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Sample records for projection x-ray microscopy

  1. Tomographic reconstruction in soft x-ray microscopy using focus-stack back-projection.

    PubMed

    Selin, Mårten; Fogelqvist, Emelie; Werner, Stephan; Hertz, Hans M

    2015-05-15

    Tomographic reconstruction in soft x-ray microscopy is a powerful technique for obtaining high-resolution 3D images of biological samples. However, the depth of focus of such zone-plate-based microscopes is typically shorter than the thickness of many relevant biological objects, challenging the validity of the projection assumption used in conventional reconstruction algorithms. In order to make full use of the soft x-ray microscopes' high resolution, the tomographic reconstruction needs to take the depth of focus into account. Here we present a method to achieve high resolution in the full sample when the depth of focus is short compared to the sample thickness. The method relies on the back-projection of focus-stacked image data from x-ray microscopy. We demonstrate the method on theoretical and experimental data. PMID:26393699

  2. Tomographic reconstruction in soft x-ray microscopy using focus-stack back-projection.

    PubMed

    Selin, Mårten; Fogelqvist, Emelie; Werner, Stephan; Hertz, Hans M

    2015-05-15

    Tomographic reconstruction in soft x-ray microscopy is a powerful technique for obtaining high-resolution 3D images of biological samples. However, the depth of focus of such zone-plate-based microscopes is typically shorter than the thickness of many relevant biological objects, challenging the validity of the projection assumption used in conventional reconstruction algorithms. In order to make full use of the soft x-ray microscopes' high resolution, the tomographic reconstruction needs to take the depth of focus into account. Here we present a method to achieve high resolution in the full sample when the depth of focus is short compared to the sample thickness. The method relies on the back-projection of focus-stacked image data from x-ray microscopy. We demonstrate the method on theoretical and experimental data.

  3. Projection phase contrast microscopy with a hard x-ray nanofocused beam: Defocus and contrast transfer

    SciTech Connect

    Salditt, T.; Giewekemeyer, K.; Fuhse, C.; Krueger, S. P.; Tucoulou, R.; Cloetens, P.

    2009-05-01

    We report a projection phase contrast microscopy experiment using hard x-ray pink beam undulator radiation focused by an adaptive mirror system to 100-200 nm spot size. This source is used to illuminate a lithographic test pattern with a well-controlled range of spatial frequencies. The oscillatory nature of the contrast transfer function with source-to-sample distance in this holographic imaging scheme is quantified and the validity of the weak phase object approximation is confirmed for the experimental conditions.

  4. Quantitative X-ray projection microscopy: phase-contrast and multi-spectral imaging.

    PubMed

    Mayo, S C; Miller, P R; Wilkins, S W; Davis, T J; Gao, D; Gureyev, T E; Paganin, D; Parry, D J; Pogany, A; Stevenson, A W

    2002-08-01

    We outline a new approach to X-ray projection microscopy in a scanning electron microscope (SEM), which exploits phase contrast to boost the quality and information content of images. These developments have been made possible by the combination of a high-brightness field-emission gun (FEG)-based SEM, direct detection CCD technology and new phase retrieval algorithms. Using this approach we have been able to obtain spatial resolution of < 0.2 micro m and have demonstrated novel features such as: (i) phase-contrast enhanced visibility of high spatial frequency image features (e.g. edges and boundaries) over a wide energy range; (ii) energy-resolved imaging to simultaneously produce multiple quasi-monochromatic images using broad-band polychromatic illumination; (iii) easy implementation of microtomography; (iv) rapid and robust phase/amplitude-retrieval algorithms to enable new real-time and quantitative modes of microscopic imaging. These algorithms can also be applied successfully to recover object-plane information from intermediate-field images, unlocking the potentially greater contrast and resolution of the intermediate-field regime. Widespread applications are envisaged for fields such as materials science, biological and biomedical research and microelectronics device inspection. Some illustrative examples are presented. The quantitative methods described here are also very relevant to projection microscopy using other sources of radiation, such as visible light and electrons.

  5. 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.

  6. Effect of contrast enhancement prior to iteration procedure on image correction for soft x-ray projection microscopy

    NASA Astrophysics Data System (ADS)

    Jamsranjav, Erdenetogtokh; Shiina, Tatsuo; Kuge, Kenichi; Kinjo, Yasuhito; Nakamura, Yuichi; Shinohara, Kunio; Ito, Atsushi

    2016-01-01

    Soft X-ray microscopy is well recognized as a powerful tool of high-resolution imaging for hydrated biological specimens. Projection type of it has characteristics of easy zooming function, simple optical layout and so on. However the image is blurred by the diffraction of X-rays, leading the spatial resolution to be worse. In this study, the blurred images have been corrected by an iteration procedure, i.e., Fresnel and inverse Fresnel transformations repeated. This method was confirmed by earlier studies to be effective. Nevertheless it was not enough to some images showing too low contrast, especially at high magnification. In the present study, we tried a contrast enhancement method to make the diffraction fringes clearer prior to the iteration procedure. The method was effective to improve the images which were not successful by iteration procedure only.

  7. X-ray microscopy using synchrotron radiation

    SciTech Connect

    Jones, K.W.; Gordon, B.M.; Hanson, A.L.; Pounds, J.G.; Rivers, M.L.; Schidlovsky, G.; Smith, J.V.; Spanne, P.; Sutton, S.R.

    1989-01-01

    The system for x-ray microscopy now being developed at the X-26 beam line of the Brookhaven National Synchrotron Light Source (NSLS) is described here. Examples of the use of x-ray microscopy for trace element geochemistry, biology and medicine, and materials investigations are given to emphasize the scientific applications of the technique. Future directions for the improvement and further development of the X-26 microscope and of the x-ray microscopy field in general are discussed. 11 refs., 7 figs.

  8. Four-dimensional in vivo X-ray microscopy with projection-guided gating

    NASA Astrophysics Data System (ADS)

    Mokso, Rajmund; Schwyn, Daniel A.; Walker, Simon M.; Doube, Michael; Wicklein, Martina; Müller, Tonya; Stampanoni, Marco; Taylor, Graham K.; Krapp, Holger G.

    2015-03-01

    Visualizing fast micrometer scale internal movements of small animals is a key challenge for functional anatomy, physiology and biomechanics. We combine phase contrast tomographic microscopy (down to 3.3 μm voxel size) with retrospective, projection-based gating (in the order of hundreds of microseconds) to improve the spatiotemporal resolution by an order of magnitude over previous studies. We demonstrate our method by visualizing 20 three-dimensional snapshots through the 150 Hz oscillations of the blowfly flight motor.

  9. Four-dimensional in vivo X-ray microscopy with projection-guided gating

    PubMed Central

    Mokso, Rajmund; Schwyn, Daniel A.; Walker, Simon M.; Doube, Michael; Wicklein, Martina; Müller, Tonya; Stampanoni, Marco; Taylor, Graham K.; Krapp, Holger G.

    2015-01-01

    Visualizing fast micrometer scale internal movements of small animals is a key challenge for functional anatomy, physiology and biomechanics. We combine phase contrast tomographic microscopy (down to 3.3 μm voxel size) with retrospective, projection-based gating (in the order of hundreds of microseconds) to improve the spatiotemporal resolution by an order of magnitude over previous studies. We demonstrate our method by visualizing 20 three-dimensional snapshots through the 150 Hz oscillations of the blowfly flight motor. PMID:25762080

  10. 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

  11. 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. PMID:27446649

  12. 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.

  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. 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.

  15. Observation of living cells by x-ray microscopy with a laser-plasma x-ray source

    NASA Astrophysics Data System (ADS)

    Tomie, Toshihisa; Shimizu, Hazime; Majima, Toshikazu; Yamada, Mitsuo; Kanayama, Toshihiko; Yano, M.; Kondo, H.

    1991-12-01

    We studied laser-produced plasma as an x-ray source for x-ray microscopy. Using water- window x rays, contact x-ray images of living sea urchin sperm were taken by a 500 picosecond x-ray pulse. The resist relief was examined by atomic force microscope and informations characteristic of x-ray microscopy were obtained. The finest feature noticed in the x-ray image was 0.1 micrometers .

  16. Cryotomography x-ray microscopy state

    DOEpatents

    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.

  17. 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.

  18. 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.

  19. Studies on X-ray diffraction microscopy

    NASA Astrophysics Data System (ADS)

    Miao, Huijie

    This dissertation includes three main parts: studies on coherence requirements for the diffraction microscopy experiments, ice formation on frozen-hydrated sample during data collection, and centering of the diffraction data sets. These three subjects are all in support of our groups overall goal of high resolution 3D imaging of frozen hydrated eukaryotic cells via x-ray diffraction microscopy. X-ray diffraction microscopy requires coherent illumination. However, the actual degree of coherence at some beamlines has never been tested. In research on coherence, our first aim is to determine the transverse coherence width at the sample plane at BL 9.0.1 at the Advanced Light Source in Lawrence Berkeley National Laboratory. An analytical calculation of the coherence at the sample plane is presented. Experimental diffraction patterns of pinhole-pair samples were also taken at the beamline to determine the coherence. Due to the irregular shape of the pinholes and other optics complexity, it was very difficult to fit the data with known theoretical equations as it was traditionally done with 1D data. However, we found out that the auto-correlation function shows clearly three spots. Theoretical calculation have been carried out to show that the degree of coherence can be obtained from the intensities of the three spots. These results are compared with the results from the analytical calculation. We then perform a simulation, showing the required transverse coherence width for reconstructing samples with a given size. Ice accumulation has been a major problem in X-ray diffraction microscopy with frozen hydrated samples. Since the ice structure is different from point to point, we cannot subtract the scattering from ice, nor assume a completely "empty" region outside the finite support constraint area as required for reconstruction. Ice forms during the sample preparation and transfer. However, from the tests we did in September 2007, we found that the ice layer thickens

  20. Differential interference contrast x-ray microscopy with submicron resolution

    NASA Astrophysics Data System (ADS)

    Wilhein, Thomas; Kaulich, Burkhard; Di Fabrizio, Enzo; Romanato, Fillipo; Cabrini, Stefano; Susini, Jean

    2001-04-01

    Progress in lithography and nanofabrication [E. Di Fabrizio et al., Nature (London) 401, 895 (1999)] has made it possible to apply differential interference contrast (DIC) in x-ray microscopy using an original x-ray doublet lens based on two specially developed zone plates. Switching from bright-field imaging (absorption contrast) to x-ray DIC, we observe, similar to visible-light microscopy, a dramatic increase in image contrast for weak absorbing samples. We anticipate that this technique will have a significant impact on x-ray imaging and may play a role comparable to DIC imaging in visible-light microscopy.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

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

    NASA Astrophysics Data System (ADS)

    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.

    2007-01-01

    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.

  8. X-ray microscopy study of bone mineralization

    NASA Astrophysics Data System (ADS)

    Salomé, M.; Lafage-Proust, M. H.; Vico, L.; Amblard, D.; Kaulich, B.; Oestreich, S.; Susini, J.; Barrett, R.

