absorption spectroscopy (XAS) measurements, our studies provide unambiguous structural assignments for this model catalytic system. The atomic resolution C(s)-STEM images reveal strong and specific lattice-directed strains in the clusters that follow local bonding configurations of the γ-Al(2)O(3) support. Combined nanobeam diffraction (NBD) and high-resolution transmission electron microscopy (HRTEM) data suggest the polycrystalline γ-Al(2)O(3) support material predominantly exposes (001) and (011) surface planes (ones commensurate with the zone axis orientations frequently exhibited by the bimetallic clusters). The data reveal that the supported bimetallic clusters exhibit complex patterns of structural dynamics, ones evidencing perturbations of an underlying oblate/hemispherical cuboctahedral cluster-core geometry with cores that are enriched in Ir (a result consistent with models based on surface energetics, which favor an ambient cluster termination by Pt) due to the dynamical responses of the M-M bonding to the specifics of the adsorbate and metal-support interactions. Taken together, the data demonstrate that strong temperature-dependent charge-transfer effects occur that are likely mediated variably by the cluster-support, cluster-adsorbate, and intermetallic bonding interactions.

  12. Analysis of particles produced during airbag deployment by scanning electron microscopy with energy dispersive x-ray spectroscopy and their deposition on surrounding surfaces: a mid-research summary

    NASA Astrophysics Data System (ADS)

    Wyatt, J. Matney

    2011-06-01

    Airbags can be encountered in forensic work when investigating a car crash and are typically constructed with primerlike material to begin the deployment apparatus. The mechanisms of airbag deployment can produce particles ideal for scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDS) analysis. A recent study published by Berk studied airbags with vents and showed that it is possible for particles generated from the deployment of these airbags to deposit on surfaces in the vehicle as the airbags deflate.1 Another paper published by Berk reported particles similar in morphology and composition to primer gunshot residue (GSR) are produced by side impact airbags.2 This paper's aim will be to show mid-point results of a study still in progress in which non-vented airbags were analyzed to determine if they exhibited the same particle depositing features as their vented airbag counterparts. Further investigation in this study is being performed to find more airbags which produce primer gunshot residue-like particles containing lead, barium, and antimony from airbag deployment. To date, the study has resulted in (1) non-vented airbags exhibiting deposition of particles suitable for SEM/EDS analysis and (2) no gunshot residue-like particles being detected from the airbag residues studied thus far.

  13. Scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX) and aerosol time-of-flight mass spectrometry (ATOFMS) single particle analysis of metallurgy plant emissions.

    PubMed

    Arndt, J; Deboudt, K; Anderson, A; Blondel, A; Eliet, S; Flament, P; Fourmentin, M; Healy, R M; Savary, V; Setyan, A; Wenger, J C

    2016-03-01

    The chemical composition of single particles deposited on industrial filters located in three different chimneys of an iron-manganese (Fe-Mn) alloy manufacturing plant have been compared using aerosol time-of-flight mass spectrometry (ATOFMS) and scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX). Very similar types of particles were observed using both analytical techniques. Calcium-containing particles dominated in the firing area of the sintering unit, Mn and/or Al-bearing particles were observed at the cooling area of the sintering unit, while Mn-containing particles were dominant at the smelting unit. SEM-EDX analysis of particles collected downstream of the industrial filters showed that the composition of the particles emitted from the chimneys is very similar to those collected on the filters. ATOFMS analysis of ore samples was also performed to identify particulate emissions that could be generated by wind erosion and manual activities. Specific particle types have been identified for each emission source (chimneys and ore piles) and can be used as tracers for source apportionment of ambient PM measured in the vicinity of the industrial site.

  14. Field-emission scanning electron microscopy and energy-dispersive x-ray analysis to understand the role of tannin-based dyes in the degradation of historical wool textiles.

    PubMed

    Restivo, Annalaura; Degano, Ilaria; Ribechini, Erika; Pérez-Arantegui, Josefina; Colombini, Maria Perla

    2014-10-01

    An innovative approach, combining field-emission scanning electron microscopy (FESEM) with energy dispersive X-ray spectroscopy (EDX) analysis, is presented to investigate the degradation mechanisms affecting tannin-dyed wool. In fact, tannin-dyed textiles are more sensitive to degradation then those dyed with other dyestuffs, even in the same conservation conditions. FESEM-EDX was first used to study a set of 48 wool specimens (artificially aged) dyed with several raw materials and mordants, and prepared according to historical dyeing recipes. EDX analysis was performed on the surface of wool threads and on their cross-sections. In addition, in order to validate the model formulated by the analysis of reference materials, several samples collected from historical and archaeological textiles were subjected to FESEM-EDX analysis. FESEM-EDX investigations enabled us to reveal the correlation between elemental composition and morphological changes. In addition, aging processes were clarified by studying changes in the elemental composition of wool from the protective cuticle to the fiber core in cross-sections. Morphological and elemental analysis of wool specimens and of archaeological and historical textiles showed that the presence of tannins increases wool damage, primarily by causing a sulfur decrease and fiber oxidation.

  15. Investigation of the structure, elemental and phase compositions of Fe3O4-SiO2 composite layers by scanning electron microscopy, X-ray spectroscopy, and thermal nitrogen desorption methods

    NASA Astrophysics Data System (ADS)

    Al'myashev, V. I.; Gareev, K. G.; Ionin, S. A.; Levitskii, V. S.; Moshnikov, V. A.; Terukov, E. I.

    2014-11-01

    The composite layers formed by drying a Fe3O4-SiO2-based colloidal solution were studied. The colloidal solution was obtained by the precipitation of Fe3O4 in the presence of highly dispersed silicon dioxide synthesized by the sol-gel method from a tetraethoxysilane alcohol solution. The microstructure and composition of the layers were analyzed using scanning electron microscopy, energy-dispersive X-ray microanalysis, thermal nitrogen desorption, and Raman spectroscopy. The emphasis was placed on the study of phase transitions in iron oxides under laser radiation. It was found that the tetraethoxysilane content has a substantial influence on the ratio of iron oxide and silicon dioxide in the layer, the specific surface area of SiO2 powders, the threshold laser radiation power necessary to induce the Fe3O4 α -Fe2O3 phase transformation, and on the position of the maximum of the absorption band corresponding to the A 1 g vibrations in α-Fe2O3.

  16. Epitaxial BaTiO{sub 3}(100) films on Pt(100): A low-energy electron diffraction, scanning tunneling microscopy, and x-ray photoelectron spectroscopy study

    SciTech Connect

    Foerster, Stefan; Huth, Michael; Schindler, Karl-Michael; Widdra, Wolf

    2011-09-14

    The growth of epitaxial ultrathin BaTiO{sub 3} films on a Pt(100) substrate has been studied by scanning tunneling microscopy (STM), low-energy electron diffraction (LEED), and x-ray photoelectron spectroscopy (XPS). The films have been prepared by radio-frequency-assisted magnetron sputter deposition at room temperature and develop a long-range order upon annealing at 900 K in O{sub 2}. By adjusting the Ar and O{sub 2} partial pressures of the sputter gas, the stoichiometry was tuned to match that of a BaTiO{sub 3}(100) single crystal as determined by XPS. STM reveals the growth of continuous BaTiO{sub 3} films with unit cell high islands on top. With LEED already for monolayer thicknesses, the formation of a BaTiO{sub 3}(100)-(1 x 1) structure has been observed. Films of 2-3 unit cell thickness show a brilliant (1 x 1) LEED pattern for which an extended set of LEED I-V data has been acquired. At temperatures above 1050 K the BaTiO{sub 3} thin film starts to decay by formation of vacancy islands. In addition (4 x 4) and (3 x 3) surface reconstructions develop upon prolonged heating.

  17. Two-dimensional X-ray diffraction and transmission electron microscopy study on the effect of magnetron sputtering atmosphere on GaN/SiC interface and gallium nitride thin film crystal structure

    SciTech Connect

    Shen, Huaxiang; Zhu, Guo-Zhen; Botton, Gianluigi A.; Kitai, Adrian

    2015-03-21

    The growth mechanisms of high quality GaN thin films on 6H-SiC by sputtering were investigated by X-ray diffraction (XRD) and scanning transmission electron microscopy (STEM). The XRD θ-2θ scans show that high quality (0002) oriented GaN was deposited on 6H-SiC by reactive magnetron sputtering. Pole figures obtained by 2D-XRD clarify that GaN thin films are dominated by (0002) oriented wurtzite GaN and (111) oriented zinc-blende GaN. A thin amorphous silicon oxide layer on SiC surfaces observed by STEM plays a critical role in terms of the orientation information transfer from the substrate to the GaN epilayer. The addition of H{sub 2} into Ar and/or N{sub 2} during sputtering can reduce the thickness of the amorphous layer. Moreover, adding 5% H{sub 2} into Ar can facilitate a phase transformation from amorphous to crystalline in the silicon oxide layer and eliminate the unwanted (33{sup ¯}02) orientation in the GaN thin film. Fiber texture GaN thin films can be grown by adding 10% H{sub 2} into N{sub 2} due to the complex reaction between H{sub 2} and N{sub 2}.

  18. Structural enzymology using X-ray free electron lasers

    PubMed Central

    Kupitz, Christopher; Olmos, Jose L.; Holl, Mark; Tremblay, Lee; Pande, Kanupriya; Pandey, Suraj; Oberthür, Dominik; Hunter, Mark; Liang, Mengning; Aquila, Andrew; Tenboer, Jason; Calvey, George; Katz, Andrea; Chen, Yujie; Wiedorn, Max O.; Knoska, Juraj; Meents, Alke; Majriani, Valerio; Norwood, Tyler; Poudyal, Ishwor; Grant, Thomas; Miller, Mitchell D.; Xu, Weijun; Tolstikova, Aleksandra; Morgan, Andrew; Metz, Markus; Martin-Garcia, Jose M.; Zook, James D.; Roy-Chowdhury, Shatabdi; Coe, Jesse; Nagaratnam, Nirupa; Meza, Domingo; Fromme, Raimund; Basu, Shibom; Frank, Matthias; White, Thomas; Barty, Anton; Bajt, Sasa; Yefanov, Oleksandr; Chapman, Henry N.; Zatsepin, Nadia; Nelson, Garrett; Weierstall, Uwe; Spence, John; Schwander, Peter; Pollack, Lois; Fromme, Petra; Ourmazd, Abbas; Phillips, George N.; Schmidt, Marius

    2016-01-01

    Mix-and-inject serial crystallography (MISC) is a technique designed to image enzyme catalyzed reactions in which small protein crystals are mixed with a substrate just prior to being probed by an X-ray pulse. This approach offers several advantages over flow cell studies. It provides (i) room temperature structures at near atomic resolution, (ii) time resolution ranging from microseconds to seconds, and (iii) convenient reaction initiation. It outruns radiation damage by using femtosecond X-ray pulses allowing damage and chemistry to be separated. Here, we demonstrate that MISC is feasible at an X-ray free electron laser by studying the reaction of M. tuberculosis ß-lactamase microcrystals with ceftriaxone antibiotic solution. Electron density maps of the apo-ß-lactamase and of the ceftriaxone bound form were obtained at 2.8 Å and 2.4 Å resolution, respectively. These results pave the way to study cyclic and non-cyclic reactions and represent a new field of time-resolved structural dynamics for numerous substrate-triggered biological reactions. PMID:28083542

  19. Structural enzymology using X-ray free electron lasers.

    PubMed

    Kupitz, Christopher; Olmos, Jose L; Holl, Mark; Tremblay, Lee; Pande, Kanupriya; Pandey, Suraj; Oberthür, Dominik; Hunter, Mark; Liang, Mengning; Aquila, Andrew; Tenboer, Jason; Calvey, George; Katz, Andrea; Chen, Yujie; Wiedorn, Max O; Knoska, Juraj; Meents, Alke; Majriani, Valerio; Norwood, Tyler; Poudyal, Ishwor; Grant, Thomas; Miller, Mitchell D; Xu, Weijun; Tolstikova, Aleksandra; Morgan, Andrew; Metz, Markus; Martin-Garcia, Jose M; Zook, James D; Roy-Chowdhury, Shatabdi; Coe, Jesse; Nagaratnam, Nirupa; Meza, Domingo; Fromme, Raimund; Basu, Shibom; Frank, Matthias; White, Thomas; Barty, Anton; Bajt, Sasa; Yefanov, Oleksandr; Chapman, Henry N; Zatsepin, Nadia; Nelson, Garrett; Weierstall, Uwe; Spence, John; Schwander, Peter; Pollack, Lois; Fromme, Petra; Ourmazd, Abbas; Phillips, George N; Schmidt, Marius

    2017-07-01

    Mix-and-inject serial crystallography (MISC) is a technique designed to image enzyme catalyzed reactions in which small protein crystals are mixed with a substrate just prior to being probed by an X-ray pulse. This approach offers several advantages over flow cell studies. It provides (i) room temperature structures at near atomic resolution, (ii) time resolution ranging from microseconds to seconds, and (iii) convenient reaction initiation. It outruns radiation damage by using femtosecond X-ray pulses allowing damage and chemistry to be separated. Here, we demonstrate that MISC is feasible at an X-ray free electron laser by studying the reaction of M. tuberculosis ß-lactamase microcrystals with ceftriaxone antibiotic solution. Electron density maps of the apo-ß-lactamase and of the ceftriaxone bound form were obtained at 2.8 Å and 2.4 Å resolution, respectively. These results pave the way to study cyclic and non-cyclic reactions and represent a new field of time-resolved structural dynamics for numerous substrate-triggered biological reactions.

  20. Structural enzymology using X-ray free electron lasers

    DOE PAGES

    Kupitz, Christopher; Olmos, Jose L.; Holl, Mark; ...

    2017-07-01

    Mix-and-inject serial crystallography (MISC) is a technique designed to image enzyme catalyzed reactions in which small protein crystals are mixed with a substrate just prior to being probed by an X-ray pulse. This approach offers several advantages over flow cell studies. It provides (i) room temperature structures at near atomic resolution, (ii) time resolution ranging from microseconds to seconds, and (iii) convenient reaction initiation. It outruns radiation damage by using femtosecond X-ray pulses allowing damage and chemistry to be separated. Here, we demonstrate that MISC is feasible at an X-ray free electron laser by studying the reaction of M. tuberculosismore » ß-lactamase microcrystals with ceftriaxone antibiotic solution. Electron density maps of the apo-ß-lactamase and of the ceftriaxone bound form were obtained at 2.8 Å and 2.4 Å resolution, respectively. Finally, these results pave the way to study cyclic and non-cyclic reactions and represent a new field of time-resolved structural dynamics for numerous substrate-triggered biological reactions.« less

  1. Suborbital Soft X-Ray Spectroscopy with Gaseous Electron Multipliers

    NASA Astrophysics Data System (ADS)

    Rogers, Thomas D.

    This thesis consists of the design, fabrication, and launch of a sounding rocket payload to observe the spectrum of the soft X-ray emission (0.1-1 keV) from the Cygnus Loop supernova remnant. This instrument, designated the Off-plane Grating Rocket for Extended Source Spectroscopy (OGRESS), was launched from White Sands Missile Range on May 2nd, 2015. The X-ray spectrograph incorporated a wire-grid focuser feeding an array of gratings in the extreme off-plane mount which dispersed the spectrum onto Gaseous Electron Multiplier (GEM) detectors. The gain characteristics of OGRESS's GEM detectors were fully characterized with respect to applied voltage and internal gas pressure, allowing operational settings to be optimized. The GEMs were optimized to operate below laboratory atmospheric pressure, allowing lower applied voltages, thus reducing the risk of both electrical arcing and tearing of the thin detector windows. The instrument recorded 388 seconds of data and found highly uniform count distributions over both detector faces, in sharp contrast to the expected thermal line spectrum. This signal is attributed to X-ray fluorescence lines generated inside the spectrograph. The radiation is produced when thermal ionospheric particles are accelerated into the interior walls of the spectrograph by the high voltages of the detector windows. A fluorescence model was found to fit the flight data better than modeled supernova spectra. Post-flight testing and analysis revealed that electrons produce distinct signal on the detectors which can also be successfully modeled as fluorescence emission.

  2. Note: Studies on x-ray production in electron cyclotron resonance x-ray source based on ridged cylindrical cavity

    SciTech Connect

    Selvakumaran, T. S.; Baskaran, R.

    2012-02-15

    A ridged cylindrical cavity has been designed using MICROWAVE STUDIO programme and it is used in the electron cyclotron resonance (ECR) x-ray source. The experimental parameters of the source are optimized for maximizing the x-ray output, and an x-ray dose rate of {approx}1000 {mu}Sv/h was observed at 20 cm from the port, for 500 W of microwave power without using any target. With the molybdenum target located at optimum position of the ridged cavity, the dose rate is found to be increased only by 10%. In order to understand the experimental observation, the electric field pattern of the cavity with the target placed at various radial distances is studied. In this note, the experimental and theoretical studies on ECR x-ray source using the ridged cylindrical cavity are presented.

  3. Scanning transmission x-ray microscopy of unaltered biological specimens

    SciTech Connect

    Iskander, N.

    1987-05-01

    A scanning transmission x-ray microscope at the National Synchrotron Light Source was used to image fresh, wet biological specimens at 32 Angstroms, with resolution better than 750 Angstroms. A gold Fresnel zone plate (outer zone width 500 Angstroms) was used to focus the undulator radiation, and the sample was scanned through the spot. Absorption data was recorded digitally as a gridded array. The major accomplishment of the experiment was the demonstration of the ability to image biological samples in their natural state with high resolution and natural elemental contrast mechanisms. This was achieved through the design of a sample holder that maintains an aqueous environment for the sample, yet is transparent to x-rays at 32 Angstroms. The specimens used were isolated zymogen granules (approximately 1 micron diameter) from the pancreatic acinar cells of rats. The absorption data were correlated to protein concentration, and estimates of the protein concentrations within the granules were obtained. The data also yields some information about the spatial organization of the protein in the granules, and our data is compared to models for the internal structure. The success of this experiment points toward future opportunities for dynamical studies on living systems. 6 refs., 28 figs., 2 tabs.

  4. Quantitative Electron-Excited X-Ray Microanalysis of Borides, Carbides, Nitrides, Oxides, and Fluorides with Scanning Electron Microscopy/Silicon Drift Detector Energy-Dispersive Spectrometry (SEM/SDD-EDS) and NIST DTSA-II.

    PubMed

    Newbury, Dale E; Ritchie, Nicholas W M

    2015-10-01

    A scanning electron microscope with a silicon drift detector energy-dispersive X-ray spectrometer (SEM/SDD-EDS) was used to analyze materials containing the low atomic number elements B, C, N, O, and F achieving a high degree of accuracy. Nearly all results fell well within an uncertainty envelope of ±5% relative (where relative uncertainty (%)=[(measured-ideal)/ideal]×100%). Quantification was performed with the standards-based "k-ratio" method with matrix corrections calculated based on the Pouchou and Pichoir expression for the ionization depth distribution function, as implemented in the NIST DTSA-II EDS software platform. The analytical strategy that was followed involved collection of high count (>2.5 million counts from 100 eV to the incident beam energy) spectra measured with a conservative input count rate that restricted the deadtime to ~10% to minimize coincidence effects. Standards employed included pure elements and simple compounds. A 10 keV beam was employed to excite the K- and L-shell X-rays of intermediate and high atomic number elements with excitation energies above 3 keV, e.g., the Fe K-family, while a 5 keV beam was used for analyses of elements with excitation energies below 3 keV, e.g., the Mo L-family.

  5. Flash imaging of fine structures of cellular organelles by contact x-ray microscopy with a high intensity laser plasma x-ray source

    NASA Astrophysics Data System (ADS)

    Kado, Masataka; Ishino, Masahiko; Kishimoto, Maki; Tamotsu, Satoshi; Yasuda, Keiko; Kinjo, Yasuhito; Shinohara, Kunio

    2011-09-01

    X-ray flash imaging by contact microscopy with a highly intense laser-plasma x-ray source was achieved for the observation of wet biological cells. The exposure time to obtain a single x-ray image was about 600 ps as determined by the pulse duration of the driving laser pulse. The x-ray flash imaging makes it possible to capture an x-ray image of living biological cells without any artificial treatment such as staining, fixation, freezing, and so on. The biological cells were cultivated directly on the surface of the silicon nitride membranes, which are used for the x-ray microscope. Before exposing the cells to x-rays they were observed by a conventional fluorescent microscope as reference, since the fluorescent microscopes can visualize specific organelles stained with fluorescent dye. Comparing the x-ray images with the fluorescent images of the exact same cells, each cellular organelle observed in the x-ray images was identified one by one and actin filaments and mitochondria were clearly identified in the x-ray images.

  6. Focused ion beam patterned Fe thin films A study by selective area Stokes polarimetry and soft x-Ray microscopy

    SciTech Connect

    Cook, P. J.; Shen, T. H.; Grundy, P. J.; Im, M.-Y.; Fischer, P.; Morton, S. A.; Kilcoyne, A. L. D.

    2010-11-14

    We demonstrate the potential to modify the magnetic behavior and structural properties of ferromagnetic thin films using focused ion beam 'direct-write' lithography. Patterns inspired by the split-ring resonators often used as components in meta-materials were defined upon 15 nm Fe films using a 30 keV Ga{sup +} focused ion beam at a dose of 2 x 10{sup 16} ions cm{sup -2}. Structural, chemical and magnetic changes to the Fe were studied using transmission soft X-ray microscopy at the ALS, Berkeley CA. X-ray absorption spectra showed a 23% reduction in the thickness of the film in the Ga irradiated areas, but no chemical change to the Fe was evident. X-ray images of the magnetic reversal process show domain wall pinning around the implanted areas, resulting in an overall increase in the coercivity of the film. Transmission electron microscopy showed significant grain growth in the implanted regions.

  7. Atmospheric Electron-Induced X-Ray Spectrometer (AEXS) Development

    NASA Technical Reports Server (NTRS)

    Wilcox, Jaroslava Z.; Urgiles, Eduardo; Toda, Risaku; George, Thomas; Douglas, Susanne; Crisp, Joy

    2005-01-01

    This paper describes the progress in the development of the so-called Atmospheric Electron X-ray Spectrometer (AEXS) instrument in our laboratory at JPL. The AEXS is a novel miniature instrument concept based on the excitation of characteristic X-Ray Fluorescence (XRF) and luminescence spectra using a focused electron beam, for non-destructive evaluation of surfaces of samples in situ, in planetary ambient atmosphere. In situ operation is obtained through the use of a thin electron transmissive membrane to isolate the vacuum within the AEXS electron source from the outside ambient atmosphere. By using a focused electron beam, the impinging electrons on samples in the external atmosphere excite XRF spectra from the irradiated spots with high-to-medium spatial resolution. The XRF spectra are analyzed using an energy-dispersive detector to determine surface elemental composition. The use of high- intensity electron beam results in rapid spectrum acquisition (several minutes), and consequently low energy consumption (several tens of Joules) per acquired XRF spectrum in comparison to similar portable instruments.

  8. Soft X-Ray Microscopy Radiation Damage On Fixed Cells Investigated With Synchrotron Radiation FTIR Microscopy.

    PubMed

    Gianoncelli, A; Vaccari, L; Kourousias, G; Cassese, D; Bedolla, D E; Kenig, S; Storici, P; Lazzarino, M; Kiskinova, M

    2015-05-14

    Radiation damage of biological samples remains a limiting factor in high resolution X-ray microscopy (XRM). Several studies have attempted to evaluate the extent and the effects of radiation damage, proposing strategies to minimise or prevent it. The present work aims to assess the impact of soft X-rays on formalin fixed cells on a systematic manner. The novelty of this approach resides on investigating the radiation damage not only with XRM, as often reported in relevant literature on the topic, but by coupling it with two additional independent non-destructive microscopy methods: Atomic Force Microscopy (AFM) and FTIR Microscopy (FTIRM). Human Embryonic Kidney 293 cells were exposed to different radiation doses at 1 keV. In order to reveal possible morphological and biochemical changes, the irradiated cells were systematically analysed with AFM and FTIRM before and after. Results reveal that while cell morphology is not substantially affected, cellular biochemical profile changes significantly and progressively when increasing dose, resulting in a severe breakdown of the covalent bonding network. This information impacts most soft XRM studies on fixed cells and adds an in-depth understanding of the radiation damage for developing better prevention strategies.

  9. Ultra-high vacuum compatible optical chopper system for synchrotron x-ray scanning tunneling microscopy

    SciTech Connect

    Chang, Hao; Cummings, Marvin; Shirato, Nozomi; Stripe, Benjamin; Preissner, Curt; Freeland, John W.; Rosenmann, Daniel; Kersell, Heath; Hla, Saw-Wai; Rose, Volker

    2016-01-28

    High-speed beam choppers are a crucial part of time-resolved x-ray studies as well as a necessary component to enable elemental contrast in synchrotron x-ray scanning tunneling microscopy (SX-STM). However, many chopper systems are not capable of operation in vacuum, which restricts their application to x-ray studies with high photon energies, where air absorption does not present a significant problem. To overcome this limitation, we present a fully ultra-high vacuum (UHV) compatible chopper system capable of operating at variable chopping frequencies up to 4 kHz. The lightweight aluminum chopper disk is coated with Ti and Au films to provide the required beam attenuation for soft and hard x-rays with photon energies up to about 12 keV. The chopper is used for lock-in detection of x-ray enhanced signals in SX-STM.

  10. Phase-contrast microscopy at high x-ray energy with a laboratory setup.

    PubMed

    Endrizzi, Marco; Vittoria, Fabio A; Diemoz, Paul C; Lorenzo, Rodolfo; Speller, Robert D; Wagner, Ulrich H; Rau, Christoph; Robinson, Ian K; Olivo, Alessandro

    2014-06-01

    We report on the design and realization of an x-ray imaging system for quantitative phase-contrast microscopy at high x-ray energy with laboratory-scale instrumentation. Phase and amplitude were separated quantitatively at x-ray energies up to 80 keV with micrometric spatial resolution. The accuracy of the results was tested against numerical simulations, and the spatial resolution was experimentally quantified by measuring a Siemens star phase object. This simple setup should find broad application in those areas of x-ray imaging where high energy and spatial resolution are simultaneously required and in those difficult cases where the sample contains materials with similar x-ray absorption.

  11. Electronic structure of cobalt doped CdSe quantum dots using soft X-ray spectroscopy

    SciTech Connect

    Joshua T. Wright; Su, Dong; van Buuren, Tony; Meulenberg, Robert W.

    2014-08-21

    The electronic structure and magnetic properties of cobalt doped CdSe quantum dots (QDs) are studied using electron microscopy, soft X-ray spectroscopy, and magnetometry. Magnetometry measurements suggest these QDs are superparamagnetic, contrary to a spin-glass state observed in the bulk analogue. Moreover, the electron microscopy shows well formed QDs, but with cobalt existing as doped into the QD and as unreacted species not contained in the QD. X-ray absorption measurements at the Co L3-edge suggest that changes in spectra features as a function of particle size can be described considering combination of a cobalt ion in a tetrahedral crystal field and an octahedrally coordinated (impurity) phase. With decreasing particle sizes, the impurity phase increases, suggesting that small QDs can be difficult to dope.

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

    PubMed Central

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

    2016-01-01

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

  13. Quantitative x-ray magnetic circular dichroism mapping with high spatial resolution full-field magnetic transmission soft x-ray spectro-microscopy

    NASA Astrophysics Data System (ADS)

    Robertson, MacCallum J.; Agostino, Christopher J.; N'Diaye, Alpha T.; Chen, Gong; Im, Mi-Young; Fischer, Peter

    2015-05-01

    The spectroscopic analysis of X-ray magnetic circular dichroism (XMCD), which serves as strong and element-specific magnetic contrast in full-field magnetic transmission soft x-ray microscopy, is shown to provide information on the local distribution of spin (S) and orbital (L) magnetic moments down to a spatial resolution of 25 nm limited by the x-ray optics used in the x-ray microscope. The spatially resolved L/S ratio observed in a multilayered (Co 0.3 nm/Pt 0.5 nm) × 30 thin film exhibiting a strong perpendicular magnetic anisotropy decreases significantly in the vicinity of domain walls, indicating a non-uniform spin configuration in the vertical profile of a domain wall across the thin film. Quantitative XMCD mapping with x-ray spectro-microscopy will become an important characterization tool for systems with topological or engineered magnetization inhomogeneities.

  14. Quantitative x-ray magnetic circular dichroism mapping with high spatial resolution full-field magnetic transmission soft x-ray spectro-microscopy

    SciTech Connect

    Robertson, MacCallum J.; Agostino, Christopher J.; N'Diaye, Alpha T.; Chen, Gong; Im, Mi-Young; Fischer, Peter

    2015-05-07

    The spectroscopic analysis of X-ray magnetic circular dichroism (XMCD), which serves as strong and element-specific magnetic contrast in full-field magnetic transmission soft x-ray microscopy, is shown to provide information on the local distribution of spin (S) and orbital (L) magnetic moments down to a spatial resolution of 25 nm limited by the x-ray optics used in the x-ray microscope. The spatially resolved L/S ratio observed in a multilayered (Co 0.3 nm/Pt 0.5 nm) × 30 thin film exhibiting a strong perpendicular magnetic anisotropy decreases significantly in the vicinity of domain walls, indicating a non-uniform spin configuration in the vertical profile of a domain wall across the thin film. Quantitative XMCD mapping with x-ray spectro-microscopy will become an important characterization tool for systems with topological or engineered magnetization inhomogeneities.

  15. Shock-reflected electrons and X-ray line spectra

    NASA Astrophysics Data System (ADS)

    Dzifčáková, E.; Vandas, M.; Karlický, M.

    2017-07-01

    Aims: The aim of this paper is to try to explain the physical origin of the non-thermal electron distribution that is able to form the enhanced intensities of satellite lines in the X-ray line spectra observed during the impulsive phases of some solar flares. Methods: Synthetic X-ray line spectra of the distributions composed of the distribution of shock reflected electrons and the background Maxwellian distribution are calculated in the approximation of non-Maxwellian ionization, recombination, excitation and de-excitation rates. The distribution of shock reflected electrons is determined analytically. Results: We found that the distribution of electrons reflected at the nearly-perpendicular shock resembles, at its high-energy part, the so called n-distribution. Therefore it could be able to explain the enhanced intensities of Si xiid satellite lines. However, in the region immediately in front of the shock its effect is small because electrons in background Maxwellian plasma are much more numerous there. Therefore, we propose a model in which the shock reflected electrons propagate to regions with smaller densities and different temperatures. Combining the distribution of the shock-reflected electrons with the Maxwellian distribution having different densities and temperatures we found that spectra with enhanced intensities of the satellite lines are formed at low densities and temperatures of the background plasma when the combined distribution is very similar to the n-distribution also in its low-energy part. In these cases, the distribution of the shock-reflected electrons controls the intensity ratio of the allowed Si xiii and Si xiv lines to the Si xiid satellite lines. The high electron densities of the background plasma reduce the effect of shock-reflected electrons on the composed electron distribution function, which leads to the Maxwellian spectra.

  16. Imaging of lateral spin valves with soft x-ray microscopy

    SciTech Connect

    Mosendz, O.; Mihajlovic, G.; Pearson, J. E.; Fischer, P.; Im, M.-Y.; Bader, S. D.; Hoffmann, A.

    2009-05-01

    We investigated Co/Cu lateral spin valves by means of high-resolution transmission soft x-ray microscopy with magnetic contrast that utilizes x-ray magnetic circular dichroism (XMCD). No magnetic XMCD contrast was observed at the Cu L{sub 3} absorption edge, which should directly image the spin accumulation in Cu. Although electrical transport measurements in a non-local geometry clearly detected the spin accumulation in Cu, which remained unchanged during illumination with circular polarized x-rays at the Co and Cu L{sub 3} absorption edges.

  17. Compact laser produced plasma soft x-ray source for contact microscopy experiments

    NASA Astrophysics Data System (ADS)

    Ayele, Mesfin G.; Czwartos, Joanna; Adjei, Daniel; Wachulak, Przemysław; Bartnik, Andrzej; Wegrzynski, Łukasz; Szczurek, Mirosław; Jarocki, Roman; Fiedorowicz, Henryk

    2015-05-01

    The detail characteristics of a compact laser-plasma X-ray source, dedicated for application in soft X-ray contact microscopy is presented in the paper. The source is based on a double-stream gas puff target, irradiated with nanosecond laser pulses from a commercial Nd:YAG laser. The use of the gas puff target makes possible to produce soft X-ray radiation in the "water window" region without target debris production. Details of the characterization measurements and optimization of the source are presented and discussed.

  18. X-ray holographic microscopy experiments at the Brookhaven synchrotron light source

    SciTech Connect

    Howells, M.R.; Iarocci, M.; Kenney, J.; Kirz, J.; Rarback, H.

    1983-01-01

    Soft x-ray holographic microscopy is discussed from an experimental point of view. Three series of measurements have been carried out using the Brookhaven 750 MeV storage ring as an x-ray source. Young slits fringes, Gabor (in line) holograms and various data pertaining to the soft x-ray performance of photographic plates are reported. The measurements are discussed in terms of the technique for recording them and the experimental limitations in effect. Some discussion is also given of the issues involved in reconstruction using visible light.

  19. Differential phase contrast in scanning x-ray microscopy with half-wavelength phase shifter

    SciTech Connect

    Suzuki, Yoshio Takeuchi, Akihisa

    2016-01-28

    A method for differential-phase-contrast imaging in scanning x-ray microscopy is proposed. The microfocus beam is produced with an x-ray focusing optics, and a half of the optical aperture is masked with a λ/2 phase shifter. This generates a pair of focused beam at the focal plane, with π phase difference. Combining with a diaphragm in front of the transmission beam detector, differential phase contrast (contrast proportional to the phase-difference between two foci) can be obtained. Preliminary results with a Fresnel zone plate focusing optics at 12.4 keV x-ray energy are shown.