    2000-05-01

    Transmission spectro-microscopy around the calcium K-edge and fluorescence microscopy were performed respectively on the Transmission X-ray Microscope (TXM) and Scanning X-ray Microscope (SXM) end-stations of ID21 beamline at ESRF, to map the calcium distribution and the Ca/P ratio in bone samples. Preliminary results are presented. The motivation for these experiments is the study of the genetic determinism of bone mineralisation parameters in two different strains of mice.

  9. X-ray diffraction microscopy of magnetic structures.

    PubMed

    Turner, Joshua J; Huang, Xiaojing; Krupin, Oleg; Seu, Keoki A; Parks, Daniel; Kevan, Stephen; Lima, Enju; Kisslinger, Kim; McNulty, Ian; Gambino, Richard; Mangin, Stephane; Roy, Sujoy; Fischer, Peter

    2011-07-15

    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 L3 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.

  10. 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.

  11. 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

  12. 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.

  13. Cryogenic X-ray Diffraction Microscopy for Biological Samples

    SciTech Connect

    E Lima; L Wiegart; P Pernot; M Howells; J Timmins; F Zontone; A Madsen

    2011-12-31

    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.

  14. X-ray microscopy using collimated and focussed synchrotron radiation

    SciTech Connect

    Jones, K.W.; Kwiatek, W.M.; Gordon, B.M.; Hanson, A.L.; Pounds, J.G.; Rivers, M.L.; Sutton, S.R.; Thompson, A.C.; Underwood, J.H.; Giauque, R.D.

    1987-01-01

    X-ray microscopy is a field that has developed rapidly in recent years. Two different approaches have been used. Zone plates have been employed to produce focused beams with sizes as low as 0.07 ..mu..m for x-ray energies below 1 keV. Images of biological materials and elemental maps for major and minor low Z have been produced using above and below absorption edge differences. At higher energies collimators and focusing mirrors have been used to make small diameter beams for excitation of characteristic K- or L-x rays of all elements in the periodic table. The practicality of a single instrument combining all the features of these two approaches is unclear. The use of high-energy x rays for x-ray microscopy has intrinsic value for characterization of thick samples and determination of trace amounts of most elements. A summary of work done on the X-26 beam line at the National Synchrotron Light Source (NSLS) with collimated and focused x rays with energies above 4 keV is given here. 6 refs., 5 figs., 1 tab.

  15. 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.

  16. 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

  17. X-ray absorption microscopy of aqueous samples

    NASA Astrophysics Data System (ADS)

    Frazer, Brad; Gilbert, Benjamin; De Stasio, Gelsomina

    2002-03-01

    X-ray photoelectron emission microscopy (X-PEEM) is used for numerous applications in surface microchemical analysis of material science and biological specimens. We have reconfigured the MEPHISTO X-PEEM instrument that is installed at the University of Wisconsin Synchrotron Radiation Center to measure true x-ray transmission spectra by converting transmitted photons to photoelectrons via a thin photocathode layer of gold. We have also developed a method by which to introduce aqueous samples into ultrahigh vacuum. Hence x-ray spectroscopy can be performed on biologically relevant elements (such as K, Ca, etc.) in a physiological environment, i.e., in solution. More important, when coupled with X-PEEM imaging this technique may offer the unique and exciting possibility of studying living cells. We present initial x-ray absorption spectra of solutions of aqueous ionic and chelated Ca, with the aim of distinguishing bound and free ionic calcium in vivo.

  18. 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.

  19. Biological imaging by soft x-ray diffraction microscopy

    DOE PAGES

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

    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

  20. 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).

  1. 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).

  2. Transmission X-ray microscopy of spider dragline silk.

    PubMed

    Glisović, Anja; Thieme, Jürgen; Guttmann, Peter; Salditt, Tim

    2007-01-30

    We have investigated the structure of spider silk fibers from two different Nephila species and three different Araneus species by transmission X-ray microscopy (TXM). Single fibers and double fibers have been imaged. All images are in agreement with a homogenous density on length scales between the fiber diameter and the resolution of the instrument, which is about 25 nm. PMID:16889826

  3. Soft X-ray contact microscopy of nematode Caenorhabditis elegans

    NASA Astrophysics Data System (ADS)

    Poletti, G.; Orsini, F.; Batani, D.; Bernardinello, A.; Desai, T.; Ullschmied, J.; Skala, J.; Kralikova, B.; Krousky, E.; Juha, L.; Pfeifer, M.; Kadlec, Ch.; Mocek, T.; Präg, A.; Renner, O.; Cotelli, F.; Lora Lamia, C.; Zullini, A.

    2004-08-01

    Soft X-ray Contact Microscopy (SXCM) of Caenorhabditis elegans nematodes with typical length ~800 μ m and diameter ~30 μ m has been performed using the PALS laser source of wavelength λ = 1.314~μ m and pulse duration τ (FWHM) = 400 ps. Pulsed soft X-rays were generated using molybdenum and gold targets with laser intensities I ≥ 1014 W/cm2. Images have been recorded on PMMA photo resists and analyzed using an atomic force microscope operating in contact mode. Cuticle features and several internal organs have been identified in the SXCM images including lateral field, cuticle annuli, pharynx, and hypodermal and neuronal cell nuclei.

  4. 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.

  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. Synchrotron X-ray Enhanced Scanning Tunneling Microscopy

    NASA Astrophysics Data System (ADS)

    Rose, Volker; Freeland, John

    2011-03-01

    Proper understanding of complex phenomena occurring in nanostructures requires tools with both the ability to resolve the nanometer scale as well as provide detailed information about chemical, electronic, and magnetic structure. Scanning tunneling microscopy (STM) achieves the requisite high spatial resolution; however, direct elemental determination is not easily accomplished. X-ray microscopies, on the other hand, provide elemental selectivity, but currently have spatial resolution only of tens of nanometers. We present a novel and radically different concept that employs detection of local synchrotron x-ray interactions utilizing a STM that provides spatial resolution, and x-ray absorption directly yields chemical, electronic, and magnetic sensitivity. If during tunneling the sample is simultaneously illuminated with monochromatic x-rays, characteristic absorption will arise. Electrons that are excited into unoccupied levels close to the Fermi level modulate the tunneling current giving rise to elemental contrast. This work was supported by the U. S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under contract DE-AC02-06CH11357.

  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. 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.

  9. 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.

  10. X-ray Microscopy Beamlines at SSRF--Present Status and Future Plan

    SciTech Connect

    Xu, H.; Yu, X.; Tai, R.

    2011-09-09

    The Shanghai Synchrotron Radiation Facility (SSRF) is a 3.5-GeV third-generation light source. The facility has been open for user experiments since May, 2009. This high-brightness x-ray source is an ideal platform for x-ray microscopy. Presently, SSRF has three beamlines related to x-ray microscopy or imaging, namely the soft x-ray spectromicroscopy beamline (STXM), the hard x-ray microfocusing beamline, and the x-ray imaging beamline. The construction of SSRF phase-II beamlines will be carried out during 2011-2017. Seven additional beamlines for x-ray microscopy or imaging will be built.

  11. 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.

  12. 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.

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

    PubMed

    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

    2016-09-01

    Owing to its extreme sensitivity, quantitative mapping of elemental distributions via X-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. PMID:27577770

  14. X-ray Induced Pinhole Closure in Point Projection X-ray Radiography

    SciTech Connect

    Bullock, A B; Landen, O L; Blue, B E; Edwards, J; Bradley, D K

    2006-01-13

    In pinhole-assisted point-projection x-ray radiography (or ''backlighting''), pinholes are placed between the sample of interest and an x-ray source (or ''backlighter'') to effectively limit the source size and hence improve the spatial resolution of the system. Pinholes are generally placed close to such x-ray backlighters to increase the field-of-view, leading to possible vaporization and pinhole closure due to x-ray driven ablation, thereby potentially limiting the usefulness of this method. An experimental study and modeling of time-dependent closure and resolution is presented. The pinhole closure timescale is studied for various pinhole sizes, pinhole to backlighter separations and filtering conditions. In addition the time-dependent resolution is extracted from one-dimensional wire imaging prior to pinhole closure. Cylindrical hydrodynamic modeling of the pinhole closure shows reasonable agreement with data, giving us a predictive capability for pinhole closure in future experiments.

  15. Soft X-ray microscopy to characterize polyelectrolyte assemblies.

    PubMed

    Köhler, Karen; Déjugnat, Christophe; Dubois, Monique; Zemb, Thomas; Sukhorukov, Gleb B; Guttmann, Peter; Möhwald, Helmuth

    2007-07-26

    Transmission microscopy with soft X-rays (TXM) is applied to image in-situ polyelectrolyte assemblies in aqueous environment. The method is element specific and at this stage exhibits a lateral resolution of 20 nm. With the specific examples of hollow capsules and full spheres made of PAH/PSS polyelectrolyte multilayers, it is shown quantitatively that heat treatment irreversibly reduces the water content in the membrane. These experiments complement those reported recently on the polyion system PDADMAC/PSS, which shows a different glass-transition behavior. Finally, the potential and present limitations of TXM are discussed. PMID:17428089

  16. 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.

  17. Soft X-ray Microscopy of Green Cements

    NASA Astrophysics Data System (ADS)

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

    2011-09-01

    The present status of the cement and concrete industry is not sustainable. The production of Portland cement is responsible for 7% of the CO2 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.

  18. 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.

  19. Soft X-Ray Microscopy: Imaging Magnetism at Small Sizes

    NASA Astrophysics Data System (ADS)

    Fischer, Peter

    2010-03-01

    The manipulation of spins on the nanoscale is of both fundamental and technological interest. In spin based electronics the observation that spin currents can exert a torque onto local spin configurations which can e.g. push a domain wall has stimulated significant research activities in order to provide a fundamental understanding of the physical processes involved. Magnetic soft X-ray microscopy is a unique analytical technique combining X-ray magnetic circular dichroism (X-MCD) as element specific magnetic contrast mechanism with high spatial and temporal resolution. Fresnel zone plates used as X-ray optical elements provide a spatial resolution down to currently <12nm [1] thus approaching fundamental magnetic length scales such as the grain size [2] and magnetic exchange lengths. Images can be recorded in external magnetic fields giving access to study magnetization reversal phenomena on the nanoscale and its stochastic character [3] with elemental sensitivity [4]. Utilizing the inherent time structure of current synchrotron sources fast magnetization dynamics with 70ps time resolution, limited by the lengths of the electron bunches, can be performed with a stroboscopic pump-probe scheme. In this talk I will review recent achievements with magnetic soft X-ray microscopy with focus on current induced wall [5] and vortex dynamics in ferromagnetic elements [6]. Future magnetic microscopies are faced with the challenge to provide both spatial resolution in the nanometer regime, a time resolution on a ps to fs scale and elemental specificity to be able to study novel multicomponent and multifunctional magnetic nanostructures and their ultrafast spin dynamics.[4pt] References[0pt] [1] W. Chao, et al., Optics Express 17(20) 17669 (2009) [0pt] [2] M.-Y. Im, et al, Advanced Materials 20 1750 (2008) [0pt] [3] M.-Y. Im, et al., Phys Rev Lett 102 147204 (2009) [0pt] [4] M.-Y. Im, et al., Appl Phys Lett 95 182504 (2009) [0pt] [5] L. Bocklage, et al., Phys Rev B 78 180405(R

  20. 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.