  20. Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy

    PubMed Central

    Nho, Hyun Woo; Kalegowda, Yogesh; Shin, Hyun-Joon; Yoon, Tae Hyun

    2016-01-01

    For the structural characterization of the polystyrene (PS)-based photonic crystals (PCs), fast and direct imaging capabilities of full field transmission X-ray microscopy (TXM) were demonstrated at soft X-ray energy. PS-based PCs were prepared on an O2-plasma treated Si3N4 window and their local structures and defects were investigated using this label-free TXM technique with an image acquisition speed of ~10 sec/frame and marginal radiation damage. Micro-domains of face-centered cubic (FCC (111)) and hexagonal close-packed (HCP (0001)) structures were dominantly found in PS-based PCs, while point and line defects, FCC (100), and 12-fold symmetry structures were also identified as minor components. Additionally, in situ observation capability for hydrated samples and 3D tomographic reconstruction of TXM images were also demonstrated. This soft X-ray full field TXM technique with faster image acquisition speed, in situ observation, and 3D tomography capability can be complementally used with the other X-ray microscopic techniques (i.e., scanning transmission X-ray microscopy, STXM) as well as conventional characterization methods (e.g., electron microscopic and optical/fluorescence microscopic techniques) for clearer structure identification of self-assembled PCs and better understanding of the relationship between their structures and resultant optical properties. PMID:27087141

  1. Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Nho, Hyun Woo; Kalegowda, Yogesh; Shin, Hyun-Joon; Yoon, Tae Hyun

    2016-04-01

    For the structural characterization of the polystyrene (PS)-based photonic crystals (PCs), fast and direct imaging capabilities of full field transmission X-ray microscopy (TXM) were demonstrated at soft X-ray energy. PS-based PCs were prepared on an O2-plasma treated Si3N4 window and their local structures and defects were investigated using this label-free TXM technique with an image acquisition speed of ~10 sec/frame and marginal radiation damage. Micro-domains of face-centered cubic (FCC (111)) and hexagonal close-packed (HCP (0001)) structures were dominantly found in PS-based PCs, while point and line defects, FCC (100), and 12-fold symmetry structures were also identified as minor components. Additionally, in situ observation capability for hydrated samples and 3D tomographic reconstruction of TXM images were also demonstrated. This soft X-ray full field TXM technique with faster image acquisition speed, in situ observation, and 3D tomography capability can be complementally used with the other X-ray microscopic techniques (i.e., scanning transmission X-ray microscopy, STXM) as well as conventional characterization methods (e.g., electron microscopic and optical/fluorescence microscopic techniques) for clearer structure identification of self-assembled PCs and better understanding of the relationship between their structures and resultant optical properties.

  2. Three-dimensional readout of flash x-ray images of living sperm in water by atomic-force microscopy.

    PubMed

    Tomie, T; Shimizu, H; Majima, T; Yamada, M; Kanayama, T; Kondo, H; Yano, M; Ono, M

    1991-05-03

    The imaging of living specimens in water by x-ray microscopy can be greatly enhanced with the use of an intense flash x-ray source and sophisticated technologies for reading x-ray images. A subnanosecond [corrected] x-ray pulse from a laser-produced plasma was used to record the x-ray image of living sea urchin sperm in an x-ray resist. The resist relief was visualized at high resolution by atomic-force microscopy. Internal structure of the sperm head was evident, and the carbon density in a flagellum was estimated from the relief height.

  3. Ultrasensitive Scanning Transmission X-ray Microscopy: Pushing the Limits of Time Resolution and Magnetic Sensitivity

    NASA Astrophysics Data System (ADS)

    Ohldag, Hendrik

    Understanding magnetic properties at ultrafast timescales is crucial for the development of new magnetic devices. Samples of interest are often thin film magnetic multilayers with thicknesses in the range of a few atomic layers. This fact alone presents a sensitivity challenge in STXM microscopy, which is more suited toward studying thicker samples. In addition the relevant time scale is of the order of 10 ps, which is well below the typical x-ray pulse length of 50 - 100 ps. The SSRL STXM is equipped with a single photon counting electronics that effectively allows using a double lock-in detection at 476MHz (the x-ray pulse frequency) and 1.28MHz (the synchrotron revelation frequency) to provide the required sensitivity. In the first year of operation the excellent spatial resolution, temporal stability and sensitivity of the detection electronics of this microscope has enabled researchers to acquire time resolved images of standing as well as traveling spin waves in a spin torque oscillator in real space as well as detect the real time spin accumulation in non magnetic Copper once a spin polarized current is injected into this material. The total magnetic moment is comparable to that of a single nanocube of magnetic Fe buried under a micron of non-magnetic material.

  4. Ptychography: Pushing the limits of X-ray microscopy

    SciTech Connect

    Fromm, Cayla

    2015-08-23

    Ptychography is an advanced diffraction based imaging technique that can achieve resolution of 5 nm, and below. It is done by scanning a sample through a beam of focused x-rays using discrete yet overlapping scan steps. Scattering data is collected on a CCD camera, and the phase of the scattered light is reconstructed with sophisticated iterative algorithms. Because the experimental setup is similar, ptychography setups can be created by retrofitting existing STXM beam lines with new hardware. The other challenge comes in the reconstruction of the collected scattering images. Scattering data must be adjusted and packaged with experimental parameters to calibrate the reconstruction software. The necessary pre-processing of data prior to reconstruction is unique to each beamline setup, and even the optical alignments used on that particular day. Pre-processing software must be developed to be flexible and efficient in order to allow experimenters appropriate control and freedom in the analysis of their hard-won data. This paper will describe the implementation of pre-processing software which successfully connects data collection steps to reconstruction steps, letting the user accomplish accurate and reliable ptychography.

  5. Electro-deposition of Cu studied with in situ electrochemical scanning transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Hitchcock, A. P.; Qin, Z.; Rosendahl, S. M.; Lee, V.; Reynolds, M.; Hosseinkhannazer, H.

    2016-01-01

    Soft X-ray scanning transmission X-ray microscopy (STXM) was used to investigate Cu deposition onto, and stripping from a Au surface. Cu 2p spectromicroscopy was used to analyze initial and final states (ex situ processing) and follow the processes in situ. The in situ experiments were carried out using a static electrochemical cell with an electrolyte layer thickness of ˜1 μm. A new apparatus for in situ electrochemical STXM is described.

  6. Scanning transmission x-ray microscopy: A new ``looking glass`` into coal chemical structure

    SciTech Connect

    Botto, R.E.; Cody, G.D.

    1994-02-01

    This paper reports the use of scanning transmission x-ray microscopy to spatially map the chemistry of aromatic and aliphatic carbon functionalities in coal to a resolution of less than 0.1 {mu}m. Localized x-ray absorption spectroscopy recorded at the carbon K absorption edge was also used to facilitate analysis of variations in fundamental chemistry at maceral interfaces and within maceral boundaries.

  7. Visible/IR light and x-rays in femtosecond synchronism from an x-ray free-electron laser

    NASA Astrophysics Data System (ADS)

    Adams, B. W.

    2005-08-01

    A way is proposed to obtain pulses of visible/infrared light in femtosecond synchronism with x-rays from an x-ray free-electron laser (XFEL), using the recently proposed emittance-slicing technique. In an XFEL undulator, only the short section of an electron bunch whose emittance is left unchanged by the slicing will emit intense coherent x-rays in the XFEL undulator. At the same time, the bunch emits highly collimated transition undulator radiation (TUR) into a cone whose opening angle is the reciprocal relativisticity parameter gamma. Due to the variation of the transverse momentum induced by the emittance slicing, the effective number of charges contributing to the TUR varies along the bunch, and is higher in the sliced-out part that emits the coherent x-rays. As with coherent synchrotron radiation (CSR), the TUR is thus coherently enhanced (CTUR) at near-infrared wavelengths. Coming from the same part of the bunch the CTUR and the coherent x-rays are perfectly synchronized to each other. Because both types of radiation are generated in the long straight XFEL undulator, there are no dispersion effects that might induce a timing jitter. With typical XFEL parameters, the energy content of the single optical cycle of near-IR CTUR light is about 100 Nano-Joule, which is quite sufficient for most pump-probe experiments.

  8. 3D X-ray ultra-microscopy of bone tissue.

    PubMed

    Langer, M; Peyrin, F

    2016-02-01

    We review the current X-ray techniques with 3D imaging capability at the nano-scale: transmission X-ray microscopy, ptychography and in-line phase nano-tomography. We further review the different ultra-structural features that have so far been resolved: the lacuno-canalicular network, collagen orientation, nano-scale mineralization and their use as basis for mechanical simulations. X-ray computed tomography at the micro-metric scale is increasingly considered as the reference technique in imaging of bone micro-structure. The trend has been to push towards increasingly higher resolution. Due to the difficulty of realizing optics in the hard X-ray regime, the magnification has mainly been due to the use of visible light optics and indirect detection of the X-rays, which limits the attainable resolution with respect to the wavelength of the visible light used in detection. Recent developments in X-ray optics and instrumentation have allowed to implement several types of methods that achieve imaging that is limited in resolution by the X-ray wavelength, thus enabling computed tomography at the nano-scale. We review here the X-ray techniques with 3D imaging capability at the nano-scale: transmission X-ray microscopy, ptychography and in-line phase nano-tomography. Further, we review the different ultra-structural features that have so far been resolved and the applications that have been reported: imaging of the lacuno-canalicular network, direct analysis of collagen orientation, analysis of mineralization on the nano-scale and use of 3D images at the nano-scale to drive mechanical simulations. Finally, we discuss the issue of going beyond qualitative description to quantification of ultra-structural features.

  9. X-ray microscopy of plant cells by using LiF crystal as a detector.

    PubMed

    Reale, Lucia; Bonfigli, Francesca; Lai, Antonia; Flora, Francesco; Poma, Anna; Albertano, Patrizia; Bellezza, Simona; Montereali, Rosa Maria; Faenov, Anatoly; Pikuz, Tania; Almaviva, Salvatore; Vincenti, Maria Aurora; Francucci, Massimo; Gaudio, Pasqualino; Martellucci, Sergio; Richetta, Maria

    2008-12-01

    A lithium fluoride (LiF) crystal has been utilized as a new soft X-ray detector to image different biological samples at a high spatial resolution. This new type of image detector for X-ray microscopy has many interesting properties: high resolution (nanometer scale), permanent storage of images, the ability to clear the image and reuse the LiF crystal, and high contrast with greater dynamic range. Cells of the unicellular green algae Chlamydomonas dysosmos and Chlorella sorokiniana, and pollen grains of Olea europea have been used as biological materials for imaging. The biological samples were imaged on LiF crystals by using the soft X-ray contact microscopy and contact micro-radiography techniques. The laser plasma soft X-ray source was generated using a Nd:YAG/Glass laser focused on a solid target. The X-ray energy range for image acquisition was in the water-window spectral range for single shot contact microscopy of very thin biological samples (single cells) and around 1 keV for multishots microradiography. The main aim of this article is to highlight the possibility of using a LiF crystal as a detector for the biological imaging using soft X-ray radiation and to demonstrate its ability to visualize the microstructure within living cells. 2008 Wiley-Liss, Inc.

  10. In situ X-ray Microscopy Studies of Electromigration in Copper Interconnects

    NASA Astrophysics Data System (ADS)

    Schneider, G.; Meyer, M.-A.; Zschech, E.; Denbeaux, G.; Neuhäusler, U.; Guttmann, P.

    2003-09-01

    Real-time X-ray microscopy is applied for degradation studies to understand electromigration-induced transport processes in on-chip copper interconnects. The material transport in inlaid Cu line/via structures is observed with about 40 nm lateral resolution. The image sequences show void formation, migration and nucleation processes. Correlation of the real-time X-ray images with post-mortem SEM micrographs is used to discuss degradation mechanisms in inlaid copper interconnects. Due to the high penetration power of X-rays through matter and its high spatial resolution, X-ray microscopy (XRM) overcomes several limitations of conventional microscopic techniques. It utilizes the natural absorption contrast between the structures of interest, i.e. for on-chip copper interconnects embedded in dielectrics. Due to their different X-ray absorption characteristics at 0.52 keV, even different silicon compounds like Si, SiO2, and Si3N4 can be distinguished in X-ray images of thinned layers as demonstrated. For failure analysis of thicker layers, phase contrast microscopy in the multi-keV photon energy range is proposed.

  11. Scanning electron microscope/energy dispersive x ray analysis of impact residues in LDEF tray clamps

    NASA Technical Reports Server (NTRS)

    Bernhard, Ronald P.; Durin, Christian; Zolensky, Michael E.

    1993-01-01

    Detailed optical scanning of tray clamps is being conducted in the Facility for the Optical Inspection of Large Surfaces at JSC to locate and document impacts as small as 40 microns in diameter. Residues from selected impacts are then being characterized by Scanning Electron Microscopy/Energy Dispersive X-ray Analysis at CNES. Results from this analysis will be the initial step to classifying projectile residues into specific sources.

  12. Conservation of Moroccan manuscript papers aged 150, 200 and 800 years. Analysis by infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD), and scanning electron microscopy energy dispersive spectrometry (SEM-EDS)

    NASA Astrophysics Data System (ADS)

    Hajji, Latifa; Boukir, Abdellatif; Assouik, Jamal; Lakhiari, Hamid; Kerbal, Abdelali; Doumenq, Pierre; Mille, Gilbert; De Carvalho, Maria Luisa

    2015-02-01

    The preservation of manuscripts and archive materials is a serious problem for librarians and restorers. Paper manuscript is subjected to numerous degradation factors affecting their conservation state. This research represents an attempt to evaluate the conservation restoration process applied in Moroccan libraries, especially the alkaline treatment for strengthening weakened paper. In this study, we focused on six samples of degraded and restored paper taken from three different Moroccan manuscripts aged 150, 200 and 800 years. In addition, the Japanese paper used in restoration has been characterized. A modern paper was also analyzed as reference. A three-step analytical methodology based on infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD) and scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS) analysis was developed before and after restoration in order to determine the effect of the consolidation treatment on the paper structure. The results obtained by XRD and ATR-FTIR disclosed the presence of barium sulfate (BaSO4) in all restored paper manuscripts. The presence of calcium carbonate (CaCO3) in all considered samples was confirmed by FTIR spectroscopy. The application of de-acidification treatment causes significant changes connected with the increase of intensity mostly in the region 1426 cm-1, assigned to the asymmetric and symmetric Csbnd O stretching mode of calcite, indicating the effectiveness of de-acidification procedure proved by the rise of the alkaline reserve content allowing the long term preservation of paper. Observations performed by SEM magnify the typical paper morphology and the structure of fibbers, highlighting the effect of the restoration process, manifested by the reduction of impurities.

  13. The lack of age-pigments and the alterations in intracellular monovalent electrolytes in spontaneously hypertensive, stroke-prone (SHRsp) rats as revealed by electron microscopy and X-ray microanalysis

    SciTech Connect

    Zs.-Nagy, I.; Zs.-Nagy, V.; Casoli, T.; Lustyik, G. )

    1989-01-01

    Male, spontaneously hypertensive, stroke-prone (SHRsp) rats established by Okamoto et al. were studied. About 80% of the males of this strain have a particularly short life span (33-41 weeks); they display a considerable hypertension (above 220 mmHg) and a tendency for plurifocal brain strokes. Hypertension and strokes can be provoked in an accelerated and synchronized fashion by supplementing 1% NaCl into their drinking water. Symptoms of the appearance of brain strokes can be judged from characteristic signs of motor disorders, and can be established also by pathohistology. Since hypertension and arteriosclerosis are frequently involved in aging, the question we intended to answer was whether these animals may represent a model of the normal aging process or not. Two approaches are described: (1) Accumulation of lipofuscin granules in their brain, liver and myocardium was followed by transmission electron microscopy before and after the appearance of strokes. It has been established that these tissues do not show any typical accumulation of lipofuscin granules, although submicroscopic signs of an enhanced damage of cell organelles (especially of mitochondria in liver and brain cells, but not in myocardium) were encountered. (2) The intracellular monovalent composition in the brain and liver was measured by using bulk-specimen X-ray microanalysis. The intracellular Na-content (mEq/kg water) was significantly higher (170-200%) in both the brain and liver cells, whereas the K-content increased only moderately (118-130%). The results suggest that although the SHRsp rats do not represent a direct model for the normal aging process from the point of view of lipofuscin accumulation, the shifts of the monovalent electrolyte contents in the brain and liver cells observed already in the youngest ages, are similar to those observed in aged normal rats.

  14. Elemental composition of strawberry plants inoculated with the plant growth-promoting bacterium Azospirillum brasilense REC3, assessed with scanning electron microscopy and energy dispersive X-ray analysis.

    PubMed

    Guerrero-Molina, M F; Lovaisa, N C; Salazar, S M; Díaz-Ricci, J C; Pedraza, R O

    2014-07-01

    The elemental composition of strawberry plants (Fragaria ananassa cv. Macarena) inoculated with the plant growth-promoting bacterium Azospirillum brasilense REC3, and non-inoculated controls, was studied using scanning electron microscopy (SEM) and energy dispersive X-ray (EDS) analysis. This allowed simultaneous semi-quantification of different elements in a small, solid sample. Plants were inoculated and grown hydroponically in 50% or 100% Hoagland solution, corresponding to limited or optimum nutrient medium, respectively. Bacteria-inoculated plants increased the growth index 45% and 80% compared to controls when grown in 100% and 50% Hoagland solution, respectively. Thus, inoculation with A. brasilense REC3 in a nutrient-limited medium had the strongest effect in terms of increasing both shoot and root biomass and growth index, as already described for Azospirillum inoculated into nutrient-poor soils. SEM-EDS spectra and maps showed the elemental composition and relative distribution of nutrients in strawberry tissues. Leaves contained C, O, N, Na, P, K, Ca and Cu, while roots also had Si and Cl. The organic fraction (C, O and N) accounted for over 96.3% of the total chemical composition; of the mineral fraction, Na had higher accumulation in both leaves and roots. Azospirillum-inoculated and control plants had similar elemental quantities; however, in bacteria-inoculated roots, P was significantly increased (34.33%), which constitutes a major benefit for plant nutrition, while Cu content decreased (35.16%). © 2013 German Botanical Society and The Royal Botanical Society of the Netherlands.