  1. 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.

  2. 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.

  3. Preparation of tissue samples for X-ray fluorescence microscopy

    NASA Astrophysics Data System (ADS)

    Chwiej, Joanna; Szczerbowska-Boruchowska, Magdalena; Lankosz, Marek; Wojcik, Slawomir; Falkenberg, Gerald; Stegowski, Zdzislaw; Setkowicz, Zuzanna

    2005-12-01

    As is well-known, trace elements, especially metals, play an important role in the pathogenesis of many disorders. The topographic and quantitative elemental analysis of pathologically changed tissues may shed some new light on processes leading to the degeneration of cells in the case of selected diseases. An ideal and powerful tool for such purpose is the Synchrotron Microbeam X-ray Fluorescence technique. It enables the carrying out of investigations of the elemental composition of tissues even at the single cell level. The tissue samples for histopathological investigations are routinely fixed and embedded in paraffin. The authors try to verify the usefulness of such prepared tissue sections for elemental analysis with the use of X-ray fluorescence microscopy. Studies were performed on rat brain samples. Changes in elemental composition caused by fixation in formalin or paraformaldehyde and embedding in paraffin were examined. Measurements were carried out at the bending magnet beamline L of the Hamburger Synchrotronstrahlungslabor HASYLAB in Hamburg. The decrease in mass per unit area of K, Br and the increase in P, S, Fe, Cu and Zn in the tissue were observed as a result of the fixation. For the samples embedded in paraffin, a lower level of most elements was observed. Additionally, for these samples, changes in the composition of some elements were not uniform for different analyzed areas of rat brain.

  4. 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.

  5. Present and Future X-ray Tomographic Microscopy at TOMCAT

    SciTech Connect

    Marone, F.; Mokso, R.; Mikuljan, G.; Isenegger, A.; Modregger, P.; Pinzer, B.; Thuering, T.; Mader, K.; Stampanoni, M.; Fife, J.

    2011-09-09

    During its first four years of life, the TOMCAT beamline at the Swiss Light Source has established itself as a state-of-the art hard x-ray tomographic microscopy endstation for experiments on a large variety of samples, ranging from the fields of biology to materials science. It routinely performs absorption as well as phase-contrast imaging with an isotropic voxel size ranging from 0.360 up to 14.8 microns. Phase contrast is obtained either with simple edge-enhancement, a modified transport of intensity approach or grating interferometry. Typical acquisition times are on the order of a few minutes, depending on energy and resolution. A recently implemented automatic sample exchanger is now available for high-throughput studies. In addition to further developments in phase-contrast imaging, current scientific activities at the beamline focus on pushing spatial and temporal resolution by a few orders of magnitude, aiming at nano- and 'real-time' tomography.

  6. 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

  7. X-ray tomography as a complementary technique to nuclear microscopy for biomedical applications

    NASA Astrophysics Data System (ADS)

    Gomez-Morilla, Inmaculada; Pinheiro, Teresa; Odenbach, Stefan; Alcala, Maria Dolores Ynsa

    2009-06-01

    X-ray micro-computed tomography is an excellent tool to examine the morphology of a sample in a non-destructive way, making its inner structure visible. Nuclear microscopy provides quantitative information about the elemental distribution and concentration. Both can be used as complementary techniques in order to get more information about the samples. Osteoporosis is a disease that deteriorates the bone due to, among other things, a failure in the normal hormonal function. In this project, bones from rats under osteoporosis treatments based on hormonal supplementation, as well as healthy bones and osteoporotic ones without treatment, have been analyzed by both nuclear microscopy and X-ray micro-tomography. Following the results achieved by nuclear microscopy, quantitative concentration and distribution of elements such as Ca and P suggested a change in bone density. In order to image this change of density, the same samples have been analyzed by micro-tomography.

  8. 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.

  9. Study of titanate nanotubes by X-ray and electron diffraction and electron microscopy

    SciTech Connect

    Brunatova, Tereza; Popelkova, Daniela; Wan, Wei; Oleynikov, Peter; Danis, Stanislav; Zou, Xiaodong; Kuzel, Radomir

    2014-01-15

    The structure of titanate nanotubes (Ti-NTs) was studied by a combination of powder X-ray diffraction (PXRD), electron diffraction and high resolution transmission electron microscopy (HRTEM). Ti-NTs are prepared by hydrothermal treatment of TiO{sub 2} powder. The structure is identified by powder X-ray diffraction as the one based on the structure of H{sub 2}Ti{sub 2}O{sub 5}·H{sub 2}O phase. The same structure is obtained by projected potential from HRTEM through-focus image series. The structure is verified by simulated PXRD pattern with the aid of the Debye formula. The validity of the model is tested by computing Fourier transformation of a single nanotube which is proportional to measured electron diffraction intensities. A good agreement of this calculation with measured precession electron diffraction data is achieved. - Highlights: • Titanate nanotubes were prepared by hydrothermal method. • X-ray powder diffraction indicated their structure based on that of H{sub 2}Ti{sub 2}O{sub 5}·H{sub 2}O. • Structural model was created with the aid of high-resolution electron microscopy. • The model was verified with electron diffraction data. • X-ray powder diffraction pattern was calculated with the aid of the Debye formula.

  10. 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.

  11. 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.

  12. Halo suppression in full-field x-ray Zernike phase contrast microscopy.

    PubMed

    Vartiainen, Ismo; Mokso, Rajmund; Stampanoni, Marco; David, Christian

    2014-03-15

    Visible light Zernike phase contrast (ZPC) microscopy is a well established method for imaging weakly absorbing samples. The method is also used with hard x-ray photon energies for structural evaluation of material science and biological applications. However, the method suffers from artifacts that are inherent for the Zernike image formation. In this Letter, we investigate their origin and experimentally show how to suppress them in x-ray full-field ZPC microscopy based on diffractive x-ray optics.

  13. 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. PMID:16021423

  14. 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.

  15. 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.

  16. Contact x-ray microscopy. A new technique for imaging cellular fine structure.

    PubMed Central

    Beese, L; Feder, R; Sayre, D

    1986-01-01

    Contact x-ray microscopy potentially allows living, wet cells to be visualized at a resolution of up to 100 A. Furthermore, differential absorption by specific elements permits the study of the distribution of those elements in biological specimens. In contact x-ray microscopy, soft x-rays (10 A to 100 A) pass through a biological sample and expose an underlying x-ray sensitive polymer (resist), producing an image that reflects the photon absorbance within the specimen. The high penetrating power of soft x-ray enables images to be obtained from specimens up to several microns thick. In this paper, the technique is described, some of the areas currently under study are considered, and biological examples of the use of contact x-ray microscopy are given. Images FIGURE 4 FIGURE 5 FIGURE 6 FIGURE 7 PMID:3955174

  17. 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.

  18. Hard X-ray Microscopy with sub 30 nm Spatial Resolution

    NASA Astrophysics Data System (ADS)

    Tang, Mau-Tsu; Song, Yen-Fang; Yin, Gung-Chian; Chen, Fu-Rong; Chen, Jian-Hua; Chen, Yi-Ming; Liang, Keng S.; Duewer, F.; Yun, Wenbing

    2007-01-01

    A transmission X-ray microscope (TXM) has been installed at the BL01B beamline at National Synchrotron Radiation Research Center in Taiwan. This state-of-the-art TXM operational in a range 8-11 keV provides 2D images and 3D tomography with spatial resolution 60 nm, and with the Zernike-phase contrast mode for imaging light materials such as biological specimens. A spatial resolution of the TXM better than 30 nm, apparently the best result in hard X-ray microscopy, has been achieved by employing the third diffraction order of the objective zone plate. The TXM has been applied in diverse research fields, including analysis of failure mechanisms in microelectronic devices, tomographic structures of naturally grown photonic specimens, and the internal structure of fault zone gouges from an earthquake core. Here we discuss the scope and prospects of the project, and the progress of the TXM in NSRRC.

  19. Hard X-ray Microscopy with sub 30 nm Spatial Resolution

    SciTech Connect

    Tang, M.-T.; Song, Y.-F.; Yin, G.-C.; Chen, J.-H.; Chen, Y.-M.; Liang, Keng S.; Chen, F.-R.; Duewer, F.; Yun Wenbing

    2007-01-19

    A transmission X-ray microscope (TXM) has been installed at the BL01B beamline at National Synchrotron Radiation Research Center in Taiwan. This state-of-the-art TXM operational in a range 8-11 keV provides 2D images and 3D tomography with spatial resolution 60 nm, and with the Zernike-phase contrast mode for imaging light materials such as biological specimens. A spatial resolution of the TXM better than 30 nm, apparently the best result in hard X-ray microscopy, has been achieved by employing the third diffraction order of the objective zone plate. The TXM has been applied in diverse research fields, including analysis of failure mechanisms in microelectronic devices, tomographic structures of naturally grown photonic specimens, and the internal structure of fault zone gouges from an earthquake core. Here we discuss the scope and prospects of the project, and the progress of the TXM in NSRRC.

  20. 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.

  1. X-Ray Microscopy at BESSY: From Nano-Tomography to Fs-Imaging

    SciTech Connect

    Schneider, G.; Heim, S.; Rehbein, S.; Eichert, D.; Guttmann, P.

    2007-01-19

    The BESSY X-ray microscopy group has developed a new full-field x-ray microscope with glass capillary condenser. It permits tomography and spectromicroscopy of cryogenic as well as heated samples. Correlative light and x-ray microscopy is supported by an incorporated high resolution light microscope. Spectromicroscopy with polarized x-rays from a helical undulator can be performed with E/{delta}E = 104. With the planned BESSY High Gain Harmonic Generation Free Electron Laser (HGHG-FEL) x-ray imaging with ultra-short pulses and an integral photon flux of about 1011 photons/pulse in an energy bandwidth of 0.1% will be possible. Single shot imaging with a full field Transmission X-ray Microscope (TXM) employing a beam shaper as a condenser will be feasible with 20 fs pulses.

  2. X-Ray Microscopy at BESSY: From Nano-Tomography to Fs-Imaging

    NASA Astrophysics Data System (ADS)

    Schneider, G.; Guttmann, P.; Heim, S.; Rehbein, S.; Eichert, D.; Niemann, B.

    2007-01-01

    The BESSY X-ray microscopy group has developed a new full-field x-ray microscope with glass capillary condenser. It permits tomography and spectromicroscopy of cryogenic as well as heated samples. Correlative light and x-ray microscopy is supported by an incorporated high resolution light microscope. Spectromicroscopy with polarized x-rays from a helical undulator can be performed with E/ΔE = 104. With the planned BESSY High Gain Harmonic Generation Free Electron Laser (HGHG-FEL) x-ray imaging with ultra-short pulses and an integral photon flux of about 1011 photons/pulse in an energy bandwidth of 0.1% will be possible. Single shot imaging with a full field Transmission X-ray Microscope (TXM) employing a beam shaper as a condenser will be feasible with 20 fs pulses.

  3. Nanoscale Examination of Microdamage in Sheep Cortical Bone Using Synchrotron Radiation Transmission X-Ray Microscopy

    PubMed Central

    Brock, Garry R.; Kim, Grace; Ingraffea, Anthony R.; Andrews, Joy C.; Pianetta, Piero; van der Meulen, Marjolein C. H.

    2013-01-01

    Microdamage occurs in bone through repeated and excessive loading. Accumulation of microdamage weakens bone, leading to a loss of strength, stiffness and energy dissipation in the tissue. Imaging techniques used to examine microdamage have typically been limited to the microscale. In the current study microdamage was examined at the nanoscale using transmission x-ray microscopy with an x-ray negative stain, lead-uranyl acetate. Microdamage was generated in notched and unnotched beams of sheep cortical bone (2×2×20 mm), with monotonic and fatigue loading. Bulk sections were removed from beams and stained with lead-uranyl acetate to identify microdamage. Samples were sectioned to 50 microns and imaged using transmission x-ray microscopy producing projection images of microdamage with nanoscale resolution. Staining indicated microdamage occurred in both the tensile and compressive regions. A comparison between monotonic and fatigue loading indicated a statistically significant greater amount of stain present in fatigue loaded sections. Microdamage occurred in three forms: staining to existing bone structures, cross hatch damage and a single crack extending from the notch tip. Comparison to microcomputed tomography demonstrated differences in damage morphology and total damage between the microscale and nanoscale. This method has future applications for understanding the underlying mechanisms for microdamage formation as well as three-dimensional nanoscale examination of microdamage. PMID:23472121

  4. 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.

  5. 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.

  6. 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.

  7. Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

    DOE PAGES

    Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; Lima, Enju; Marchesini, Stefano; Miao, Huijie; Neiman, Aaron M.; Shapiro, David; Steinbrener, Jan; Stewart, Andrew; et al

    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.

  8. Anti-contamination device for cryogenic soft X-ray diffraction microscopy

    DOE PAGES

    Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; Turner, Joshua; Steinbrener, Jan; Shapiro, David; Kirz, Janos; Jacobsen, Chris

    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.

  9. Transmission X-ray microscopy for full-field nano imaging of biomaterials.

    PubMed

    Andrews, Joy C; Meirer, Florian; Liu, Yijin; Mester, Zoltan; Pianetta, Piero

    2011-07-01

    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 imaging. These techniques are discussed and compared in light of results from the 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

  10. 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

  11. Synchrotron Radiation and X-ray FEL Projects in Korea

    NASA Astrophysics Data System (ADS)

    Cho, M. H.

    2012-03-01

    There are two on-going major projects in Pohang Accelerator Laboratory (PAL), the PLS-II light source upgrade and the construction of PAL-XFEL facility. PLS-II is a new light source upgraded from PLS(Pohang Light Source) which had been operated for 16 years from 1995 and shut down in Dec. 2010. The performance will be improved from ``18.9 nm-rad, 2.5 GeV, and 200 mA'' to ``5.8 nm-rad, 3 GeV, and 400 mA'' using three superconducting RF cavities. The old storage ring has been completely dismantled and new DBA ring has been re-installed in the same tunnel within 6 months, and is under commissioning now. The unique feature of PLS-II is the compact employment of 20 insertion-devices including 14 in-vacuum undulators. The PALXFEL is a 0.1-nm hard X-ray FEL construction project started in 2011 and to compete in 2014 with a total budget of 400 M. The PAL-XFEL is designed to have hard X-ray undulator lines at the end of 10-GeV linac, and a dog-leg branch line at 2.65 GeV point for a soft X-ray undulator line simultaneously and independently from hard X-ray FEL undulator line. The overview of two projects with current status is presented.

  12. Imaging of magnetic domains by transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Fischer, P.; Eimüller, T.; Schütz, G.; Guttmann, P.; Schmahl, G.; Pruegl, K.; Bayreuther, G.

    1998-03-01

    The combination of the high-resolution transmission x-ray microscope (TXM) based on the zone plate technique with the x-ray magnetic circular dichroism (X-MCD) providing a huge magnetic contrast is a new technique to image magnetic domain structures. It is inherently element specific and contains information on the local spin and orbital moments of the absorbing species that can be obtained by applying magneto-optical sum rules. A lateral spatial resolution depending on the quality of the zone plates down to 30 nm can be achieved. We report on first results at the Fe 0022-3727/31/6/012/img9 edges of Fe both in amorphous and in multilayered Gd-Fe systems. With a TXM set-up at BESSY I adapted to record magnetic images in varying magnetic fields the evolution of magnetic domains within a complete hysteresis loop and magnetic aftereffects have been studied.

  13. 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)

  14. Coherent Cone-Beam X-ray Microscopy

    SciTech Connect

    Harder, R.; Xiao, X.

    2011-09-09

    A novel full-field imaging method using the (111) Bragg diffraction of a sub-micron gold crystal as the divergent cone-beam for sample illumination is reported. The divergence of the illumination allows for very high magnification, limited only by the achievable ratio of the crystal-to-sample and sample-to-detector distances. In this case an x-ray magnification of approximately 115 was achieved.

  15. 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.

  16. Goldhelox: a project to view the x-ray sun

    NASA Astrophysics Data System (ADS)

    Fair, Melody

    1991-10-01

    The `Goldhelox' project (`GOLD' for the color of the sun and `HELOX' for heliocentric observations in x rays) includes a student run research team, involving more than 30 volunteer students and five advising professors, to design and build a project to obtain observations of the sun in x rays by using the Space Shuttle as a platform while situated in a NASA Get-Away Special (GAS) canister. The GAS program allows universities, companies, and others to send small self-contained experiments into space in canisters that are placed in the Shuttle's cargo bay. The main scientific objective is to construct a high-resolution soft x-ray telescope to take rapid succession, full disk pictures of the sun, hopefully during Solar Max. These images will help in the understanding of such solar features as the corona, flares, and chromosphere. The project is organized into four major groups. The Flight Readiness Team is in charge of testing, quality control, all safety aspects, and NASA documentation. The optics system is being designed and built by the Optics Team, and this includes the telescope that has curved- substrate, multilayer mirrors, an x-ray filter, a microchannel plate (MCP) detector, a phosphor screen, a fiberoptic plate, and a customized camera that uses ordinary film. The motors for driving the telescope in two axes, worm drives, sealed container for the electronics and batteries, and the overall structure are part of the Mechanical Team. The Electrical Team's responsibilities include the photodiode sun sensor, a small heater for environmental control, lead-acid gel batteries, the main data collecting computer, telescope controller, supporting electronics, and electrical feedthroughs. This project should increase knowledge in the area of x-ray optics and spaced-based physics.

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

    DOE PAGES

    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 andmore » freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy.« less

  18. 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.

  19. 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.

  20. Halo suppression in full-field x-ray Zernike phase contrast microscopy.

    PubMed

    Vartiainen, Ismo; Mokso, Rajmund; Stampanoni, Marco; David, Christian

    2014-03-15

    Visible light Zernike phase contrast (ZPC) microscopy is a well established method for imaging weakly absorbing samples. The method is also used with hard x-ray photon energies for structural evaluation of material science and biological applications. However, the method suffers from artifacts that are inherent for the Zernike image formation. In this Letter, we investigate their origin and experimentally show how to suppress them in x-ray full-field ZPC microscopy based on diffractive x-ray optics. PMID:24690848

  1. Retrieving spin textures on curved magnetic thin films with full-field soft X-ray microscopies

    DOE PAGES

    Streubel, Robert; Kronast, Florian; Fischer, Peter; Parkinson, Dula; Schmidt, Oliver G.; Makarov, Denys

    2015-07-03

    X-ray tomography is a well-established technique to characterize 3D structures in material sciences and biology; its magnetic analogue—magnetic X-ray tomography—is yet to be developed. We demonstrate the visualization and reconstruction of magnetic domain structures in a 3D curved magnetic thin films with tubular shape by means of full-field soft X-ray microscopies. In the 3D arrangement of the magnetization is retrieved from a set of 2D projections by analysing the evolution of the magnetic contrast with varying projection angle. By using reconstruction algorithms to analyse the angular evolution of 2D projections provides quantitative information about domain patterns and magnetic coupling phenomenamore » between windings of azimuthally and radially magnetized tubular objects. In conclusion, the present approach represents a first milestone towards visualizing magnetization textures of 3D curved thin films with virtually arbitrary shape.« less

  2. Retrieving spin textures on curved magnetic thin films with full-field soft X-ray microscopies

    PubMed Central

    Streubel, Robert; Kronast, Florian; Fischer, Peter; Parkinson, Dula; Schmidt, Oliver G.; Makarov, Denys

    2015-01-01

    X-ray tomography is a well-established technique to characterize 3D structures in material sciences and biology; its magnetic analogue—magnetic X-ray tomography—is yet to be developed. Here we demonstrate the visualization and reconstruction of magnetic domain structures in a 3D curved magnetic thin films with tubular shape by means of full-field soft X-ray microscopies. The 3D arrangement of the magnetization is retrieved from a set of 2D projections by analysing the evolution of the magnetic contrast with varying projection angle. Using reconstruction algorithms to analyse the angular evolution of 2D projections provides quantitative information about domain patterns and magnetic coupling phenomena between windings of azimuthally and radially magnetized tubular objects. The present approach represents a first milestone towards visualizing magnetization textures of 3D curved thin films with virtually arbitrary shape. PMID:26139445

  3. Retrieving spin textures on curved magnetic thin films with full-field soft X-ray microscopies.

    PubMed

    Streubel, Robert; Kronast, Florian; Fischer, Peter; Parkinson, Dula; Schmidt, Oliver G; Makarov, Denys

    2015-01-01

    X-ray tomography is a well-established technique to characterize 3D structures in material sciences and biology; its magnetic analogue--magnetic X-ray tomography--is yet to be developed. Here we demonstrate the visualization and reconstruction of magnetic domain structures in a 3D curved magnetic thin films with tubular shape by means of full-field soft X-ray microscopies. The 3D arrangement of the magnetization is retrieved from a set of 2D projections by analysing the evolution of the magnetic contrast with varying projection angle. Using reconstruction algorithms to analyse the angular evolution of 2D projections provides quantitative information about domain patterns and magnetic coupling phenomena between windings of azimuthally and radially magnetized tubular objects. The present approach represents a first milestone towards visualizing magnetization textures of 3D curved thin films with virtually arbitrary shape. PMID:26139445

  4. Retrieving spin textures on curved magnetic thin films with full-field soft X-ray microscopies

    SciTech Connect

    Streubel, Robert; Kronast, Florian; Fischer, Peter; Parkinson, Dula; Schmidt, Oliver G.; Makarov, Denys

    2015-07-03

    X-ray tomography is a well-established technique to characterize 3D structures in material sciences and biology; its magnetic analogue—magnetic X-ray tomography—is yet to be developed. We demonstrate the visualization and reconstruction of magnetic domain structures in a 3D curved magnetic thin films with tubular shape by means of full-field soft X-ray microscopies. In the 3D arrangement of the magnetization is retrieved from a set of 2D projections by analysing the evolution of the magnetic contrast with varying projection angle. By using reconstruction algorithms to analyse the angular evolution of 2D projections provides quantitative information about domain patterns and magnetic coupling phenomena between windings of azimuthally and radially magnetized tubular objects. In conclusion, the present approach represents a first milestone towards visualizing magnetization textures of 3D curved thin films with virtually arbitrary shape.