  15. Microstructural investigation of plastically deformed Ti{sub 20}Zr{sub 20}Hf{sub 20}Nb{sub 20}Ta{sub 20} high entropy alloy by X-ray diffraction and transmission electron microscopy

    SciTech Connect

    Dirras, G.; Gubicza, J.; Heczel, A.; Lilensten, L.; Couzinié, J.-P.; Perrière, L.; Guillot, I.; Hocini, A.

    2015-10-15

    The microstructure evolution in body-centered cubic (bcc) Ti{sub 20}Zr{sub 20}Hf{sub 20}Nb{sub 20}Ta{sub 20} high entropy alloy during quasi-static compression test was studied by X-ray line profile analysis (XLPA) and transmission electron microscopy (TEM). The average lattice constant and other important parameters of the microstructure such as the mean crystallite size, the dislocation density and the edge/screw character of dislocations were determined by XLPA. The elastic anisotropy factor required for XLPA procedure was determined by nanoindentation. XLPA shows that the crystallite size decreased while the dislocation density increased with strain during compression, and their values reached about 39 nm and 15 × 10{sup 14} m{sup −2}, respectively, at a plastic strain of ~ 20%. It was revealed that with increasing strain the dislocation character became more screw. This can be explained by the reduced mobility of screw dislocations compared to edge dislocations in bcc structures. These observations are in line with TEM investigations. The development of dislocation density during compression was related to the yield strength evolution. - Highlights: • Ti{sub 20}Zr{sub 20}Hf{sub 20}Nb{sub 20}Ta{sub 20} high entropy alloy was processed by arc-melting. • The mechanical was evaluated by RT compression test. • The microstructure evolution was studied by XLPA and TEM. • With increasing strain the dislocation character became more screw. • The yield strength was related to the development of the dislocation density.

  16. Conservation of Moroccan manuscript papers aged 150, 200 and 800 years. Analysis by infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD), and scanning electron microscopy energy dispersive spectrometry (SEM-EDS).

    PubMed

    Hajji, Latifa; Boukir, Abdellatif; Assouik, Jamal; Lakhiari, Hamid; Kerbal, Abdelali; Doumenq, Pierre; Mille, Gilbert; De Carvalho, Maria Luisa

    2015-02-05

    The preservation of manuscripts and archive materials is a serious problem for librarians and restorers. Paper manuscript is subjected to numerous degradation factors affecting their conservation state. This research represents an attempt to evaluate the conservation restoration process applied in Moroccan libraries, especially the alkaline treatment for strengthening weakened paper. In this study, we focused on six samples of degraded and restored paper taken from three different Moroccan manuscripts aged 150, 200 and 800 years. In addition, the Japanese paper used in restoration has been characterized. A modern paper was also analyzed as reference. A three-step analytical methodology based on infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD) and scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS) analysis was developed before and after restoration in order to determine the effect of the consolidation treatment on the paper structure. The results obtained by XRD and ATR-FTIR disclosed the presence of barium sulfate (BaSO4) in all restored paper manuscripts. The presence of calcium carbonate (CaCO3) in all considered samples was confirmed by FTIR spectroscopy. The application of de-acidification treatment causes significant changes connected with the increase of intensity mostly in the region 1426 cm(-1), assigned to the asymmetric and symmetric CO stretching mode of calcite, indicating the effectiveness of de-acidification procedure proved by the rise of the alkaline reserve content allowing the long term preservation of paper. Observations performed by SEM magnify the typical paper morphology and the structure of fibbers, highlighting the effect of the restoration process, manifested by the reduction of impurities. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. European X-Ray Free Electron Laser (EXFEL): local implications

    NASA Astrophysics Data System (ADS)

    Romaniuk, Ryszard S.

    2013-10-01

    European X-Ray FEL - free electron laser is under construction in DESY Hamburg. It is scheduled to be operational at 2015/16 at a cost more than 1 billion Euro. The laser uses SASE method to generate x-ray light. It is propelled by an electron linac of 17,5GeV energy and more than 2km in length. The linac uses superconducting SRF TESLA technology working at 1,3 GHz in frequency. The prototype of EXFEL is FLASH Laser (200 m in length), where the "proof of principle" was checked, and from the technologies were transferred to the bigger machine. The project was stared in the nineties by building a TTF Laboratory -Tesla Test Facility. The EXFEL laser is a child of a much bigger teraelectronovolt collider project TESLA (now abandoned in Germany but undertaken by international community in a form the ILC). A number of experts and young researchers from Poland participate in the design, construction and research of the FLASH and EXFEL lasers.

  18. Bent diamond-crystal x-ray spectrographs for x-ray free-electron laser noninvasive diagnostics

    NASA Astrophysics Data System (ADS)

    Terentyev, Sergey; Blank, Vladimir; Kolodziej, Tomasz; Shvyd'ko, Yuri

    2016-09-01

    We report on the manufacturing and X-ray tests of bent diamond-crystal X-ray spectrographs, designed for noninvasive diagnostics of the X-ray free-electron laser (XFEL) spectra in the spectral range from 5 to 15 keV. The key component is a curved, 20-μm thin, single crystalline diamond triangular plate in the (110) orientation. The radius of curvature can be varied between R = 0:6 m and R = 0:1 m in a controlled fashion, ensuring imaging in a spectral window of up to 60 eV for 8 keV X-rays. All of the components of the bending mechanism (about 10 parts) are manufactured from diamond, thus ensuring safe operations in intense XFEL beams. The spectrograph is transparent to 88% for 5-keV photons, and to 98% for 15-keV photons. Therefore, it can be used for noninvasive diagnostics of the X-ray spectra during XFEL operations.

  19. Food Irradiation Using Electron Beams and X-Rays

    NASA Astrophysics Data System (ADS)

    Miller, Bruce

    2003-04-01

    In this presentation we will discuss the technology of food irradiation using electron accelerators. Food irradiation has generally come to describe the use of ionizing radiation to decrease the population of, or prevent the growth of, undesirable biological organisms in food. The many beneficial applications include insect disinfestation, sprouting inhibition, delayed ripening, and the enhanced safety and sterilization of fresh and frozen meat products, seafood, and eggs. With special regard to food safety, bacteria such as Salmonella enteridis, Listeria monocytogenes, Campylobacter jejuni and Escherichia coli serotype O157:H7 are the primary causes of food poisoning in industrialized countries. Ionizing doses in the range of only 1-5 kilogray (kGy) can virtually eliminate these organisms from food, without affecting the food's sensory and nutritional qualities, and without inducing radioactivity. The key elements of an accelerator-based irradiation facility include the accelerator system, a scanning system, and a material handling system that moves the product through the beam in a precisely controlled manner. Extensive radiation shielding is necessary to reduce the external dose to acceptable levels, and a safety system is necessary to prevent accidental exposure of personnel during accelerator operation. Parameters that affect the dose distribution must be continuously monitored and controlled with process control software. The choice of electron beam vs x-ray depends on the areal density (density times thickness) of the product and the anticipated mass throughput. To eliminate nuclear activation concerns, the maximum kinetic energy of the accelerator is limited by regulation to 10 MeV for electron beams, and 5 MeV for x-rays. From penetration considerations, the largest areal density that can be treated by double-sided electron irradiation at 10 MeV is about 8.8 g/cm2. Products having greater areal densities must be processed using more penetrating x-rays. The

  20. Magnetic x-ray microscopy at low temperatures – Visualization of flux distributions in superconductors

    SciTech Connect

    Stahl, Claudia Ruoß, Stephen; Weigand, Markus; Bechtel, Michael; Schütz, Gisela; Albrecht, Joachim

    2016-01-28

    X-ray Magnetic Circular Dichroism (XMCD) microscopy at liquid nitrogen temperature has been performed on bilayers of high-T{sub c} superconducting YBCO (YBa{sub 2}Cu{sub 3}O{sub 7-δ}) and soft-magnetic Co{sub 40}Fe{sub 40}B{sub 20}. This should allow us to map the magnetic flux density distribution in the current-carrying state of the superconductor with high spatial resolution. For that purpose the UHV scanning X-ray microscope MAXYMUS has been upgraded by a MMR Micro Miniature Joule-Thompson cryostat capable of temperatures between 75 K and 580 K. Resulting XMCD images of the magnetic flux density in the superconductor with a field of view ranging from millimeters to micrometers are presented. The microscope’s unique combination of total electron yield (TEY) measurements together with low temperatures offers novel possibilities concerning the current transport in superconductors on small length scales.

  1. Calibration Of A KrF Laser-Plasma Source For X-Ray Microscopy Applications

    NASA Astrophysics Data System (ADS)

    Turcu, I. C. E.; O'Neill, F.; Zammit, U.; Al-Hadithi, Y.; Eason, R. W.; Rogayski, A. M.; Hills, C. P. B.; Michette, A. G.

    1988-02-01

    Plasma X-ray sources for biological microscopy in the water-window have been produced by focusing tige 200 3, 50 ns Sprit q KrF laser onto carbon targets at irradiance between 2.2 x 10" W/cm4 and 3.7 x 10i3W/cm. Absolute measurements of X-ray production have been made using a calibrated, vacuum X-ray diode detector. A peak conversion efficiency . 10% is measured from KrF laseri)Tight tcto wate-window X-rays at 280 eV < hv < 530 eV for a target irradiance . 1 x x 10 W/cm'. Some measurements with gold and tungsten targets give conversion efficiencies 2$25% at a similar laser irradiance.

  2. Synchrotron X-ray microscopy and spectroscopy analysis of iron in hemochromatosis liver and intestines

    SciTech Connect

    Ko, J .Y. Peter; Sham, Tsun-Kong; Chakrabarti, Subrata; Adams, Paul C.

    2009-12-01

    Hemochromatosis is a genetic disorder that causes body to store excess iron in organs such as heart or liver. Distribution of iron, as well as copper, zinc and calcium, and chemical identity of iron in hemochromatosis liver and intestine were investigated by X-ray microprobe experiments, which consist of X-ray microscopy and micro-X-ray absorption fine structure. Our results show that iron concentration in hemochromatosis liver tissue is high, while much less Fe is found in intestinal tissue. Moreover, chemical identity of Fe in hemochromatosis liver can be identified. X-ray microprobe experiments allows for examining elemental distribution at an excellent spatial resolution. Moreover, chemical identity of element of interest can be obtained.

  3. Synchrotron X-ray microscopy and spectroscopy analysis of iron in hemochromatosis liver and intestines

    NASA Astrophysics Data System (ADS)

    Ko, J. Y. Peter; Sham, Tsun-Kong; Chakrabarti, Subrata; Adams, Paul C.

    2009-11-01

    Hemochromatosis is a genetic disorder that causes body to store excess iron in organs such as heart or liver. Distribution of iron, as well as copper, zinc and calcium, and chemical identity of iron in hemochromatosis liver and intestine were investigated by X-ray microprobe experiments, which consist of X-ray microscopy and micro-X-ray absorption fine structure. Our results show that iron concentration in hemochromatosis liver tissue is high, while much less Fe is found in intestinal tissue. Moreover, chemical identity of Fe in hemochromatosis liver can be identified. X-ray microprobe experiments allows for examining elemental distribution at an excellent spatial resolution. Moreover, chemical identity of element of interest can be obtained.

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

    PubMed

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

    2017-11-01

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

  5. Measurement of the unstained biological sample by a novel scanning electron generation X-ray microscope based on SEM.

    PubMed

    Ogura, Toshihiko

    2009-08-07

    We introduced a novel X-ray microscope system based on scanning electron microscopy using thin film, which enables the measurement of unstained biological samples without damage. An unstained yeast sample was adsorbed under a titanium (Ti)-coated silicon nitride (Si3N4) film 90 nm thick. The X-ray signal from the film was detected by an X-ray photodiode (PD) placed below the sample. With an electron beam at 2.6 kV acceleration and 6.75 nA current, the yeast image is obtained using the X-ray PD. The image is created by soft X-rays from the Ti layer. The Ti layer is effective in generating the characteristic 2.7-nm wavelength X-rays by the irradiation of electrons. Furthermore, we investigated the electron trajectory and the generation of the characteristic X-rays within the Ti-coated Si3N4 film by Monte Carlo simulation. Our system can be easily utilized to observe various unstained biological samples of cells, bacteria, and viruses.

  6. ELECTRON MICROSCOPE AND X-RAY DIFFRACTION STUDIES ON A HOMOLOGOUS SERIES OF SATURATED PHOSPHATIDYLCHOLINES.

    PubMed

    ELBERS, P F; VERVERGAERT, P H

    1965-05-01

    Three homologous saturated phosphatidylcholines were studied by electron microscopy after tricomplex fixation. The results are compared with those obtained by x-ray diffraction analysis of the same and some other homologous compounds, in the dry crystalline state and after tricomplex fixation. By electron microscopy alternating dark and light bands are observed which are likely to correspond to phosphatide double layers. X-Ray diffraction reveals the presence of lamellar structures of regular spacing. The layer spacings obtained by both methods are in good agreement. From the electron micrographs the width of the polar parts of the double layers can be derived directly. The width of the carboxylglycerylphosphorylcholine moiety of the layers is found by extrapolating the x-ray diffraction data to zero chain length of the fatty acids. When from this width the contribution of the carboxylglyceryl part of the molecules is subtracted, again we find good agreement with the electron microscope measurements. An attempt has been made to account for the different layer spacings measured in terms of orientation of the molecules within the double layers.

  7. Electron Microscopy.

    ERIC Educational Resources Information Center

    Beer, Michael

    1980-01-01

    Reviews technical aspects of structure determination in biological electron microscopy (EM). Discusses low dose EM, low temperature microscopy, electron energy loss spectra, determination of mass or molecular weight, and EM of labeled systems. Cites 34 references. (CS)

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

    SciTech Connect

    Mascali, David Castro, Giuseppe; Celona, Luigi; Neri, Lorenzo; Gammino, Santo; Biri, Sándor; Rácz, Richárd; Pálinkás, József; Romano, Francesco Paolo; Torrisi, Giuseppe

    2016-02-15

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

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

    NASA Astrophysics Data System (ADS)

    Mascali, David; Castro, Giuseppe; Biri, Sándor; Rácz, Richárd; Pálinkás, József; Caliri, Claudia; Celona, Luigi; Neri, Lorenzo; Romano, Francesco Paolo; Torrisi, Giuseppe; Gammino, Santo

    2016-02-01

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

  10. Reflection of attosecond x-ray free electron laser pulses

    SciTech Connect

    Hau-Riege, S; Chapman, H

    2006-10-30

    In order to utilize hard x-ray free electron lasers (XFEL's) when they are extended to attosecond pulse lengths, it is necessary to choose optical elements with minimal response time. Specular grazing incidence optics made of low-Z materials are popular candidates for reflectors since they are likely to withstand x-ray damage and provide sufficiently large reflectivities. Using linear-optics reflection theory, we calculated the transient reflectivity of a delta-function electric pulse from a homogeneous semi-infinite medium as a function of angle of incidence for s- and p-polarized light. We specifically considered the pulse response of Be, diamond, silicon carbide, and silicon, all of which are of relevance to the XFEL's that are currently being built. We found that the media emit energy in a damped oscillatory way, and that the impulse-response times are shorter than 0.3 fs for normal incidence. For grazing incidence, the impulse-response time is substantially shorter, making grazing-incidence mirrors a good choice for deep-sub-femtosecond reflective optics.

  11. Reflection of attosecond x-ray free electron laser pulses

    SciTech Connect

    Hau-Riege, Stefan P.; Chapman, Henry N.

    2007-01-15

    In order to utilize hard x-ray free electron lasers (XFEL's) when they are extended to attosecond pulse lengths, it is necessary to choose optical elements with minimal response time. Specular grazing-incidence optics made of low-Z materials are popular candidates for reflectors since they are likely to withstand x-ray damage and provide sufficiently large reflectivities. Using linear-optics reflection theory, we calculated the transient reflectivity of a delta-function electric pulse from a homogenous semi-infinite medium as a function of angle of incidence for s- and p-polarized light. We specifically considered the pulse response of beryllium, diamond, silicon carbide, and silicon, all of which are of relevance to the XFEL's that are currently being built. We found that the media emit energy in a damped oscillatory way, and that the impulse-response times are shorter than 0.3 fs for normal incidence. For grazing incidence, the impulse-response time is substantially shorter, making grazing-incidence mirrors a good choice for deep subfemtosecond reflective optics.

  12. WHOLE CELL TOMOGRAPHY/MOLECULAR BIOLOGY/STRUCTURAL BIOLOGY: Affordable x-ray microscopy with nanoscale resolution

    SciTech Connect

    Evans, James E.; Blackborow, Paul; Horne, Stephen J.; Gelb, Jeff

    2013-03-01

    Biological research spans 10 orders of magnitude from angstroms to meters. While electron microscopy can reveal structural details at most of these spatial length scales, transmission electron tomography only reliably reconstructs three-dimensional (3-D) volumes of cellular material with a spatial resolution between 1-5 nm from samples less than 500 nm thick1. Most biological cells are 2-30 times thicker than this threshold, which means that a cell must be cut into consecutive slices with each slice reconstructed individually in order to approximate the contextual information of the entire cell. Fortunately, due to a larger penetration depth2, X-ray computed tomography bypasses the need to physically section a cell and enables imaging of intact cells and tissues on the micrometer or larger scale with tens to hundreds of nanometer spatial resolution. While the technique of soft x-ray microscopy has been extensively developed in synchrotron facilities, advancements in laboratory x-ray source designs now increase its accessibility by supporting commercial systems suitable for a standard laboratory. In this paper, we highlight a new commercial compact cryogenic soft x-ray microscope designed for a standard laboratory setting and explore its capabilities for mesoscopic investigations of intact prokaryotic and eukaryotic cells.