  5. 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.

  6. Soft X-Ray Microscopy Radiation Damage On Fixed Cells Investigated With Synchrotron Radiation FTIR Microscopy

    PubMed Central

    Gianoncelli, A.; Vaccari, L.; Kourousias, G.; Cassese, D.; Bedolla, D. E.; Kenig, S.; Storici, P.; Lazzarino, M.; Kiskinova, M.

    2015-01-01

    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. PMID:25974639

  7. 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.

  8. Soft X-Ray Microscopy Radiation Damage On Fixed Cells Investigated With Synchrotron Radiation FTIR Microscopy

    NASA Astrophysics Data System (ADS)

    Gianoncelli, A.; Vaccari, L.; Kourousias, G.; Cassese, D.; Bedolla, D. E.; Kenig, S.; Storici, P.; Lazzarino, M.; Kiskinova, M.

    2015-05-01

    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. Evaluation of gratings for X-ray and neutron phase imaging techniques by using x-ray projection microscope

    SciTech Connect

    Minami, Katsunori; Yashiro, Wataru; Olbinado, Margie; Momose, Atsushi

    2012-07-31

    In the X-ray and neutron Talbot (-Lau) interferometry, fabrication of phase or amplitude grating with a high-aspect ratio is a key factor to obtain high quality images. To improve the ability of the grating, evaluation of shape and thickness variation and feed-back to the fabrication process are essential. Here, it is shown that X-ray projection microscope with a spatial resolution of sub-micrometer is a powerful tool for the purpose. Three kinds of gratings have been evaluated by using a projection X-ray microscope with X-ray source size of 0.6 micrometer. Uniformity of thickness of the grating has been visualized nondestructively.

  10. 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.

  11. Ultra-high vacuum compatible optical chopper system for synchrotron x-ray scanning tunneling microscopy

    NASA Astrophysics Data System (ADS)

    Chang, Hao; Cummings, Marvin; Shirato, Nozomi; Stripe, Benjamin; Rosenmann, Daniel; Preissner, Curt; Freeland, John W.; Kersell, Heath; Hla, Saw-Wai; Rose, Volker

    2016-01-01

    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.

  12. Feasibility study on X-ray microscopy in tumor diagnosis at sub-cellular level

    SciTech Connect

    Takemoto, Kuniko; Kihara, Hiroshi

    2007-03-30

    As the first step on utilization of X-ray microscope to tumor diagnosis at sub-cellular level, we have started investigating intracellular localization of heavy metal marker in cancer cells. We calculated the image contrast and photon density for platinum and gold of 100 nm thickness in the protein at various X-ray energies. At hard X-ray region, phase contrast gave effective contrast to image heavy metal marker localization in the cancer cell of 10{mu}m thickness. Minimum incident photons on the specimen were calculated as about 1011 photons/mm2. Combined with a suitable tumor marker and a high brilliant X-ray compact source. X-ray microscopy has capability to be in use as a tumor diagnosis tool with high special resolution.

  13. 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

  14. X-ray microscopy and imaging of Caenorhabditis elegans nematode using a laser-plasma-pulsed x-ray source

    NASA Astrophysics Data System (ADS)

    Poletti, Giulio; Orsini, Franceasco; Ullschmied, Jiri; Skala, Jiri; Kralikova, Bozena; Pfeifer, Miroslav; Kadlec, Christelle; Mocek, Tomas; Prag, A. R.; Cotelli, F.; Lora Lamia, C.; Batani, Dimitri; Bernardinello, A.; Desai, Tara; Zullini, A.

    2004-01-01

    An experiment on Soft X-ray Contact Microscopy (SXCM) performed on Caenorhabditis elegans nematodes is discussed. This sample has been selected since it is a well studied case used as model in many biological contexts. The experiment has been performed using the iodine PALS laser source to generate pulsed soft X-rays from laser-plasma interaction, using molybdenum and gold as targets. Typical intensities on the targets exceeded 1014 W/cm2. The SXCM imprints have been recorded on Polymethilmetacrylate (PMMA) photo resists which have been chemically developed and analyzed with an Atomic Force Microscope (AFM) operating in constant force mode. The use of error signal AFM images together with topography AFM images, did allow an easier recognition of biological patterns, and the identification of observed structures with internal organs. Several organs were identified in the SXCM images, including cuticle annuli, alae, pharynx, and three different types of cell nuclei. These are the first SXCM images of multi-cellular complex organisms.

  15. 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.

  16. Differential phase contrast in scanning x-ray microscopy with half-wavelength phase shifter

    NASA Astrophysics Data System (ADS)

    Suzuki, Yoshio; Takeuchi, Akihisa

    2016-01-01

    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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. Use of backscattered electron imaging, X-ray microanalysis and X-ray microscopy in demonstrating physiological cell death

    SciTech Connect

    Bowen, I.D.; Worrill, N.A.; Winters, C.A.; Mullarkey, K.

    1988-09-01

    The cytochemical localization of enzymatic activity by means of backscattered electron imaging (BEI) is reviewed and the application of BEI to changes in acid phosphatase and ATPase distribution during physiological (programmed) cell death in Heliothis midgut is explored. Programmed cell death entails the release of nascent free acid phosphatase as extracisternal hydrolase. This shift can readily be detected by means of the atomic number contrast imparted by BEI of the lead phosphatase reaction product, thus enabling the distribution of dying cells to be mapped. BEI is particularly useful in this context as it allows the examination of bulk specimens at low magnification. Death of cells is also accompanied by a collapse in ATPase activity which shows up as cytochemically negative areas in the X-ray microscope and by means of BEI. Acid phosphatase in normal cells is localized in the apical microvilli and lysosomes. Senescent or dying cells, however, clearly show a basally situated free hydrolase which migrates throughout the cell. Parallel TEM results confirm that this enzyme is ribosomal and extracisternal rather than lysosomal in origin. ATPase activity is largely limited to the apical microvilli, although there is some activity associated with the basal plasma membranes. The apical ATPase, however is partially resistant to ouabain. Young and mature cells are positive although in the latter case some microvilli may be lost as the cells acquire a negative cap or dome. Inhibition by bromotetramizole indicates that apical activity is not to any significant extent contributed to by alkaline phosphatase. Degenerate or dead cells are negative and can be seen as a mozaic of black patches among normal cells when imaged by means of BEI or X-ray microscopy.

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

    DOE PAGES

    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.; et al

    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

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

    NASA Astrophysics Data System (ADS)

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

    2016-01-01

    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

    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.

  5. 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.

  6. Full-field hard x-ray microscopy with interdigitated silicon lenses

    NASA Astrophysics Data System (ADS)

    Simons, Hugh; Stöhr, Frederik; Michael-Lindhard, Jonas; Jensen, Flemming; Hansen, Ole; Detlefs, Carsten; Poulsen, Henning Friis

    2016-01-01

    Full-field x-ray microscopy using x-ray objectives has become a mainstay of the biological and materials sciences. However, the inefficiency of existing objectives at x-ray energies above 15 keV has limited the technique to weakly absorbing or two-dimensional (2D) samples. Here, we show that significant gains in numerical aperture and spatial resolution may be possible at hard x-ray energies by using silicon-based optics comprising 'interdigitated' refractive silicon lenslets that alternate their focus between the horizontal and vertical directions. By capitalizing on the nano-manufacturing processes available to silicon, we show that it is possible to overcome the inherent inefficiencies of silicon-based optics and interdigitated geometries. As a proof-of-concept of Si-based interdigitated objectives, we demonstrate a prototype interdigitated lens with a resolution of ≈255 nm at 17 keV.

  7. 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.

  8. 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.

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

    PubMed

    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

    2006-05-01

    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.

  10. 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.

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

    PubMed Central

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

    2015-01-01

    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 present 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 X-ray 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. PMID:26226459

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

    PubMed

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

    2015-09-01

    Structures of multisubunit macromolecular machines are primarily determined either by electron microscopy (EM) or by 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 a higher resolution (with finer detail) by X-ray crystallography. The integration of these two structural techniques is becoming increasingly important for the generation of 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 present 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 noncrystallographic symmetry. As the resolution gap between EM and X-ray 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.

  13. 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.

  14. 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. PMID:27505613

  15. 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.

  16. High-energy synchrotron radiation x-ray microscopy: Present status and future prospects

    SciTech Connect

    Jones, K.W.; Gordon, B.M.; Spanne, P. ); Rivers, M.L.; Sutton, S.R. )

    1991-01-01

    High-energy radiation synchrotron x-ray microscopy is used to characterize materials of importance to the chemical and materials sciences and chemical engineering. The x-ray microscope (XRM) forms images of elemental distributions fluorescent x rays or images of mass distributions by measurement of the linear attenuation coefficient of the material. Distributions of sections through materials are obtained non-destructively using the technique of computed microtomography. The energy range of the x rays used for the XRM ranges from a few keV at the minimum value to more than 100 keV, which is sufficient to excite the K-edge of all naturally occurring elements. The work in progress at the Brookhaven NSLS X26 and X17 XRM is described in order to show the current status of the XRM. While there are many possible approaches to the XRM instrumentation, this instrument gives state-of-the-art performance in most respects and serves as a reasonable example of the present status of the instrumentation in terms of the spatial resolution and minimum detection limits obtainable. The examples of applications cited give an idea of the types of research fields that are currently under investigation. They can be used to illustrate how the field of x-ray microscopy will benefit from the use of bending magnets and insertion devices at the Advanced Photon Source. 8 refs., 5 figs.

  17. Visualization of magnetic dipolar interaction based on scanning transmission X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Ohtori, Hiroyuki; Iwano, Kaoru; Mitsumata, Chiharu; Takeichi, Yasuo; Yano, Masao; Kato, Akira; Miyamoto, Noritaka; Shoji, Tetsuya; Manabe, Akira; Ono, Kanta

    2014-04-01

    Using scanning transmission X-ray microscopy (STXM), in this report we visualized the magnetic dipolar interactions in nanocrystalline Nd-Fe-B magnets and imaged their magnetization distributions at various applied fields. We calculated the magnetic dipolar interaction by analyzing the interaction between the magnetization at each point and those at the other points on the STXM image.

  18. In-situ Scanning Transmission X-ray Microscopy of catalytic materials under reaction conditions

    NASA Astrophysics Data System (ADS)

    de Smit, Emiel; Creemer, J. Fredrik; Zandbergen, Henny W.; Weckhuysen, Bert M.; de Groot, Frank M. F.

    2009-11-01

    In-situ Scanning X-ray Transmission Microscopy (STXM) allows the measurement of the soft X-ray absorption spectra with 10 to 30 nm spatial resolution under realistic reaction conditions. We show that STXM-XAS in combination with a micromachined nanoreactor can image a catalytic system under relevant reaction conditions, and provide detailed information on the morphology and composition of the catalyst material. The nanometer resolution combined with powerful chemical speciation by XAS and the ability to image materials under realistic conditions opens up new opportunities to study many chemical processes.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. Mesoscale Science with High Energy X-ray Diffraction Microscopy at the Advanced Photon Source

    NASA Astrophysics Data System (ADS)

    Suter, Robert

    2014-03-01

    Spatially resolved diffraction of monochromatic high energy (> 50 keV) x-rays is used to map microstructural quantities inside of bulk polycrystalline materials. The non-destructive nature of High Energy Diffraction Microscopy (HEDM) measurements allows tracking of responses as samples undergo thermo-mechanical or other treatments. Volumes of the order of a cubic millimeter are probed with micron scale spatial resolution. Data sets allow direct comparisons to computational models of responses that frequently involve long-ranged, multi-grain interactions; such direct comparisons have only become possible with the development of HEDM and other high energy x-ray methods. Near-field measurements map the crystallographic orientation field within and between grains using a computational reconstruction method that simulates the experimental geometry and matches orientations in micron sized volume elements to experimental data containing projected grain images in large numbers of Bragg peaks. Far-field measurements yield elastic strain tensors through indexing schemes that sort observed diffraction peaks into sets associated with individual crystals and detect small radial motions in large numbers of such peaks. Combined measurements, facilitated by a new end station hutch at Advanced Photon Source beamline 1-ID, are mutually beneficial and result in accelerated data reduction. Further, absorption tomography yields density contrast that locates secondary phases, void clusters, and cracks, and tracks sample shape during deformation. A collaboration led by the Air Force Research Laboratory and including the Advanced Photon Source, Lawrence Livermore National Laboratory, Carnegie Mellon University, Petra-III, and Cornell University and CHESS is developing software and hardware for combined measurements. Examples of these capabilities include tracking of grain boundary migrations during thermal annealing, tensile deformation of zirconium, and combined measurements of nickel

  7. 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.

  8. 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

  9. X-ray Microscopy Studies of Electromigration in Advanced Copper Interconnects

    SciTech Connect

    Schneider, G.; Rudolph, S.; Heim, S.; Rehbein, S.; Guttmann, P.

    2006-02-07

    X-rays have the advantage that they penetrate samples which are several micrometers thick without significant sample damage, and that they provide a chemical image contrast between different dielectric layers of the Cu/low-k on-chip interconnect stack. Therefore, x-ray microscopy is an ideal tool for quantitative 3-D investigations of void dynamics with high spatial resolution of 20 nm. Using the BESSY full-field transmission x-ray microscope (TXM), we performed electromigration studies of advanced backend-of-line (BEoL) stacks of high-performance microprocessors containing copper interconnects and low-k materials. We observed void movement along the top copper/dielectric (SiNx) interface which is found to be the main pathway for electromigration-induced atomic copper transport.

  10. 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

    2009-08-01

    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

  11. X-ray Microscopy Studies of Electromigration in Advanced Copper Interconnects

    NASA Astrophysics Data System (ADS)

    Schneider, G.; Guttmann, P.; Rudolph, S.; Heim, S.; Rehbein, S.; Meyer, M. A.; Zschech, E.

    2006-02-01

    X-rays have the advantage that they penetrate samples which are several micrometers thick without significant sample damage, and that they provide a chemical image contrast between different dielectric layers of the Cu/low-k on-chip interconnect stack. Therefore, x-ray microscopy is an ideal tool for quantitative 3-D investigations of void dynamics with high spatial resolution of 20 nm. Using the BESSY full-field transmission x-ray microscope (TXM), we performed electromigration studies of advanced backend-of-line (BEoL) stacks of high-performance microprocessors containing copper interconnects and low-k materials. We observed void movement along the top copper/dielectric (SiNx) interface which is found to be the main pathway for electromigration-induced atomic copper transport.

  12. 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. PMID:22349401

  13. 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.

  14. 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.

  15. 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.

  16. Signal-to-noise and radiation exposure considerations in conventional and diffraction x-ray microscopy

    DOE PAGES

    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 imagesmore » using fewer photons. As a result, this can be an important advantage for studying radiation-sensitive biological and soft matter specimens.« less

  17. 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.

  18. Laser Plasma Soft X-Ray Contact Microscopy of Polymer Composites

    NASA Astrophysics Data System (ADS)

    Azuma, Hirozumi; Takeichi, Akihiro; Noda, Shoji

    1994-08-01

    Microstructures of polymer composites are observed with a good contrast and with a submicron spatial resolution by contact soft X-ray microscopy with a laser plasma as a soft X-ray source. An iron target was irradiated by a YAG laser ( 2ω=532 nm, 0.4 J) at laser power density of 2.5×1012 W/cm2 and the emitted soft X-rays were filtered with a thin aluminum foil. For a 0.1-µ m-thick poly acrylonitrile-butadiene-styrene specimen, poly-butadiene or copolymer of butadiene spheres of about 500 nm diameter, which are selectively stained with osmium, is observed with soft X-rays in the wavelength region between 17 and 20 nm. For a 4-µ m-thick polyvinyl chloride film specimen formed by polymer powder compaction, peripheral areas of holes, grain boundaries, and areas probably degraded by HCl reduction are observed with soft X-rays in the wavelength region mainly around 2 nm.

  19. 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.

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

    DOE PAGES

    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.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

  1. 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.

  2. 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. PMID:26074579

  3. 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

  4. 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

  5. In-situ scanning transmission X-ray microscopy of catalytic solids and related nanomaterials.

    PubMed

    de Groot, Frank M F; de Smit, Emiel; van Schooneveld, Matti M; Aramburo, Luis R; Weckhuysen, Bert M

    2010-04-01

    The present status of in-situ scanning transmission X-ray microscopy (STXM) is reviewed, with an emphasis on the abilities of the STXM technique in comparison with electron microscopy. The experimental aspects and interpretation of X-ray absorption spectroscopy (XAS) are briefly introduced and the experimental boundary conditions that determine the potential applications for in-situ XAS and in-situ STXM studies are discussed. Nanoscale chemical imaging of catalysts under working conditions is outlined using cobalt and iron Fischer-Tropsch catalysts as showcases. In the discussion, we critically compare STXM-XAS and STEM-EELS (scanning transmission electron microscopy-electron energy loss spectroscopy) measurements and indicate some future directions of in-situ nanoscale imaging of catalytic solids and related nanomaterials.

  6. Multimodal imaging of human cerebellum - merging X-ray phase microtomography, magnetic resonance microscopy and histology

    NASA Astrophysics Data System (ADS)

    Schulz, Georg; Waschkies, Conny; Pfeiffer, Franz; Zanette, Irene; Weitkamp, Timm; David, Christian; Müller, Bert

    2012-11-01

    Imaging modalities including magnetic resonance imaging and X-ray computed tomography are established methods in daily clinical diagnosis of human brain. Clinical equipment does not provide sufficient spatial resolution to obtain morphological information on the cellular level, essential for applying minimally or non-invasive surgical interventions. Therefore, generic data with lateral sub-micrometer resolution have been generated from histological slices post mortem. Sub-cellular spatial resolution, lost in the third dimension as a result of sectioning, is obtained using magnetic resonance microscopy and micro computed tomography. We demonstrate that for human cerebellum grating-based X-ray phase tomography shows complementary contrast to magnetic resonance microscopy and histology. In this study, the contrast-to-noise values of magnetic resonance microscopy and phase tomography were comparable whereas the spatial resolution in phase tomography is an order of magnitude better. The registered data with their complementary information permit the distinct segmentation of tissues within the human cerebellum.

  7. Structural characterisation of Ni clusters in AlN via X-ray absorption, X-ray diffraction and transmission electron microscopy

    NASA Astrophysics Data System (ADS)

    Zanghi, D.; Traverse, A.; Dallas, J.-P.; Snoeck, E.

    Ni ions were implanted in bulk AlN with the goal to form embedded metallic clusters. Combining several characterisation techniques such as X-ray absorption spectroscopy, X-ray diffraction and high resolution transmission electron microscopy, we determined the lattice parameter of the Ni clusters that display a fcc crystalline structure. The average size increases when the ion fluence is increased or after a thermal treatment. Thanks to moiré fringes observed by high resolution transmission electron microscopy and to satellite peaks seen on the diffraction patterns, we concluded that the annealed Ni clusters orientate their (002) planes on the (101) of AlN. Moreover, the satellite positions allowed us to calculate Ni cluster average diameters, that are in agreement with average sizes deduced by X-ray absorption spectroscopy.

  8. Imaging interfacial micro- and nano-bubbles by scanning transmission soft X-ray microscopy.

    PubMed

    Zhang, Lijuan; Zhao, Binyu; Xue, Lian; Guo, Zhi; Dong, Yaming; Fang, Haiping; Tai, Renzhong; Hu, Jun

    2013-05-01

    Synchrotron-based scanning transmission soft X-ray microscopy (STXM) with nanometer resolution was used to investigate the existence and behavior of interfacial gas nanobubbles confined between two silicon nitride windows. The observed nanobubbles of SF6 and Ne with diameters smaller than 2.5 µm were quite stable. However, larger bubbles became unstable and grew during the soft X-ray imaging, indicating that stable nanobubbles may have a length scale, which is consistent with a previous report using atomic force microscopy [Zhang et al. (2010), Soft Matter, 6, 4515-4519]. Here, it is shown that STXM is a promising technique for studying the aggregation of gases near the solid/water interfaces at the nanometer scale.

  9. X-ray photoemission electron microscopy, a tool for the investigation of complex magnetic structures.

    SciTech Connect

    Scholl, Andreas; Ohldag, Hendrik; Nolting, Frithjof; Stohr, Joachim; Padmore, Howard A.