  13. Miniature, low-power X-ray tube using a microchannel electron generator electron source

    NASA Technical Reports Server (NTRS)

    Elam, Wm. Timothy (Inventor); Kelliher, Warren C. (Inventor); Hershyn, William (Inventor); DeLong, David P. (Inventor)

    2011-01-01

    Embodiments of the invention provide a novel, low-power X-ray tube and X-ray generating system. Embodiments of the invention use a multichannel electron generator as the electron source, thereby increasing reliability and decreasing power consumption of the X-ray tube. Unlike tubes using a conventional filament that must be heated by a current power source, embodiments of the invention require only a voltage power source, use very little current, and have no cooling requirements. The microchannel electron generator comprises one or more microchannel plates (MCPs), Each MCP comprises a honeycomb assembly of a plurality of annular components, which may be stacked to increase electron intensity. The multichannel electron generator used enables directional control of electron flow. In addition, the multichannel electron generator used is more robust than conventional filaments, making the resulting X-ray tube very shock and vibration resistant.

  14. Ultrafast Science Opportunities with Electron Microscopy

    SciTech Connect

    Durr, Hermann

    2016-04-28

    X-rays and electrons are two of the most fundamental probes of matter. When the Linac Coherent Light Source (LCLS), the world’s first x-ray free electron laser, began operation in 2009, it transformed ultrafast science with the ability to generate laser-like x-ray pulses from the manipulation of relativistic electron beams. This document describes a similar future transformation. In Transmission Electron Microscopy, ultrafast relativistic (MeV energy) electron pulses can achieve unsurpassed spatial and temporal resolution. Ultrafast temporal resolution will be the next frontier in electron microscopy and can ideally complement ultrafast x-ray science done with free electron lasers. This document describes the Grand Challenge science opportunities in chemistry, material science, physics and biology that arise from an MeV ultrafast electron diffraction & microscopy facility, especially when coupled with linac-based intense THz and X-ray pump capabilities.

  15. A tunable optical cavity for an x-ray free-electron laser oscillator.

    SciTech Connect

    Kim, K.-J.; Shvyd'ko, Y.

    2009-03-01

    An x-ray free-electron laser oscillator proposed recently for hard x rays [K. Kim, Y. Shvydko, and S. Reiche, Phys. Rev. Lett. 100, 244802 (2008)] can be made tunable by using an x-ray cavity composed of four crystals, instead of two. The tunability of x-ray energy will significantly enhance the usefulness of an x-ray free-electron laser oscillator. We present a detailed analysis of the four-crystal optical cavity and choice of crystals for several applications: inelastic x-ray scattering, nuclear resonant scattering, bulk-sensitive hard x-ray photoemission spectroscopy, other high-energy-resolution ({le} 1 meV) spectroscopic probes, and for imaging with hard x rays at near-atomic resolution ({approx} 1 nm).

  16. X-ray Phase Imaging Microscopy using a Fresnel Zone Plate and a Transmission Grating

    SciTech Connect

    Yashiro, Wataru; Momose, Atsushi; Takeuchi, Akihisa; Suzuki, Yoshio

    2010-06-23

    We report on a hard X-ray phase imaging microscopy (a phase-difference microscopy) that consists of an objective and a transmission grating. The simple optical system provides a quantitative phase image, and does not need a wave field mostly coherent on the objective. Our method has a spatial resolution almost same as that of the absorption contrast microscope image obtained by removing the grating. We demonstrate how our approach provides a phase image from experimentally obtained images. Our approach is attractive for easily appending a quantitative phase-sensitive mode to normal X-ray microscopes, and has potentially broad applications in biology and material sciences.

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

    SciTech Connect

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

    2016-09-19

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

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

    DOE PAGES

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

    2016-09-19

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

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

    PubMed Central

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

    2016-01-01

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

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

    PubMed

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

    2016-10-03

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

  1. Proposal for an x-ray free electron laser oscillator with intermediate energy electron beam.

    PubMed

    Dai, Jinhua; Deng, Haixiao; Dai, Zhimin

    2012-01-20

    Harmonic lasing of low-gain free electron laser oscillators has been experimentally demonstrated in the terahertz and infrared regions. Recently, the low-gain oscillator has been reconsidered as a promising candidate for hard x-ray free electron lasers, through the use of high reflectivity, high-resolution x-ray crystals. In this Letter, it is proposed to utilize a crystal-based cavity resonant at a higher harmonic of the undulator radiation, together with phase shifting, to enable harmonic lasing of the x-ray free electron laser oscillator, and hence allow the generation of hard x-ray radiation at a reduced electron beam energy. Results show that fully coherent free electron laser radiation with megawatt peak power, in the spectral region of 10-25 keV, can be generated with a 3.5 GeV electron beam.

  2. Diffraction data of core-shell nanoparticles from an X-ray free electron laser

    DOE PAGES

    Li, Xuanxuan; Chiu, Chun -Ya; Wang, Hsiang -Ju; ...

    2017-04-11

    X-ray free-electron lasers provide novel opportunities to conduct single particle analysis on nanoscale particles. Coherent diffractive imaging experiments were performed at the Linac Coherent Light Source (LCLS), SLAC National Laboratory, exposing single inorganic core-shell nanoparticles to femtosecond hard-X-ray pulses. Each facetted nanoparticle consisted of a crystalline gold core and a differently shaped palladium shell. Scattered intensities were observed up to about 7 nm resolution. Analysis of the scattering patterns revealed the size distribution of the samples, which is consistent with that obtained from direct real-space imaging by electron microscopy. Furthermore, scattering patterns resulting from single particles were selected and compiledmore » into a dataset which can be valuable for algorithm developments in single particle scattering research.« less

  3. Diffraction data of core-shell nanoparticles from an X-ray free electron laser

    NASA Astrophysics Data System (ADS)

    Li, Xuanxuan; Chiu, Chun-Ya; Wang, Hsiang-Ju; Kassemeyer, Stephan; Botha, Sabine; Shoeman, Robert L.; Lawrence, Robert M.; Kupitz, Christopher; Kirian, Richard; James, Daniel; Wang, Dingjie; Nelson, Garrett; Messerschmidt, Marc; Boutet, Sébastien; Williams, Garth J.; Hartmann, Elisabeth; Jafarpour, Aliakbar; Foucar, Lutz M.; Barty, Anton; Chapman, Henry; Liang, Mengning; Menzel, Andreas; Wang, Fenglin; Basu, Shibom; Fromme, Raimund; Doak, R. Bruce; Fromme, Petra; Weierstall, Uwe; Huang, Michael H.; Spence, John C. H.; Schlichting, Ilme; Hogue, Brenda G.; Liu, Haiguang

    2017-04-01

    X-ray free-electron lasers provide novel opportunities to conduct single particle analysis on nanoscale particles. Coherent diffractive imaging experiments were performed at the Linac Coherent Light Source (LCLS), SLAC National Laboratory, exposing single inorganic core-shell nanoparticles to femtosecond hard-X-ray pulses. Each facetted nanoparticle consisted of a crystalline gold core and a differently shaped palladium shell. Scattered intensities were observed up to about 7 nm resolution. Analysis of the scattering patterns revealed the size distribution of the samples, which is consistent with that obtained from direct real-space imaging by electron microscopy. Scattering patterns resulting from single particles were selected and compiled into a dataset which can be valuable for algorithm developments in single particle scattering research.

  4. Diffraction data of core-shell nanoparticles from an X-ray free electron laser.

    PubMed

    Li, Xuanxuan; Chiu, Chun-Ya; Wang, Hsiang-Ju; Kassemeyer, Stephan; Botha, Sabine; Shoeman, Robert L; Lawrence, Robert M; Kupitz, Christopher; Kirian, Richard; James, Daniel; Wang, Dingjie; Nelson, Garrett; Messerschmidt, Marc; Boutet, Sébastien; Williams, Garth J; Hartmann, Elisabeth; Jafarpour, Aliakbar; Foucar, Lutz M; Barty, Anton; Chapman, Henry; Liang, Mengning; Menzel, Andreas; Wang, Fenglin; Basu, Shibom; Fromme, Raimund; Doak, R Bruce; Fromme, Petra; Weierstall, Uwe; Huang, Michael H; Spence, John C H; Schlichting, Ilme; Hogue, Brenda G; Liu, Haiguang

    2017-04-11

    X-ray free-electron lasers provide novel opportunities to conduct single particle analysis on nanoscale particles. Coherent diffractive imaging experiments were performed at the Linac Coherent Light Source (LCLS), SLAC National Laboratory, exposing single inorganic core-shell nanoparticles to femtosecond hard-X-ray pulses. Each facetted nanoparticle consisted of a crystalline gold core and a differently shaped palladium shell. Scattered intensities were observed up to about 7 nm resolution. Analysis of the scattering patterns revealed the size distribution of the samples, which is consistent with that obtained from direct real-space imaging by electron microscopy. Scattering patterns resulting from single particles were selected and compiled into a dataset which can be valuable for algorithm developments in single particle scattering research.

  5. Compact soft x-ray transmission microscopy with sub-50 nm spatial resolution.

    PubMed

    Kim, Kyong Woo; Kwon, Youngman; Nam, Ki-Yong; Lim, Jong-Hyeok; Kim, Kyu-Gyum; Chon, Kwon Su; Kim, Byoung Hoon; Kim, Dong Eon; Kim, JinGon; Ahn, Byoung Nam; Shin, Hyun Joon; Rah, Seungyu; Kim, Ki-Ho; Chae, Jin Seok; Gweon, Dae Gab; Kang, Dong Woo; Kang, Sung Hoon; Min, Jin Young; Choi, Kyu-Sil; Yoon, Seong Eon; Kim, Eun-A; Namba, Yoshiharu; Yoon, Kwon-Ha

    2006-03-21

    In this paper, the development of compact transmission soft x-ray microscopy (XM) with sub-50 nm spatial resolution for biomedical applications is described. The compact transmission soft x-ray microscope operates at lambda = 2.88 nm (430 eV) and is based on a tabletop regenerative x-ray source in combination with a tandem ellipsoidal condenser mirror for sample illumination, an objective micro zone plate and a thinned back-illuminated charge coupled device to record an x-ray image. The new, compact x-ray microscope system requires the fabrication of proper x-ray optical devices in order to obtain high-quality images. For an application-oriented microscope, the alignment procedure is fully automated via computer control through a graphic user interface. In imaging studies using our compact XM system, a gold mesh image was obtained with 45 nm resolution at x580 magnification and 1 min exposure. Images of a biological sample (Coscinodiscus oculoides) were recorded.

  6. X-Ray Free Electron Laser Interaction With Matter

    SciTech Connect

    Hau-Riege, S

    2009-05-12

    X-ray free electron lasers (XFELs) will enable studying new areas of laser-matter interaction. We summarize the current understanding of the interaction of XFEL pulses with matter and describe some of the simulation approaches that are used to design experiments on future XFEL sources. Modified versions of these models have been successful in guiding and analyzing experiments performed at the extreme-ultraviolet FEL FLASH at wavelengths of 6 nm and longer. For photon energies of several keV, no XFEL-matter interaction experiments have been performed yet but data is anticipated to become available in the near future, which will allow to test our understanding of the interaction physics in this wavelength regime.

  7. Focusing mirror for x-ray free-electron lasers

    SciTech Connect

    Mimura, Hidekazu; Kimura, Takashi; Yamakawa, Daisuke; Matsuyama, Satoshi; Morita, Shinya; Uehara, Yoshihiro; Ohmori, Hitoshi; Lin, Weimin; Yumoto, Hirokatsu; Ohashi, Haruhiko

    2008-08-15

    We present the design, fabrication, and evaluation of a large total-reflection mirror for focusing x-ray free-electron laser beams to nanometer dimensions. We used an elliptical focusing mirror made of silicon that was 400 mm long and had a focal length of 550 mm. Electrolytic in-process dressing grinding was used for initial-step figuring and elastic emission machining was employed for final figuring and surface smoothing. A figure accuracy with a peak-to-valley height of 2 nm was achieved across the entire area. Characterization of the focused beam was performed at BL29XUL of SPring-8. The focused beam size was 75 nm at 15 keV, which is almost equal to the theoretical size.

  8. Electron Beam Pattern Writer For X-Ray Masks

    NASA Astrophysics Data System (ADS)

    Viswanathan, R.; Wilson, A. D.; Lafuente, J.; Voelker, H.; Kern, A.

    1984-03-01

    This paper discusses the capabilities of a vector scan electron-beam system as an X-ray mask writer for pattern geometries at and below one-half micron. The noise level in the deflection system has been reduced to an RMS value of 150 A over a 0.5 mm deflection field, thus making our exposure system usable in the one-quarter micron regime. Pattern geometries below 2000 A have been fabricated on a thin membrane. Drift compensation techniques, implemented in software, have reduced placement errors over the entire mask to less than 700 A. Accomplishments in the areas of noise reduction, bandwidth error compensation, system resolution, and improvements in pattern placement accuracy are discussed.

  9. Imaging nanoscale lattice variations by machine learning of x-ray diffraction microscopy data.

    PubMed

    Laanait, Nouamane; Zhang, Zhan; Schlepütz, Christian M

    2016-09-16

    We present a novel methodology based on machine learning to extract lattice variations in crystalline materials, at the nanoscale, from an x-ray Bragg diffraction-based imaging technique. By employing a full-field microscopy setup, we capture real space images of materials, with imaging contrast determined solely by the x-ray diffracted signal. The data sets that emanate from this imaging technique are a hybrid of real space information (image spatial support) and reciprocal lattice space information (image contrast), and are intrinsically multidimensional (5D). By a judicious application of established unsupervised machine learning techniques and multivariate analysis to this multidimensional data cube, we show how to extract features that can be ascribed physical interpretations in terms of common structural distortions, such as lattice tilts and dislocation arrays. We demonstrate this 'big data' approach to x-ray diffraction microscopy by identifying structural defects present in an epitaxial ferroelectric thin-film of lead zirconate titanate.

  10. Imaging nanoscale lattice variations by machine learning of x-ray diffraction microscopy data

    NASA Astrophysics Data System (ADS)

    Laanait, Nouamane; Zhang, Zhan; Schlepütz, Christian M.

    2016-09-01

    We present a novel methodology based on machine learning to extract lattice variations in crystalline materials, at the nanoscale, from an x-ray Bragg diffraction-based imaging technique. By employing a full-field microscopy setup, we capture real space images of materials, with imaging contrast determined solely by the x-ray diffracted signal. The data sets that emanate from this imaging technique are a hybrid of real space information (image spatial support) and reciprocal lattice space information (image contrast), and are intrinsically multidimensional (5D). By a judicious application of established unsupervised machine learning techniques and multivariate analysis to this multidimensional data cube, we show how to extract features that can be ascribed physical interpretations in terms of common structural distortions, such as lattice tilts and dislocation arrays. We demonstrate this ‘big data’ approach to x-ray diffraction microscopy by identifying structural defects present in an epitaxial ferroelectric thin-film of lead zirconate titanate.

  11. Scanning Transmission X-ray Microscopy: Applications in Atmospheric Aerosol Research

    SciTech Connect

    Moffet, Ryan C.; Tivanski, Alexei V.; Gilles, Mary K.

    2011-01-20

    Scanning transmission x-ray microscopy (STXM) combines x-ray microscopy and near edge x-ray absorption fine structure spectroscopy (NEXAFS). This combination provides spatially resolved bonding and oxidation state information. While there are reviews relevant to STXM/NEXAFS applications in other environmental fields (and magnetic materials) this chapter focuses on atmospheric aerosols. It provides an introduction to this technique in a manner approachable to non-experts. It begins with relevant background information on synchrotron radiation sources and a description of NEXAFS spectroscopy. The bulk of the chapter provides a survey of STXM/NEXAFS aerosol studies and is organized according to the type of aerosol investigated. The purpose is to illustrate the current range and recent growth of scientific investigations employing STXM-NEXAFS to probe atmospheric aerosol morphology, surface coatings, mixing states, and atmospheric processing.