    2001-08-30

    X-ray Photoemission Electron Microscopy unites the chemical specificity and magnetic sensitivity of soft x-ray absorption techniques with the high spatial resolution of electron microscopy. The discussed instrument possesses a spatial resolution of better than 50 nm and is located at a bending magnet beamline at the Advanced Light Source, providing linearly and circularly polarized radiation between 250 and 1300 eV. We will present examples which demonstrate the power of this technique applied to problems in the field of thin film magnetism. The chemical and elemental specificity is of particular importance for the study of magnetic exchange coupling because it allows separating the signal of the different layers and interfaces in complex multi-layered structures.

  10. Apparatus for X-ray diffraction microscopy and tomography of cryo specimens

    DOE PAGES

    Beetz, T.; Howells, M. R.; Jacobsen, C.; Kao, C. -C.; Kirz, J.; Lima, E.; Mentes, T. O.; Miao, H.; Sanchez-Hanke, C.; Sayre, D.; et al

    2005-03-14

    An apparatus for diffraction microscopy of biological and materials science specimens is described. In this system, a coherent soft X-ray beam is selected with a pinhole, and the illuminated specimen is followed by an adjustable beamstop and CCD camera to record diffraction data from non-crystalline specimens. In addition, a Fresnel zone plate can be inserted to allow for direct imaging. The system makes use of a cryogenic specimen holder with cryotransfer capabilities to allow frozen hydrated specimens to be loaded. The specimen can be tilted over a range of ± 80 ° degrees for three-dimensional imaging; this is done bymore » computer-controlled motors, enabling automated alignment of the specimen through a tilt series. The system is now in use for experiments in soft X-ray diffraction microscopy.« less

  11. Apparatus for X-ray diffraction microscopy and tomography of cryo specimens

    SciTech Connect

    Beetz, T.; Howells, M. R.; Jacobsen, C.; Kao, C. -C.; Kirz, J.; Lima, E.; Mentes, T. O.; Miao, H.; Sanchez-Hanke, C.; Sayre, D.; Shapiro, D.

    2005-03-14

    An apparatus for diffraction microscopy of biological and materials science specimens is described. In this system, a coherent soft X-ray beam is selected with a pinhole, and the illuminated specimen is followed by an adjustable beamstop and CCD camera to record diffraction data from non-crystalline specimens. In addition, a Fresnel zone plate can be inserted to allow for direct imaging. The system makes use of a cryogenic specimen holder with cryotransfer capabilities to allow frozen hydrated specimens to be loaded. The specimen can be tilted over a range of ± 80 ° degrees for three-dimensional imaging; this is done by computer-controlled motors, enabling automated alignment of the specimen through a tilt series. The system is now in use for experiments in soft X-ray diffraction microscopy.

  12. 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

  13. Simultaneous cryo X-ray ptychographic and fluorescence microscopy of green algae

    SciTech Connect

    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.

  14. Simultaneous cryo X-ray ptychographic and fluorescence microscopy of green algae

    DOE PAGES

    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 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. This combined approach offers a way to study the role of trace elements in their structural context.« less

  15. Correlative VIS-fluorescence and soft X-ray cryo-microscopy/tomography of adherent cells.

    PubMed

    Hagen, Christoph; Guttmann, Peter; Klupp, Barbara; Werner, Stephan; Rehbein, Stefan; Mettenleiter, Thomas C; Schneider, Gerd; Grünewald, Kay

    2012-02-01

    Soft X-ray cryo-microscopy/tomography of vitreous samples is becoming a valuable tool in structural cell biology. Within the 'water-window' wavelength region (2.34-4.37nm), 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

  16. 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

  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. Scanning transmission x-ray microscopy as a novel tool to probe colloidal and photonic crystals.

    PubMed

    van Schooneveld, Matti M; Hilhorst, Jan; Petukhov, Andrei V; Tyliszczak, Tolek; Wang, Jian; Weckhuysen, Bert M; de Groot, Frank M F; de Smit, Emiel

    2011-03-21

    Photonic crystals consisting of nano- to micrometer-sized building blocks, such as multiple sorts of colloids, have recently received widespread attention. It remains a challenge, however, to adequately probe the internal crystal structure and the corresponding deformations that inhibit the proper functioning of such materials. It is shown that scanning transmission X-ray microscopy (STXM) can directly reveal the local structure, orientations, and even deformations in polystyrene and silica colloidal crystals with 30-nm spatial resolution. Moreover, STXM is capable of imaging a diverse range of crystals, including those that are dry and inverted, and provides novel insights complementary to information obtained by benchmark confocal fluorescence and scanning electron microscopy techniques.

  19. Depth-resolved soft x-ray photoelectron emission microscopy in nanostructures via standing-wave excited photoemission

    SciTech Connect

    Kronast, F.; Ovsyannikov, R.; Kaiser, A.; Wiemann, C.; Yang, S.-H.; Locatelli, A.; Burgler, D.E.; Schreiber, R.; Salmassi, F.; Fischer, P.; Durr, H.A.; Schneider, C.M.; Eberhardt, W.; Fadley, C.S.

    2008-11-24

    We present an extension of conventional laterally resolved soft x-ray photoelectron emission microscopy. A depth resolution along the surface normal down to a few {angstrom} can be achieved by setting up standing x-ray wave fields in a multilayer substrate. The sample is an Ag/Co/Au trilayer, whose first layer has a wedge profile, grown on a Si/MoSi2 multilayer mirror. Tuning the incident x-ray to the mirror Bragg angle we set up standing x-ray wave fields. We demonstrate the resulting depth resolution by imaging the standing wave fields as they move through the trilayer wedge structure.

  20. Phase retrieval in x-ray coherent Fresnel projection-geometry diffraction

    SciTech Connect

    De Caro, Liberato; Giannini, Cinzia; Cedola, Alessia; Pelliccia, Daniele; Lagomarsino, Stefano; Jark, Werner

    2007-01-22

    Coherent x-ray diffraction experiments were performed in Fresnel regime, within a line-projection geometry. A planar x-ray waveguide was used to focus coherent cylindrical waves onto a 7.2 {mu}m Kevlar fiber, which acts as a phase object for hard x rays. The phase was retrieved, by using a Fourier-based iterative phasing algorithm, consistent with measured diffraction data and known constraints in real space, with a submicrometer spatial resolution.

  1. Real-time X-ray transmission microscopy of solidifying Al-In alloys

    SciTech Connect

    Curreri, P.A.; Kaukler, W.F.

    1996-03-01

    Real-time observations of transparent analog materials have provided insight, yet the results of these observations are not necessarily representative of opaque metallic systems. In order to study the detailed dynamics of the solidification process, the authors develop the technologies needed for real-time X-ray microscopy of solidifying metallic systems, which has not previously been feasible with the necessary resolution, speed, and contrast. In initial studies of Al-In monotectic alloys unidirectionally solidified in an X-ray transparent furnace, in situ records of the evolution of interface morphologies, interfacial solute accumulation, and formation of the monotectic droplets were obtained for the first time: a radiomicrograph of Al-30In grown during aircraft parabolic maneuvers is presented, showing the volumetric phase distribution in this specimen. The benefits of using X-ray microscopy for postsolidification metallography include ease of specimen preparation, increased sensitivity, and three-dimensional analysis of phase distribution. Imaging of the solute boundary layer revealed that the isoconcentration lines are not parallel (as is often assumed) to the growth interface. Striations in the solidified crystal did not accurately decorate the interface position and shape. The monotectic composition alloy under some conditions grew in an uncoupled manner.

  2. Imaging nanoscale lattice variations by machine learning of x-ray diffraction microscopy data

    DOE PAGES

    Laanait, Nouamane; Zhang, Zhan; Schlepütz, Christian M.

    2016-08-09

    In this paper, 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 datamore » 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. Finally, 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.« less

  3. Real-Time X-Ray Transmission Microscopy of Solidifying Al-In Alloys

    NASA Technical Reports Server (NTRS)

    Curreri, Peter A.; Kaukler, William F.

    1997-01-01

    Real-time observations of transparent analog materials have provided insight, yet the results of these observations are not necessarily representative of opaque metallic systems. In order to study the detailed dynamics of the solidification process, we develop the technologies needed for real-time X ray microscopy of solidifying metallic systems, which has not previously been feasible with the necessary resolution, speed, and contrast. In initial studies of Al-In monotectic alloys unidirectionally solidified in an X-ray transparent furnace, in situ records of the evolution of interface morphologies, interfacial solute accumulation, and formation of the monotectic droplets were obtained for the first time: A radiomicrograph of Al-30In grown during aircraft parabolic maneuvers is presented, showing the volumetric phase distribution in this specimen. The benefits of using X-ray microscopy for postsolidification metallography include ease of specimen preparation, increased sensitivity, and three-dimensional analysis of phase distribution. Imaging of the solute boundary layer revealed that the isoconcentration lines are not parallel (as is often assumed) to the growth interface. Striations in the solidified crystal did not accurately decorate the interface position and shape. The monotectic composition alloy under some conditions grew in an uncoupled manner.

  4. Polarization dependent soft x-ray spectro-microscopy of local spin structures

    NASA Astrophysics Data System (ADS)

    Robertson, Maccallum; Agostino, Christopher; Im, Mi-Young; Montoya, Sergio; Fullerton, Eric; Fischer, Peter

    Quantitative information about element-specific contributions to local magnetic spin and orbital moments is readily available by XMCD spectroscopy and images of magnetic domain patterns with a few tens of nanometer spatial resolution. We show that the x-ray spectroscopic analysis of x-ray microscopy images provides quantitative information about local spin structures. We have investigated two prototypical multilayered PMA film systems prepared by sputtering, specifically (Co 0.3 nm/Pt 0.5 nm)x30 and (Fe 0.7nm/Gd 0.4nm)x100 systems. A spectroscopic sequence of full-field magnetic transmission soft x-ray microscopy (MTXM) images covering about 8mm field-of-views with a spatial resolution of about 20nm were recorded across the Co and Fe L edges, resp. To modulate the magnetic contrast, two sets of images were obtained with left and right circular polarization. Standard XMCD spectroscopy analysis procedures were applied to retrieve the local spectroscopic behavior. We observe a decrease of the L3/L2 ratio when approaching the domain walls, indicating a non-uniform spin configuration along the vertical profile of a domain, which we will discuss in view of both systems' magnetic anisotropies. U.S. DOE under Contract No. DE-AC02-05-CH11231.

  5. The Measurement of MTFs in X-ray Microscopy Using Diffractograms

    SciTech Connect

    Morrison, G. R.; Charalambous, P. S.; Gianoncelli, A.; Kaulich, B.

    2011-09-09

    A novel method to characterize the optical performance of a high-resolution transmission x-ray microscope is presented. It makes use of test patterns that consist of random arrays of sub-resolution holes in a thin metal film, and so approximate to white-noise input signals for the microscope. The test patterns have been fabricated by electron-beam lithography at length scales appropriate for the resolution available in x-ray microscopy, so that diffractograms produced from the image data can be directly interpreted in terms of the contrast transfer function of the optical system. Results of this method are shown for both brightfield and differential phase contrast imaging.