  12. Exfoliated nanoplatelets of an Aurivillius phase, Bi{sub 3.25}La{sub 0.75}Ti{sub 3}O{sub 12}: Characterisation by X-ray diffraction and by high-resolution electron microscopy

    SciTech Connect

    Chevallier, Virginie Nihoul, Genevieve Madigou, Veronique

    2008-03-15

    Nanoparticles of the Aurivillius phase La-substituted BTO (Bi{sub 4-x}La{sub x}Ti{sub 3}O{sub 12}, with x=0.75) were obtained through a chemical lithiation process. They have been characterised by X-ray diffraction and transmission electron microscopy (diffraction and imaging at high resolution). The defect-free particles are platelet-shaped with the c large axis perpendicular to the plane. From high-resolution images, it is clear that the delamination process occurs at the level of the (Bi{sub 2}O{sub 2}){sup 2+} intermediate layer and is destructive for this layer. The smallest thickness measured corresponds to one cell parameter (3.3 nm) but a large range of thicknesses have been observed: this suggests that the lithium insertion does not take place in all (Bi{sub 2}O{sub 2}){sup 2+} layers, despite a large excess of lithium and a long reaction time. This is confirmed by ICP analysis, which leads to a formula Li{sub 0.99}Bi{sub 3.25}La{sub 0.77}Ti{sub 3.00}O{sub 12} for the lithiated compound. This behaviour towards lithium intercalation differs from those observed with BTO in literature, where lithium insertion is reported as occurring in every (Bi{sub 2}O{sub 2}){sup 2+} layer. Possible explanations for this difference are advanced based on microstructural and structural considerations. - Graphical abstract: Bi{sub 3.25}La{sub 0.75}Ti{sub 3}O{sub 12} nanoplatelets, of which the thickness downs to one cell parameter along the c-axis, are obtained through a soft chemical lithiation process followed by exfoliation. Li{sup +} cations intercalate in the intermediate (Bi{sub 2}O{sub 2}){sup 2+} layers. However, not all of them actually accommodate lithium. Moreover, exfoliation is destructive for the host layers.

  13. Environmental scanning electron microscopy connected with energy dispersive x-ray analysis and Raman techniques to study ProRoot mineral trioxide aggregate and calcium silicate cements in wet conditions and in real time.

    PubMed

    Gandolfi, Maria Giovanna; Van Landuyt, Kirsten; Taddei, Paola; Modena, Enrico; Van Meerbeek, Bart; Prati, Carlo

    2010-05-01

    ProRoot mineral trioxide aggregate (MTA) and calcium silicate cements are able to set in a moist environment. The aim of the study was to examine the surface structure and composition of a cement paste under wet conditions and in real time during setting by environmental scanning electron microscopy connected with energy dispersive x-ray analysis (ESEM-EDX) and micro-Raman techniques. White ProRoot MTA and experimental white tetrasilicate cement (wTC) and wTC containing bismuth oxide (wTC-Bi) were studied. Cement disks were analyzed 10 minutes after powder-liquid mixing (freshly prepared samples) and after immersion in Dulbecco phosphate-buffered saline at 37 degrees C for 24 hours (24-hour-aged samples). Freshly prepared wet cements at ESEM-EDX exposed an irregular surface (displaying calcium, silicon, aluminum, chlorine reflexes, and bismuth traces in MTA and wTC-Bi) with needle-like and cubic-hexagonal shaped crystals. Aggregates of spheroidal Ca-P-rich crystals (spherulites) appeared on the surface of 24-hour-aged samples. The starting unhydrated powders displayed the typical Raman bands of Portland cement components: alite, belite, and calcium sulfate (only as anhydrite in MTA and as both anhydrite and gypsum in wTC and wTC-Bi). MTA powder showed higher amount of calcium carbonate and lower quantities of anhydrite and higher crystallinity of the silicate component, leading to a slower hydration reaction. Products/markers of hydration reactions were present on fresh samples; ettringite formed on the surface of all the cements; calcium hydroxide (portlandite) was detected only on the surface of wTC, but no conclusion can be drawn on wTC-Bi and MTA because of the interference of bismuth oxide. Calcium phosphate and calcite/aragonite bands were detected on all 24-hour-aged cements; portlandite was no longer detected on wTC. ESEM and micro-Raman are powerful and suitable techniques to investigate endodontic calcium silicate hydrated cements in real time and in

  14. Molecular beam epitaxial growth mechanism of ZnSe epilayers on (100) GaAs as determined by reflection high-energy electron diffraction, transmission electron microscopy and X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Landwehr, G.; Wagg, A.; Heinke, H.; Behr, T.; Hommel, D.; Ruppert, P.

    1994-04-01

    The properties of the molecular beam epitaxial ZnSe epilayers deposited directly on a GaAs substrate are compared to those grown on a GaAs buffer layer. The superior quality of the latter is confirmed by RHEED, TEM and X-ray diffraction. Based on RHEED oscillation studies, a model explaining the dependence of the ZnSe growth rate on Zn and Se fluxes and the substrate temperature is developed taking into account physi- and chemisorbed states. For partially relaxed epilayers, the correlation between the relaxation state and the crystalline mosaicity, as found by high resolution X-ray diffraction, is discussed.

  15. High-resolution diffraction microscopy using the plane-wave field of a nearly diffraction limited focused x-ray beam

    SciTech Connect

    Takahashi, Yukio; Nishino, Yoshinori; Ishikawa, Tetsuya; Tsutsumi, Ryosuke; Kubo, Hideto; Furukawa, Hayato; Mimura, Hidekazu; Matsuyama, Satoshi; Zettsu, Nobuyuki; Matsubara, Eiichiro; Yamauchi, Kazuto

    2009-08-01

    X-ray waves in the center of the beam waist of nearly diffraction limited focused x-ray beams can be considered to have amplitude and phase that are both almost uniform, i.e., they are x-ray plane waves. Here we report the results of an experimental demonstration of high-resolution diffraction microscopy using the x-ray plane wave of the synchrotron x-ray beam focused using Kirkpatrik-Baez mirrors. A silver nanocube with an edge length of {approx}100 nm is illuminated with the x-ray beam focused to a {approx}1 {mu}m spot at 12 keV. A high-contrast symmetric diffraction pattern of the nanocube is observed in the forward far field. An image of the nanocube is successfully reconstructed by an iterative phasing method and its half-period resolution is 3.0 nm. This method does not only dramatically improve the spatial resolution of x-ray microscopy but also is a key technology for realizing single-pulse diffractive imaging using x-ray free-electron lasers.

  16. Flash X-Ray (FXR) Accelerator Optimization Electronic Time-Resolved Measurement of X-Ray Source Size

    SciTech Connect

    Jacob, J; Ong, M; Wargo, P

    2005-07-21

    Lawrence Livermore National Laboratory (LLNL) is currently investigating various approaches to minimize the x-ray source size on the Flash X-Ray (FXR) linear induction accelerator in order to improve x-ray flux and increase resolution for hydrodynamic radiography experiments. In order to effectively gauge improvements to final x-ray source size, a fast, robust, and accurate system for measuring the spot size is required. Timely feedback on x-ray source size allows new and improved accelerator tunes to be deployed and optimized within the limited run-time constraints of a production facility with a busy experimental schedule; in addition, time-resolved measurement capability allows the investigation of not only the time-averaged source size, but also the evolution of the source size, centroid position, and x-ray dose throughout the 70 ns beam pulse. Combined with time-resolved measurements of electron beam parameters such as emittance, energy, and current, key limiting factors can be identified, modeled, and optimized for the best possible spot size. Roll-bar techniques are a widely used method for x-ray source size measurement, and have been the method of choice at FXR for many years. A thick bar of tungsten or other dense metal with a sharp edge is inserted into the path of the x-ray beam so as to heavily attenuate the lower half of the beam, resulting in a half-light, half-dark image as seen downstream of the roll-bar; by measuring the width of the transition from light to dark across the edge of the roll-bar, the source size can be deduced. For many years, film has been the imaging medium of choice for roll-bar measurements thanks to its high resolution, linear response, and excellent contrast ratio. Film measurements, however, are fairly cumbersome and require considerable setup and analysis time; moreover, with the continuing trend towards all-electronic measurement systems, film is becoming increasingly difficult and expensive to procure. Here, we shall

  17. Hard X-ray-induced damage on carbon-binder matrix for in situ synchrotron transmission X-ray microscopy tomography of Li-ion batteries.

    PubMed

    Lim, Cheolwoong; Kang, Huixiao; De Andrade, Vincent; De Carlo, Francesco; Zhu, Likun

    2017-05-01

    The electrode of Li-ion batteries is required to be chemically and mechanically stable in the electrolyte environment for in situ monitoring by transmission X-ray microscopy (TXM). Evidence has shown that continuous irradiation has an impact on the microstructure and the electrochemical performance of the electrode. To identify the root cause of the radiation damage, a wire-shaped electrode is soaked in an electrolyte in a quartz capillary and monitored using TXM under hard X-ray illumination. The results show that expansion of the carbon-binder matrix by the accumulated X-ray dose is the key factor of radiation damage. For in situ TXM tomography, intermittent X-ray exposure during image capturing can be used to avoid the morphology change caused by radiation damage on the carbon-binder matrix.

  18. High numerical aperture tabletop soft x-ray diffraction microscopy with 70-nm resolution

    PubMed Central

    Sandberg, Richard L.; Song, Changyong; Wachulak, Przemyslaw W.; Raymondson, Daisy A.; Paul, Ariel; Amirbekian, Bagrat; Lee, Edwin; Sakdinawat, Anne E.; La-O-Vorakiat, Chan; Marconi, Mario C.; Menoni, Carmen S.; Murnane, Margaret M.; Rocca, Jorge J.; Kapteyn, Henry C.; Miao, Jianwei

    2008-01-01

    Light microscopy has greatly advanced our understanding of nature. The achievable resolution, however, is limited by optical wavelengths to ≈200 nm. By using imaging and labeling technologies, resolutions beyond the diffraction limit can be achieved for specialized specimens with techniques such as near-field scanning optical microscopy, stimulated emission depletion microscopy, and photoactivated localization microscopy. Here, we report a versatile soft x-ray diffraction microscope with 70- to 90-nm resolution by using two different tabletop coherent soft x-ray sources—a soft x-ray laser and a high-harmonic source. We also use field curvature correction that allows high numerical aperture imaging and near-diffraction-limited resolution of 1.5λ. A tabletop soft x-ray diffraction microscope should find broad applications in biology, nanoscience, and materials science because of its simple optical design, high resolution, large depth of field, 3D imaging capability, scalability to shorter wavelengths, and ultrafast temporal resolution. PMID:18162534

  19. A hybrid x-ray and microscopy method for diametrical profile measurement of internal holes in steel components

    NASA Astrophysics Data System (ADS)

    Liu, T.; Malcolm, A. A.; Yin, X. M.; Liew, S. J.; Prawiradiraja, T. P.

    2008-09-01

    High-resolution X-ray is now an essential tool for internal defect and structure inspection in electronics and advanced materials industry. However, it is always a challenge to use it for accurate dimensional measurement due to the nature of the fan-beam X-ray source, particularly for cylindrical objects. This paper presents a novel hybrid X-ray and microscopy method for the profile measurement of the internal hole of a cylinder-shaped steel component. The part to be measured has a beer bottle shape but is open at the bottom side. The objective is to measure the diametrical profile of the internal hole with an accuracy of about 10μm. Traditionally this is measured with using a microscope after cutting and polishing the specimen. This is not only a tedious work, but is also inaccurate due to the uncertainty in cutting and polishing. This report demonstrates that the two edge-profiles of the internal hole can be obtained with X-ray inspection by sequentially placing each of them at the central of the X-ray beam so that the fan-beam effect can be minimized. The resolution of the X-ray inspection is about 6µm under a 20x magnification. Subsequently, the diameter of the hole is measured at two positions through the open end using a microscope with a 20x and a 10x objectives respectively. The results obtained with the two methods are then combined to generate the whole diametrical profile of the internal hole.

  20. Image restoration applied to x-ray microscopy: application to images with low signal-to-noise ratio

    NASA Astrophysics Data System (ADS)

    Sibarita, Jean-Baptiste; Chassery, Jean-Marc; Robert-Nicoud, Michel

    1995-02-01

    X-ray microscopy makes it possible to obtain images at a higher spatial resolution (about 20 nm) as compared to optical microscopy. Moreover, x-ray microscopy permits direct acquisition from the specimen in 2D or 3D mode, without any preparation step (staining, fixation, ...), which is not possible in electron microscopy. Here we present deblurring methods to restore images after the acquisition process. An additive Poisson noise is generated by the use of x rays and also contributes to image degradation. Our purpose is to analyze such noise and to restore images. Due to the optical properties of the Fresnel zone plate, we presently associate it to an optical circular lens as is done for the optical microscope. Here we use the Richardson Lucy algorithm to deconvolute. A first step is to observe results of restoration obtained on an image grating (a star pattern) with inner zones of dimensions near the resolution. The next step involves the suppression of noise effects arising from the deconvolution process. The characteristics of the noise after deconvolution are evaluated by Fourier analysis. These effects are eliminated by a filtering process in the Fourier spectrum. This filtering is applied on images with different signal to noise ratio (obtained after different time exposures), in order to compare results obtained on noisy images with long time exposure images.

  1. Electron Paramagnetic Resonance studies of x-ray irradiated Nafion

    NASA Astrophysics Data System (ADS)

    Fragoso, Juan; Usher, Timothy

    2007-03-01

    Fuel cells promise a bright future as power sources for a variety of electronic equipment as well as more power demanding elements. Nafion (DuPont's trademark of a sulfonated tetrafluorethylene polymer modified from Teflon) is the heart of Proton Exchange Membrane Fuel Cells (PEMFCs) as well as Direct Methanol Fuel Cells (DMFCs). Fuel cells are used to power electronic equipment on spacecraft, satellites and unpiloted high altitude aircraft, where ionizing radiation can be a concern. Electron Paramagnetic Resonance (EPR) is a spectroscopic technique that is very sensitive to free radicals such as those produced by ionizing radiation therefore EPR can give us a window into the degradation of the Nafion membranes due to the ionizing radiation. Nafion samples were irradiated using a x-ray diffractometer with a copper target operating at 40kV and 55mA for at least 3hrs. X-Band EPR spectroscopy of the irradiated nafion reveals a peak at 3400G with a width of 10G, which decays over time, completely diminishing in a couple of weeks. Preliminary results from the polarization studies on the effects of ionizing radiation will also be presented.

  2. Phase contrast: the frontier of x-ray and electron imaging

    NASA Astrophysics Data System (ADS)

    Hwu, Y.; Margaritondo, G.

    2013-12-01

    Phase contrast has been a fundamental component of microscopy since the early 1940s. In broad terms, it refers to the formation of images using not the combination of wave intensities but their amplitudes with the corresponding phase factors. The impact on visible microscopy of biological specimens has been major. This contrast mechanism is now playing an increasingly important role in other kinds of microscopy, notably those based on electrons or x-rays. It notably solves the background problem of weak absorption contrast. New breakthroughs and new techniques are continuously produced, unfortunately unknown to most of the scientists that could exploit them. The present special cluster issue of reviews was inspired by this situation. The case of x-rays is very interesting. Phase contrast requires a high degree of longitudinal and lateral coherence. But conventional x-ray sources are not coherent. The progress of synchrotron sources yielded high coherence as a key byproduct—and started a rapid expansion of phase contrast radiology. No review—or cluster of reviews—can possibly cover all the facets of the recent progress. Without trying to be absolutely comprehensive, the present special cluster issue touches a variety of issues, giving a very broad picture. Liu et al review in general terms the different phase-based hard-x-ray techniques, with an interesting variety of examples. Then, Suortti et al and Wang et al present more specialized overviews of crystal and grating based x-ray imaging techniques, very powerful in the analysis of biological specimens. Mokso et al discuss the many facets of tomography using phase effects, expanding the picture of tomographic reconstruction of the three previous reviews. Wu et al treat the rapid progress in hard-x-ray focusing and its impact on radiology and tomography for materials science and biomedical research. The next two reviews deal with special and very interesting classes of applications. Specifically, Lee et al

  3. Phase contrast x-ray microscopy study of rabbit primo vessels

    NASA Astrophysics Data System (ADS)

    Kim, M.-S.; Oh, S.-W.; Lim, J.-H.; Han, S.-W.

    2010-11-01

    The microstructural properties of the primo-vascular systems of rabbits were examined by phase contrast x-ray microscopy. The primo-vascular systems with an average diameter of 32 μm were extracted from the surfaces of the rabbit internal organs. Phase contrast x-ray imaging showed that the primo-vascular systems were tubules with random holes on their lateral surfaces. The size of the holes on the vascular surface was 2-5 μm. The holes might act as size selective channels for microcells coming in and out and assist in the unidirectional flow of the primo-vascular systems.

  4. Standing-wave excited soft x-ray photoemission microscopy: application to Co microdot magnetic arrays

    SciTech Connect

    Gray, Alexander; Kronast, Florian; Papp, Christian; Yang, See-Hun; Cramm, Stefan; Krug, Ingo P.; Salmassi, Farhad; Gullikson, Eric M.; Hilken, Dawn L.; Anderson, Erik H.; Fischer, Peter; Durr, Hermann A.; Schneider, Claus M.; Fadley, Charles S.

    2010-10-29

    We demonstrate the addition of depth resolution to the usual two-dimensional images in photoelectron emission microscopy (PEEM), with application to a square array of circular magnetic Co microdots. The method is based on excitation with soft x-ray standing-waves generated by Bragg reflection from a multilayer mirror substrate. Standing wave is moved vertically through sample simply by varying the photon energy around the Bragg condition. Depth-resolved PEEM images were obtained for all of the observed elements. Photoemission intensities as functions of photon energy were compared to x-ray optical calculations in order to quantitatively derive the depth-resolved film structure of the sample.

  5. Aplanatic Three-Mirror Objective for High-Magnification Soft X-Ray Microscopy

    SciTech Connect

    Toyoda, M.; Jinno, T.; Yanagihara, M.

    2011-09-09

    An innovative solution for high-magnification microscopy, based on attaching afocal optics for focal length reduction, is proposed. The solution, consisting of three spherical mirrors, allows one to enhance a magnification of a laboratory based soft x-ray microscope over 1000x, where movies with diffraction-limited resolution can be observed with an x-ray CCD. The design example, having a numerical aperture of 0.25, was successfully demonstrated both a high magnification and a large field of view.

  6. Full-field hard x-ray microscopy below 30 nm : a challenging nanofabrication achievement.

    SciTech Connect

    Chen, Y.; Lo, T.; Chu, Y.; Yi, J.; Liu, C.; Wang, J.; Wang, C.; Chiu, C.; Hua, T.; Hwu, Y.; Shen, Q.; Yin, G.; Liang, K.; Lin, H.; Je, J.; Margaritondo, G.; X-Ray Science Division; Academia Sinica; Tatung Univ.; National Tsing Hua Univ.; National Taiwan Ocean Univ.; National Synchrotron Radiation Research Center; Pohang Univ. of Science and Technology; Ecole Polytechnique Federale de Lausanne

    2008-01-01

    The fabrication of devices to focus hard x-rays is one of the most difficult--and important--challenges in nanotechnology. Here we show that Fresnel zone plates combining 30 nm external zones and a high aspect ratio finally bring hard x-ray microscopy beyond the 30 nm Rayleigh spatial resolution level and measurable spatial frequencies down to 20-23 nm feature size. After presenting the overall nanofabrication process and the characterization test results, we discuss the potential research impact of these resolution levels.

  7. Application of X-ray microscopy in food science investigation of high pressure affected bacterial spores

    NASA Astrophysics Data System (ADS)

    Mönch, Susanne; Heinz, Volker; Guttmann, Peter; Knorr, Dietrich

    2000-05-01

    Using the Göttingen transmission X-ray microscope at BESSY the effect of different pressure and temperature levels during the high hydrostatic pressure (HP) treatment was investigated. At 150 MPa and temperatures up to 50 °C the triggering of germination was observed by standard microbiological methods with Bacillus subtilis spores. Increasing the temperature to 70 °C at the same pressure level killed the spores without any indication of germination. By X-ray microscopy images it could be shown that the typical disintegration of the protoplast is inhibited. This suggests that the enzymic reaction pathway is possibly affected under specific pressure temperature conditions.

  8. Demonstration of 12 nm resolution Fresnel zone plate lens based soft x-ray microscopy

    SciTech Connect

    Chao, W.; Kim, J.; Rekawa, S.; Fischer, P.; Anderson, E. H.

    2009-06-05

    To extend soft x-ray microscopy to a resolution of order 10 nm or better, we developed a new nanofabrication process for Fresnel zone plate lenses. The new process, based on the double patterning technique, has enabled us to fabricate high quality gold zone plates with 12 nm outer zones. Testing of the zone plate with the full-field transmission x-ray microscope, XM-1, in Berkeley, showed that the lens clearly resolved 12 nm lines and spaces. This result represents a significant step towards 10 nm resolution and beyond.

  9. Coherent X-Ray Diffraction Imaging of Chloroplasts from Cyanidioschyzon merolae by Using X-Ray Free Electron Laser.

    PubMed

    Takayama, Yuki; Inui, Yayoi; Sekiguchi, Yuki; Kobayashi, Amane; Oroguchi, Tomotaka; Yamamoto, Masaki; Matsunaga, Sachihiro; Nakasako, Masayoshi

    2015-07-01

    Coherent X-ray diffraction imaging (CXDI) is a lens-less technique for visualizing the structures of non-crystalline particles with the dimensions of submicrometer to micrometer at a resolution of several tens of nanometers. We conducted cryogenic CXDI experiments at 66 K to visualize the internal structures of frozen-hydrated chloroplasts of Cyanidioschyzon merolae using X-ray free electron laser (XFEL) as a coherent X-ray source. Chloroplast dispersed specimen disks at a number density of 7/(10×10 µm(2)) were flash-cooled with liquid ethane without staining, sectioning or chemical labeling. Chloroplasts are destroyed at atomic level immediately after the diffraction by XFEL pulses. Thus, diffraction patterns with a good signal-to-noise ratio from single chloroplasts were selected from many diffraction patterns collected through scanning specimen disks to provide fresh specimens into the irradiation area. The electron density maps of single chloroplasts projected along the direction of the incident X-ray beam were reconstructed by using the iterative phase-retrieval method and multivariate analyses. The electron density map at a resolution of 70 nm appeared as a C-shape. In addition, the fluorescence image of proteins stained with Flamingo™ dye also appeared as a C-shape as did the autofluorescence from Chl. The similar images suggest that the thylakoid membranes with an abundance of proteins distribute along the outer membranes of chloroplasts. To confirm the present results statistically, a number of projection structures must be accumulated through high-throughput data collection in the near future. Based on the results, we discuss the feasibility of XFEL-CXDI experiments in the structural analyses of cellular organelles.

  10. Development of a hard X-ray delay line for X-ray photon correlation spectroscopy and jitter-free pump-probe experiments at X-ray free-electron laser sources.

    PubMed

    Roseker, Wojciech; Franz, Hermann; Schulte-Schrepping, Horst; Ehnes, Anita; Leupold, Olaf; Zontone, Federico; Lee, Sooheyong; Robert, Aymeric; Grübel, Gerhard

    2011-05-01

    A hard X-ray delay line capable of splitting and delaying single X-ray pulses has been developed with the aim of performing X-ray photon correlation spectroscopy (XPCS) and X-ray pump-probe experiments at hard X-ray free-electron laser sources. The performance of the device was tested with 8.39 keV synchrotron radiation. Time delays up to 2.95 ns have been demonstrated. The feasibility of the device for performing XPCS studies was tested by recording static speckle patterns. The achieved speckle contrast of 56% indicates the possibility of performing ultra-fast XPCS studies with the delay line.

  11. 3-D Cellular Ultrastructure Can Be Resolved by X-ray Microscopy | Center for Cancer Research

    Cancer.gov

    X-ray microscopy (XRM) is more rapid than cryoelectron tomography or super-resolution fluorescence microscopy and could fill an important gap in current technologies used to investigate in situ three-dimensional structure of cells. New XRM methods developed by first author Gerd Schneider, Ph.D., working with James McNally. Ph.D., and a team of colleagues, is capable of revealing full cellular ultrastructure without requiring fixation, staining, or sectioning.

  12. Stereo soft x-ray microscopy and elemental mapping of hematite and clay suspensions

    SciTech Connect

    Gleber, S.-C.; Thieme, J.; Chao, W.; Fischer, P.

    2008-09-01

    The spatial arrangements of hematite particles within aqueous soil and clay samples are investigated with soft X-ray microscopy, taking advantage of the elemental contrast at the Fe-L edge around E = 707 eV. In combination with stereo microscopy, information about spatial arrangements are revealed and correlated to electrostatic interactions of the different mixtures. Manipulation of a sample mounted to the microscope is possible and particles added while imaging can be detected.

  13. Biomedical elemental analysis and imaging using synchrotron x-ray microscopy

    SciTech Connect

    Jones, K.W.; Gordon, B.M.; Schidlovsky, G.; Spanne, P.; Dejun, Xue ); Bockman, R.S. ); Saubermann, A.J. . Health Science Center)

    1990-01-01

    The application of synchrotron x-ray microscopy to biomedical research is currently in progress at the Brookhaven National Synchrotron Light Source (NSLS). The current status of the x-ray microscope (XRM) is reviewed from a technical standpoint. Some of the items considered are photon flux, spatial resolution, quantitation, minimum detection limits, and beam-induced specimen damage. Images can be produced by measurement of fluorescent x rays or of the attenuation of the incident beam by the specimen. Maps of the elemental distributions or linear attenuation of the incident beam by the specimen. Maps of the elemental distributions or linear attenuation coefficients can be made by scanning the specimen past the beam. Computed microtomography (CMT) can be used for non- destructive images through the specimen in either the emission or absorption mode. Examples of measurements made with the XRM are given.

  14. Advancement of X-Ray Microscopy Technology and its Application to Metal Solidification Studies

    NASA Technical Reports Server (NTRS)

    Kaukler, William F.; Curreri, Peter A.

    1996-01-01

    The technique of x-ray projection microscopy is being used to view, in real time, the structures and dynamics of the solid-liquid interface during solidification. By employing a hard x-ray source with sub-micron dimensions, resolutions of 2 micrometers can be obtained with magnifications of over 800 X. Specimen growth conditions need to be optimized and the best imaging technologies applied to maintain x-ray image resolution, contrast and sensitivity. It turns out that no single imaging technology offers the best solution and traditional methods like radiographic film cannot be used due to specimen motion (solidification). In addition, a special furnace design is required to permit controlled growth conditions and still offer maximum resolution and image contrast.

  15. Signal-to-noise and radiation exposure considerations in conventional and diffraction x-ray microscopy

    DOE PAGES

    Huang, Xiaojing; Miao, Huijie; Steinbrener, Jan; ...

    2009-01-01

    Using a signal-to-noise ratio estimation based on correlations between multiple simulated images, we compare the dose efficiency of two soft x-ray imaging systems: incoherent brightfield imaging using zone plate optics in a transmission x-ray microscope (TXM), and x-ray diffraction microscopy (XDM) where an image is reconstructed from the far-field coherent diffraction pattern. In XDM one must computationally phase weak diffraction signals; in TXM one suffers signal losses due to the finite numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution imagesmore » using fewer photons. As a result, this can be an important advantage for studying radiation-sensitive biological and soft matter specimens.« less

  16. Numerical model for tomographic image formation in transmission x-ray microscopy.

    PubMed

    Bertilson, Michael; von Hofsten, Olov; Hertz, Hans M; Vogt, Ulrich

    2011-06-06

    We present a numerical image-formation model for investigating the influence of partial coherence, sample thickness and depth-of-focus on the accuracy of tomographic reconstructions in transmission x-ray microscopes. The model combines wave propagation through the object by finite difference techniques with Fourier methods. We include a ray-tracing model to analyse the origin of detrimental stray light in zone plate-based x-ray microscopes. These models allow optimization of x-ray microscopy systems for quantitative tomographic imaging of thick objects. Results show that both the depth-of-focus and the reconstructed local absorption coefficient are highly dependent on the degree of coherence of the optical system.

  17. Scanning transmission X-ray microscopy with a fast framing pixel detector.

    PubMed

    Menzel, A; Kewish, C M; Kraft, P; Henrich, B; Jefimovs, K; Vila-Comamala, J; David, C; Dierolf, M; Thibault, P; Pfeiffer, F; Bunk, O

    2010-08-01

    Scanning transmission X-ray microscopy (STXM) is a powerful imaging technique, in which a small X-ray probe is raster scanned across a specimen. Complete knowledge of the complex-valued transmission function of the specimen can be gained using detection schemes whose every-day use, however, is often hindered by the need of specialized configured detectors or by slow or noisy readout of area detectors. We report on sub-50 nm-resolution STXM studies in the hard X-ray regime using the PILATUS, a fully pixelated fast framing detector operated in single-photon counting mode. We demonstrate a range of imaging modes, including phase contrast and dark-field imaging. 2010 Elsevier B.V. All rights reserved.

  18. Simple load frame for in situ computed tomography and x-ray tomographic microscopy

    SciTech Connect

    Breunig, T.M. ); Stock, S.R.; Brown, R.C. )

    1993-05-01

    In many instances, the response of a sample to external stimuli must be observed repeatedly during the course of an experiment. The sequence in which features are formed is often critical to proper identification of the mechanisms operating, for example, in fatigue and fracture. Merely observing what is visible at the surface of the sample can be misleading or can provide inadequate information about what governs fatigue crack growth or about what controls the fracture process. X-ray imaging allows one to observe the interior of samples and is an attractive technique to use with in situ stressing of test specimens. Here, a simple compact, inexpensive load frame is described for in situ x-ray computed tomography and for very high resolution computed tomography, termed x-ray tomographic microscopy. The load frame is evaluated, and its use is illustrated by observations of crack closure as a function of load in a notched tensile sample of Al-Li-2090.

  19. Signal-to-noise and radiation exposure considerations in conventional and diffraction x-ray microscopy.

    PubMed

    Huang, Xiaojing; Miao, Huijie; Steinbrener, Jan; Nelson, Johanna; Shapiro, David; Stewart, Andrew; Turner, Joshua; Jacobsen, Chris

    2009-08-03

    Using a signal-to-noise ratio estimation based on correlations between multiple simulated images, we compare the dose efficiency of two soft x-ray imaging systems: incoherent brightfield imaging using zone plate optics in a transmission x-ray microscope (TXM), and x-ray diffraction microscopy (XDM) where an image is reconstructed from the far-field coherent diffraction pattern. In XDM one must computationally phase weak diffraction signals; in TXM one suffers signal losses due to the finite numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution images using fewer photons. This can be an important advantage for studying radiation-sensitive biological and soft matter specimens.

  20. Cryogenic x-ray diffraction microscopy utilizing high-pressure cryopreservation.

    PubMed

    Lima, Enju; Chushkin, Yuriy; van der Linden, Peter; Kim, Chae Un; Zontone, Federico; Carpentier, Philippe; Gruner, Sol M; Pernot, Petra

    2014-10-01

    We present cryo x-ray diffraction microscopy of high-pressure-cryofixed bacteria and report high-convergence imaging with multiple image reconstructions. Hydrated D. radiodurans cells were cryofixed at 200 MPa pressure into ∼10-μm-thick water layers and their unstained, hydrated cellular environments were imaged by phasing diffraction patterns, reaching sub-30-nm resolutions with hard x-rays. Comparisons were made with conventional ambient-pressure-cryofixed samples, with respect to both coherent small-angle x-ray scattering and the image reconstruction. The results show a correlation between the level of background ice signal and phasing convergence, suggesting that phasing difficulties with frozen-hydrated specimens may be caused by high-background ice scattering.

  1. 3D elemental sensitive imaging using transmission X-ray microscopy.

    PubMed

    Liu, Yijin; Meirer, Florian; Wang, Junyue; Requena, Guillermo; Williams, Phillip; Nelson, Johanna; Mehta, Apurva; Andrews, Joy C; Pianetta, Piero

    2012-09-01

    Determination of the heterogeneous distribution of metals in alloy/battery/catalyst and biological materials is critical to fully characterize and/or evaluate the functionality of the materials. Using synchrotron-based transmission x-ray microscopy (TXM), it is now feasible to perform nanoscale-resolution imaging over a wide X-ray energy range covering the absorption edges of many elements; combining elemental sensitive imaging with determination of sample morphology. We present an efficient and reliable methodology to perform 3D elemental sensitive imaging with excellent sample penetration (tens of microns) using hard X-ray TXM. A sample of an Al-Si piston alloy is used to demonstrate the capability of the proposed method.

  2. Signal-to-noise and radiation exposure considerations in conventional and diffraction x-ray microscopy

    PubMed Central

    Huang, Xiaojing; Miao, Huijie; Steinbrener, Jan; Nelson, Johanna; Shapiro, David; Stewart, Andrew; Turner, Joshua; Jacobsen, Chris

    2010-01-01

    Using a signal-to-noise ratio estimation based on correlations between multiple simulated images, we compare the dose efficiency of two soft x-ray imaging systems: incoherent brightfield imaging using zone plate optics in a transmission x-ray microscope (TXM), and x-ray diffraction microscopy (XDM) where an image is reconstructed from the far-field coherent diffraction pattern. In XDM one must computationally phase weak diffraction signals; in TXM one suffers signal losses due to the finite numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution images using fewer photons. This can be an important advantage for studying radiation-sensitive biological and soft matter specimens. PMID:19654762

  3. Signal-to-noise and radiation exposure considerations in conventional and diffraction x-ray microscopy

    SciTech Connect

    Huang, Xiaojing; Miao, Huijie; Steinbrener, Jan; Nelson, Johanna; Shapiro, David; Stewart, Andrew; Turner, Joshua; Jacobsen, Chris

    2009-01-01

    Using a signal-to-noise ratio estimation based on correlations between multiple simulated images, we compare the dose efficiency of two soft x-ray imaging systems: incoherent brightfield imaging using zone plate optics in a transmission x-ray microscope (TXM), and x-ray diffraction microscopy (XDM) where an image is reconstructed from the far-field coherent diffraction pattern. In XDM one must computationally phase weak diffraction signals; in TXM one suffers signal losses due to the finite numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution images using fewer photons. As a result, this can be an important advantage for studying radiation-sensitive biological and soft matter specimens.

  4. Fracture mechanics by three-dimensional crack-tip synchrotron X-ray microscopy

    PubMed Central

    Withers, P. J.

    2015-01-01

    To better understand the relationship between the nucleation and growth of defects and the local stresses and phase changes that cause them, we need both imaging and stress mapping. Here, we explore how this can be achieved by bringing together synchrotron X-ray diffraction and tomographic imaging. Conventionally, these are undertaken on separate synchrotron beamlines; however, instruments capable of both imaging and diffraction are beginning to emerge, such as ID15 at the European Synchrotron Radiation Facility and JEEP at the Diamond Light Source. This review explores the concept of three-dimensional crack-tip X-ray microscopy, bringing them together to probe the crack-tip behaviour under realistic environmental and loading conditions and to extract quantitative fracture mechanics information about the local crack-tip environment. X-ray diffraction provides information about the crack-tip stress field, phase transformations, plastic zone and crack-face tractions and forces. Time-lapse CT, besides providing information about the three-dimensional nature of the crack and its local growth rate, can also provide information as to the activation of extrinsic toughening mechanisms such as crack deflection, crack-tip zone shielding, crack bridging and crack closure. It is shown how crack-tip microscopy allows a quantitative measure of the crack-tip driving force via the stress intensity factor or the crack-tip opening displacement. Finally, further opportunities for synchrotron X-ray microscopy are explored. PMID:25624521

  5. Fracture mechanics by three-dimensional crack-tip synchrotron X-ray microscopy.

    PubMed

    Withers, P J

    2015-03-06

    To better understand the relationship between the nucleation and growth of defects and the local stresses and phase changes that cause them, we need both imaging and stress mapping. Here, we explore how this can be achieved by bringing together synchrotron X-ray diffraction and tomographic imaging. Conventionally, these are undertaken on separate synchrotron beamlines; however, instruments capable of both imaging and diffraction are beginning to emerge, such as ID15 at the European Synchrotron Radiation Facility and JEEP at the Diamond Light Source. This review explores the concept of three-dimensional crack-tip X-ray microscopy, bringing them together to probe the crack-tip behaviour under realistic environmental and loading conditions and to extract quantitative fracture mechanics information about the local crack-tip environment. X-ray diffraction provides information about the crack-tip stress field, phase transformations, plastic zone and crack-face tractions and forces. Time-lapse CT, besides providing information about the three-dimensional nature of the crack and its local growth rate, can also provide information as to the activation of extrinsic toughening mechanisms such as crack deflection, crack-tip zone shielding, crack bridging and crack closure. It is shown how crack-tip microscopy allows a quantitative measure of the crack-tip driving force via the stress intensity factor or the crack-tip opening displacement. Finally, further opportunities for synchrotron X-ray microscopy are explored.

  6. An improved phase shift reconstruction algorithm of fringe scanning technique for X-ray microscopy

    SciTech Connect

    Lian, S.; Yang, H.; Kudo, H.; Momose, A.; Yashiro, W.

    2015-02-15

    The X-ray phase imaging method has been applied to observe soft biological tissues, and it is possible to image the soft tissues by using the benefit of the so-called “Talbot effect” by an X-ray grating. One type of the X-ray phase imaging method was reported by combining an X-ray imaging microscope equipped by a Fresnel zone plate with a phase grating. Using the fringe scanning technique, a high-precision phase shift image could be obtained by displacing the grating step by step and measuring dozens of sample images. The number of the images was selected to reduce the error caused by the non-sinusoidal component of the Talbot self-image at the imaging plane. A larger number suppressed the error more but increased radiation exposure and required higher mechanical stability of equipment. In this paper, we analyze the approximation error of fringe scanning technique for the X-ray microscopy which uses just one grating and proposes an improved algorithm. We compute the approximation error by iteration and substitute that into the process of reconstruction of phase shift. This procedure will suppress the error even with few sample images. The results of simulation experiments show that the precision of phase shift image reconstructed by the proposed algorithm with 4 sample images is almost the same as that reconstructed by the conventional algorithm with 40 sample images. We also have succeeded in the experiment with real data.

  7. Uncertainty estimates for electron probe X-ray microanalysis measurements.

    PubMed

    Ritchie, Nicholas W M; Newbury, Dale E

    2012-11-20

    It has been over 60 years since Castaing (Castaing, R. Application of Electron Probes to Local Chemical and Crystallographic Analysis. Ph.D. Thesis, University of Paris, Paris, France, 1951; translated by P. Duwez and D. Wittry, California Institute of Technology, 1955) introduced the technique of electron probe X-ray microanalysis (EPMA), yet the community remains unable to quantify some of the largest terms in the technique's uncertainty budget. Historically, the EPMA community has assigned uncertainties to its measurements which reflect the measurement precision portion of the uncertainty budget and omitted terms related to the measurement accuracy. Yet, in many cases, the precision represents only a small fraction of the total budget. This paper addresses this shortcoming by considering two significant sources of uncertainty in the quantitative matrix correction models--the mass absorption coefficient, [μ/ρ], and the backscatter coefficient, η. Understanding the influence of these sources provides insight into the utility of EPMA measurements, and equally important, it allows practitioners to develop strategies to optimize measurement accuracy by minimizing the influence of poorly known model parameters.

  8. X-ray intravital microscopy for functional imaging in rat hearts using synchrotron radiation coronary microangiography

    SciTech Connect

    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 ms 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

  9. X-ray intravital microscopy for functional imaging in rat hearts using synchrotron radiation coronary microangiography.

    PubMed

    Umetani, K; Fukushima, K

    2013-03-01

    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 μm, yielding sharp images of small arteries. The exposure time has been shortened to around 2 ms 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 μm 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 μm 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

  10. X-ray intravital microscopy for functional imaging in rat hearts using synchrotron radiation coronary microangiography

    NASA Astrophysics Data System (ADS)

    Umetani, K.; Fukushima, K.

    2013-03-01

    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 μm, yielding sharp images of small arteries. The exposure time has been shortened to around 2 ms 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 μm 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 μm 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

  11. Artifact characterization and reduction in scanning X-ray Zernike phase contrast microscopy.

    PubMed

    Vartiainen, Ismo; Holzner, Christian; Mohacsi, Istvan; Karvinen, Petri; Diaz, Ana; Pigino, Gaia; David, Christian

    2015-05-18

    Zernike phase contrast microscopy is a well-established method for imaging specimens with low absorption contrast. It has been successfully implemented in full-field microscopy using visible light and X-rays. In microscopy Cowley's reciprocity principle connects scanning and full-field imaging. Even though the reciprocity in Zernike phase contrast has been discussed by several authors over the past thirty years, only recently it was experimentally verified using scanning X-ray microscopy. In this paper, we investigate the image and contrast formation in scanning Zernike phase contrast microscopy with a particular and detailed focus on the origin of imaging artifacts that are typically associated with Zernike phase contrast. We demonstrate experimentally with X-rays the effect of the phase mask design on the contrast and halo artifacts and present an optimized design of the phase mask with respect to photon efficiency and artifact reduction. Similarly, due to the principle of reciprocity the observations and conclusions of this work have direct applicability to Zernike phase contrast in full-field microscopy as well.

  12. UV-Visible Absorption Spectroscopy Enhanced X-ray Crystallography at Synchrotron and X-ray Free Electron Laser Sources.

    PubMed

    Cohen, Aina E; Doukov, Tzanko; Soltis, Michael S

    2016-01-01

    This review describes the use of single crystal UV-Visible Absorption micro-Spectrophotometry (UV-Vis AS) to enhance the design and execution of X-ray crystallography experiments for structural investigations of reaction intermediates of redox active and photosensitive proteins. Considerations for UV-Vis AS measurements at the synchrotron and associated instrumentation are described. UV-Vis AS is useful to verify the intermediate state of an enzyme and to monitor the progression of reactions within crystals. Radiation induced redox changes within protein crystals may be monitored to devise effective diffraction data collection strategies. An overview of the specific effects of radiation damage on macromolecular crystals is presented along with data collection strategies that minimize these effects by combining data from multiple crystals used at the synchrotron and with the X-ray free electron laser.

  13. Femtosecond synchronism of x-rays and visible/infrared light in an x-ray free-electron laser

    NASA Astrophysics Data System (ADS)

    Adams, B. W.

    2007-12-01

    A way is proposed to obtain ultrashort pulses of intense infrared/visible light in few-femtosecond synchronism with x-rays from an x-ray free-electron laser (XFEL). It makes use of the recently proposed emittance-slicing technique [Emma et al., Phys. Rev. Lett. 92, 074801 (2004)] to both restrict the duration of self-amplified spontaneous emission (SASE) to a few femtoseconds and to lead to a coherence enhancement of near-infrared transition undulator radiation (CTUR). The x-rays and the near-infrared light originate within the XFEL undulator from the same slice of electrons within a bunch and are therefore perfectly synchronized with each other. An example of realizing the scheme at the Linac Coherent Light Source is presented. A few side issues are explored briefly, such as the magnitude of the velocity term versus the acceleration term in the Lienard-Wiechert fields and the possible use of the CTUR as a diagnostic tool for the SASE process itself.

  14. Few-femtosecond time-resolved measurements of X-ray free-electron lasers.

    PubMed

    Behrens, C; Decker, F-J; Ding, Y; Dolgashev, V A; Frisch, J; Huang, Z; Krejcik, P; Loos, H; Lutman, A; Maxwell, T J; Turner, J; Wang, J; Wang, M-H; Welch, J; Wu, J

    2014-04-30

    X-ray free-electron lasers, with pulse durations ranging from a few to several hundred femtoseconds, are uniquely suited for studying atomic, molecular, chemical and biological systems. Characterizing the temporal profiles of these femtosecond X-ray pulses that vary from shot to shot is not only challenging but also important for data interpretation. Here we report the time-resolved measurements of X-ray free-electron lasers by using an X-band radiofrequency transverse deflector at the Linac Coherent Light Source. We demonstrate this method to be a simple, non-invasive technique with a large dynamic range for single-shot electron and X-ray temporal characterization. A resolution of less than 1 fs root mean square has been achieved for soft X-ray pulses. The lasing evolution along the undulator has been studied with the electron trapping being observed as the X-ray peak power approaches 100 GW.

  15. Three-dimensional imaging of chemical phase transformations at the nanoscale with full-field transmission X-ray microscopy

    PubMed Central

    Meirer, Florian; Cabana, Jordi; Liu, Yijin; Mehta, Apurva; Andrews, Joy C.; Pianetta, Piero

    2011-01-01

    The ability to probe morphology and phase distribution in complex systems at multiple length scales unravels the interplay of nano- and micrometer-scale factors at the origin of macroscopic behavior. While different electron- and X-ray-based imaging techniques can be combined with spectroscopy at high resolutions, owing to experimental time limitations the resulting fields of view are too small to be representative of a composite sample. Here a new X-ray imaging set-up is proposed, combining full-field transmission X-ray microscopy (TXM) with X-ray absorption near-edge structure (XANES) spectroscopy to follow two-dimensional and three-dimensional morphological and chemical changes in large volumes at high resolution (tens of nanometers). TXM XANES imaging offers chemical speciation at the nanoscale in thick samples (>20 µm) with minimal preparation requirements. Further, its high throughput allows the analysis of large areas (up to millimeters) in minutes to a few hours. Proof of concept is provided using battery electrodes, although its versatility will lead to impact in a number of diverse research fields. PMID:21862859

  16. Time-resolved soft X-ray microscopy of magnetic nanostructures at the P04 beamline at PETRA III

    NASA Astrophysics Data System (ADS)

    Wessels, P.; Ewald, J.; Wieland, M.; Nisius, T.; Abbati, G.; Baumbach, S.; Overbuschmann, J.; Vogel, A.; Neumann, A.; Viefhaus, J.; Oepen, H. P.; Meier, G.; Wilhein, T.; Drescher, M.

    2014-04-01

    We present first time-resolved measurements of a new mobile full-field transmission microscope [1] obtained at the soft X-ray beamline P04 at the high brilliance synchrotron radiation source PETRA III. A nanostructured magnetic permalloy (Ni80Fe20) sample can be excited by the magnetic field of a 400 ps full width at half maximum (FWHM) long electric current pulse in a coplanar waveguide. The full-field soft X-ray microscope successively probes the time evolution of the sample magnetization via X-ray magnetic circular dichroism (XMCD) [2] spectromicroscopy in a pump-probe scheme by varying the delay between pump and probe pulses electronically. Static and transient magnetic fields of a permanent magnet and a coil are available in the sample plane to reset the system and to provide external offset fields. The microscope generates a flat-top illumination field of 20 μm diameter by using a grating condenser [3] and the sample plane is directly imaged by a micro zone plate with 60 nm resolution onto a 2D gateable X-ray detector to select the particular bunch in the storage ring that contains the dynamic information. The setup is built into a mobile endstation vacuum system with in-house developed three-axis piezo motorized stages for high accuracy positioning of all microscopy-components inside the chambers.

  17. Taking X-ray Diffraction to the Limit: Macromolecular Structures from Femtosecond X-ray Pulses and Diffraction Microscopy of Cells with Synchrotron Radiation

    SciTech Connect

    Chapman, H N; Miao, J; Kirz, J; Sayre, D; Hodgson, K O

    2003-10-01

    The methodology of X-ray crystallography has recently been successfully extended to the structure determination of non-crystalline specimens. The phase problem was solved by using the oversampling method, which takes advantage of ''continuous'' diffraction pattern from non-crystalline specimens. Here we review the principle of this newly developed technique and discuss the ongoing experiments of imaging non-periodic objects, like cells and cellular structures using coherent and bright X-rays from the 3rd generation synchrotron radiation. In the longer run, the technique may be applied to image single biomolecules by using the anticipated X-ray free electron lasers. Computer simulations have so far demonstrated two important steps: (1) by using an extremely intense femtosecond X-ray pulse, a diffraction pattern can be recorded from a macromolecule before radiation damage manifests itself, and (2) the phase information can be ab initio retrieved from a set of calculated noisy diffraction patterns of single protein molecules.

  18. Taking X-Ray Diffraction to the Limit: Macromolecular Structures from Femtosecond X-Ray Pulses and Diffraction Microscopy of Cells with Synchrotron Radiation

    SciTech Connect

    Miao, J.

    2004-06-04

    Recent work is extending the methodology of X-ray crystallography to the structure determination of noncrystalline specimens. The phase problem is solved using the oversampling method, which takes advantage of ''continuous'' diffraction patterns from noncrystalline specimens. Here we review the principle of this newly developed technique and discuss the ongoing experiments of imaging nonperiodic objects, such as cells and cellular structures, using coherent and bright X rays produced by third-generation synchrotron sources. In the longer run, the technique may be applicable to image single biomolecules using anticipated X-ray free electron lasers. Here, computer simulations have so far demonstrated two important steps: (a) by using an extremely intense femtosecond X-ray pulse, a diffraction pattern can be recorded from a macromolecule before radiation damage manifests itself; and (b) the phase information can be retrieved in an ab initio fashion from a set of calculated noisy diffraction patterns of single protein molecules.

  19. Electrodynamics of relativistic electron beam x-ray sources

    NASA Astrophysics Data System (ADS)

    Niknejadi, Pardis

    Probing matter at atomic scales provides invaluable information about its structure; as a result interest in sources of x-rays and gamma-rays with high spectral resolution, low angular divergence and small source size has been on the rise. Explorations in this domain require x-ray or gamma-ray sources with high brightness. In the past decade, relativistic electron sources such as synchrotron rings and free electron lasers have proven to be the best technology available for the production of such beams. We1 start with an introduction to the physics of radiation and provide a summary of the theoretical grounds this work is based on. This dissertation is dedicated to different aspects of both fundamental processes of radiation in relativistic electron sources, and critical control and diagnostics that are required for the operation of these sources. Therefore this work is broken into two main parts. In the first part, the electron source that is currently set up at University of Hawai`i at Manoa will be introduced in detail. This source has unique capabilities as it is an inverse-Compton scattering (ICS) source that uses a free electron laser (FEL) with pulses of picosecond duration at ˜ 3 GHz rate for production of a coherent/semi-coherent x-ray beam by means of an optical cavity. After introducing the essential elements of the system and what was achieved prior to this work, we will focus on the requirements for achieving an optimum electron beam matched for the operation of the system which is the main focus of part I of this dissertation. The transport beam line of our system is unique and complex. For this reason, a simulation module has been developed for the study and delivery of an optimal beam. We will discuss the capabilities of this system and its compatibility with other elements that were already installed on the beam line. Finally, we will present results and experimental data as well as guidelines for future operation of the system when the microwave

  20. Accuracy evaluation of a Compton X-ray spectrometer with bremsstrahlung X-rays generated by a 6 MeV electron bunch.

    PubMed

    Kojima, Sadaoki; Arikawa, Yasunobu; Nishimura, Yasuhiko; Togawa, Hiromi; Zhang, Zhe; Ikenouchi, Takahito; Ozaki, Tetsuo; Morace, Alessio; Nagai, Takahiro; Abe, Yuki; Sakata, Shouhei; Inoue, Hiroaki; Utsugi, Masaru; Nakai, Mitsuo; Nishimura, Hiroaki; Shiraga, Hiroyuki; Kato, Ryukou; Fujioka, Shinsuke; Azechi, Hiroshi

    2014-11-01

    A Compton-scattering-based X-ray spectrometer is developed to obtain the energy distribution of fast electrons produced by intense laser and matter interactions. Bremsstrahlung X-rays generated by fast electrons in a material are used to measure fast electrons' energy distribution in matter. In the Compton X-ray spectrometer, X-rays are converted into recoil electrons by Compton scattering in a converter made from fused silica glass, and a magnet-based electron energy analyzer is used to measure the energy distribution of the electrons that recoil in the direction of the incident X-rays. The spectrum of the incident X-rays is reconstructed from the energy distribution of the recoil electrons. The accuracy of this spectrometer is evaluated using a quasi-monoenergetic 6 MeV electron bunch that emanates from a linear accelerator. An electron bunch is injected into a 1.5 mm thick tungsten plate to produce bremsstrahlung X-rays. The spectrum of these bremsstrahlung X-rays is obtained in the range from 1 to 9 MeV. The energy of the electrons in the bunch is estimated using a Monte Carlo simulation of particle-matter interactions. The result shows that the spectrometer's energy accuracy is ±0.5 MeV for 6.0 MeV electrons.