  6. Elemental and magnetic sensitive imaging using x-ray excited luminescence microscopy

    SciTech Connect

    Rosenberg, R. A.; Zohar, S.; Keavney, D.; Divan, R.; Rosenmann, D.; Mascarenhas, A.; Steiner, M. A.

    2012-07-15

    We demonstrate the potential of x-ray excited luminescence microscopy for full-field elemental and magnetic sensitive imaging using a commercially available optical microscope, mounted on preexisting synchrotron radiation (SR) beamline end stations. The principal components of the instrument will be described. Bench top measurements indicate that a resolution of 1 {mu}m or better is possible; this value was degraded in practice due to vibrations and/or drift in the end station and associated manipulator. X-ray energy dependent measurements performed on model solar cell materials and lithographically patterned magnetic thin film structures reveal clear elemental and magnetic signatures. The merits of the apparatus will be discussed in terms of conventional SR imaging techniques.

  7. Study of radiation effects on the cell structure and evaluation of the dose delivered by x-ray and {alpha}-particles microscopy

    SciTech Connect

    Kosior, Ewelina; Cloetens, Peter; Deves, Guillaume; Ortega, Richard; Bohic, Sylvain

    2012-12-24

    Hard X-ray fluorescence microscopy and magnified phase contrast imaging are combined to study radiation effects on cells. Experiments were performed on freeze-dried cells at the nano-imaging station ID22NI of the European synchrotron radiation facility. Quantitative phase contrast imaging provides maps of the projected mass and is used to evaluate the structural changes due to irradiation during X-ray fluorescence experiments. Complementary to phase contrast imaging, scanning transmission ion microscopy is performed and doses of all the experiments are compared. We demonstrate the sensitivity of the proposed approach to study radiation-induced damage at the sub-cellular level.

  8. X-Ray Diffraction Project Final Report, Fiscal Year 2006

    SciTech Connect

    Dane V. Morgan

    2006-10-01

    An x-ray diffraction diagnostic system was developed for determining real-time shock-driven lattice parameter shifts in single crystals at the gas gun at TA-IV at Sandia National Laboratories (SNL). The signal-to-noise ratio and resolution of the system were measured using imaging plates as the detector and by varying the slit width. This report includes tests of the x-ray diffraction system using a phosphor coupled to a charge-coupled device (CCD) camera by a coherent fiber-optic bundle. The system timing delay was measured with a newly installed transistor-transistor logic (TTL) bypass designed to reduce the x-ray delay time. The axial misalignment of the Bragg planes was determined with respect to the optical axis for a set of eight LiF [lithium fluoride] crystals provided by SNL to determine their suitability for gas gun experiments.

  9. An environmental sample chamber for reliable scanning transmission x-ray microscopy measurements under water vapor.

    PubMed

    Kelly, Stephen T; Nigge, Pascal; Prakash, Shruti; Laskin, Alexander; Wang, Bingbing; Tyliszczak, Tolek; Leone, Stephen R; Gilles, Mary K

    2013-07-01

    We have designed, fabricated, and tested a compact gas-phase reactor for performing in situ soft x-ray scanning transmission x-ray microscopy (STXM) measurements. The reactor mounts directly to the existing sample holder used in the majority of STXM instruments around the world and installs with minimal instrument reconfiguration. The reactor accommodates many gas atmospheres, but was designed specifically to address the needs of measurements under water vapor. An on-board sensor measures the relative humidity and temperature inside the reactor, minimizing uncertainties associated with measuring these quantities outside the instrument. The reactor reduces x-ray absorption from the process gas by over 85% compared to analogous experiments with the entire STXM instrument filled with process gas. Reduced absorption by the process gas allows data collection at full instrumental resolution, minimizes radiation dose to the sample, and results in much more stable imaging conditions. The reactor is in use at the STXM instruments at beamlines 11.0.2 and 5.3.2.2 at the Advanced Light Source.

  10. An environmental sample chamber for reliable scanning transmission x-ray microscopy measurements under water vapor

    NASA Astrophysics Data System (ADS)

    Kelly, Stephen T.; Nigge, Pascal; Prakash, Shruti; Laskin, Alexander; Wang, Bingbing; Tyliszczak, Tolek; Leone, Stephen R.; Gilles, Mary K.

    2013-07-01

    We have designed, fabricated, and tested a compact gas-phase reactor for performing in situ soft x-ray scanning transmission x-ray microscopy (STXM) measurements. The reactor mounts directly to the existing sample holder used in the majority of STXM instruments around the world and installs with minimal instrument reconfiguration. The reactor accommodates many gas atmospheres, but was designed specifically to address the needs of measurements under water vapor. An on-board sensor measures the relative humidity and temperature inside the reactor, minimizing uncertainties associated with measuring these quantities outside the instrument. The reactor reduces x-ray absorption from the process gas by over 85% compared to analogous experiments with the entire STXM instrument filled with process gas. Reduced absorption by the process gas allows data collection at full instrumental resolution, minimizes radiation dose to the sample, and results in much more stable imaging conditions. The reactor is in use at the STXM instruments at beamlines 11.0.2 and 5.3.2.2 at the Advanced Light Source.

  11. Simulation of image formation in x-ray coded aperture microscopy with polycapillary optics.

    PubMed

    Korecki, P; Roszczynialski, T P; Sowa, K M

    2015-04-01

    In x-ray coded aperture microscopy with polycapillary optics (XCAMPO), the microstructure of focusing polycapillary optics is used as a coded aperture and enables depth-resolved x-ray imaging at a resolution better than the focal spot dimensions. Improvements in the resolution and development of 3D encoding procedures require a simulation model that can predict the outcome of XCAMPO experiments. In this work we introduce a model of image formation in XCAMPO which enables calculation of XCAMPO datasets for arbitrary positions of the object relative to the focal plane as well as to incorporate optics imperfections. In the model, the exit surface of the optics is treated as a micro-structured x-ray source that illuminates a periodic object. This makes it possible to express the intensity of XCAMPO images as a convolution series and to perform simulations by means of fast Fourier transforms. For non-periodic objects, the model can be applied by enforcing artificial periodicity and setting the spatial period larger then the field-of-view. Simulations are verified by comparison with experimental data.

  12. Simultaneous x-ray nano-ptychographic and fluorescence microscopy at the bionanoprobe

    NASA Astrophysics Data System (ADS)

    Chen, S.; Deng, J.; Vine, D. J.; Nashed, Y. S. G.; Jin, Q.; Peterka, T.; Jacobsen, C.; Vogt, S.

    2015-09-01

    Hard X-ray fluorescence (XRF) microscopy offers unparalleled sensitivity for quantitative analysis of most of the trace elements in biological samples, such as Fe, Cu, and Zn. These trace elements play critical roles in many biological processes. With the advanced nano-focusing optics, nowadays hard X-rays can be focused down to 30 nm or below and can probe trace elements within subcellular compartments. However, XRF imaging does not usually reveal much information on ultrastructure, because the main constituents of biomaterials, i.e. H, C, N, and O, have low fluorescence yield and little absorption contrast at multi-keV X-ray energies. An alternative technique for imaging ultrastructure is ptychography. One can record far-field diffraction patterns from a coherently illuminated sample, and then reconstruct the complex transmission function of the sample. In theory the spatial resolution of ptychography can reach the wavelength limit. In this manuscript, we will describe the implementation of ptychography at the Bionanoprobe (a recently developed hard XRF nanoprobe at the Advanced Photon Source) and demonstrate simultaneous ptychographic and XRF imaging of frozen-hydrated biological whole cells. This method allows locating trace elements within the subcellular structures of biological samples with high spatial resolution. Additionally, both ptychographic and XRF imaging are compatible with tomographic approach for 3D visualization.

  13. Transmission x-ray microscopy at Diamond-Manchester I13 Imaging Branchline

    NASA Astrophysics Data System (ADS)

    Vila-Comamala, Joan; Bosgra, Jeroen; Eastwood, David S.; Wagner, Ulrich; Bodey, Andrew J.; Garcia-Fernandez, Miryam; David, Christian; Rau, Christoph

    2016-01-01

    Full-field Transmission X-ray Microscopy (TXM) has been shown to be a powerful method for obtaining quantitative internal structural and chemical information from materials at the nanoscale. The installation of a Full-field TXM station will extend the current microtomographic capabilities of the Diamond-Manchester I13 Imaging Branchline at Diamond Light Source (UK) into the sub-100 nm spatial resolution range using photon energies from 8 to 14 keV. The dedicated Full-field TXM station will be built in-house with contributions of Diamond Light Source support divisions and via collaboration with the X-ray Optics Group of Paul Scherrer Institut (Switzerland) which will develop state-of-the-art diffractive X-ray optical elements. Preliminary results of the I13 Full-field TXM station are shown. The Full-field TXM will become an important Diamond Light Source direct imaging asset for material science, energy science and biology at the nanoscale.

  14. Dynamical X-ray Microscopy Study of Stress-Induced Voiding in Cu Interconnects

    NASA Astrophysics Data System (ADS)

    Heim, S.; Friedrich, D.; Guttmann, P.; Rehbein, S.; Chumakov, D.; Ritz, Y.; Schneider, G.; Schmeisser, D.; Zschech, E.

    2009-06-01

    High-resolution x-ray imaging with a spatial resolution in the 20 nm range offers unique capabilities for process development in semiconductor industry. Buried copper on-chip interconnect structures can be studied with excellent element specific contrast. In addition, it is possible to obtain 3-D views of fully embedded copper interconnect lines and vias. Moreover, transmission x-ray microscopy (TXM) is a very suitable technique to study dynamical, reliability-limiting processes like electromigration (EM) or stress-induced voiding (SIV). Stress-induced void formation is investigated in dual damascene Cu/SiOx and Cu/low-k interconnect stacks. The initial pre-stressing of the about 1.5 μm thick focused ion beam(FIB)-prepared cross-sections was performed by heating at a temperature of 175° C for 50 hours. Subsequently, a series of x-ray images was recorded using images after every five hours of heating at the same temperature. The dynamical SIV experiments show for the first time directly that voids are formed and grown further underneath the via.

  15. Three-dimensional full-field X-ray orientation microscopy

    PubMed Central

    Viganò, Nicola; Tanguy, Alexandre; Hallais, Simon; Dimanov, Alexandre; Bornert, Michel; Batenburg, Kees Joost; Ludwig, Wolfgang

    2016-01-01

    A previously introduced mathematical framework for full-field X-ray orientation microscopy is for the first time applied to experimental near-field diffraction data acquired from a polycrystalline sample. Grain by grain tomographic reconstructions using convex optimization and prior knowledge are carried out in a six-dimensional representation of position-orientation space, used for modelling the inverse problem of X-ray orientation imaging. From the 6D reconstruction output we derive 3D orientation maps, which are then assembled into a common sample volume. The obtained 3D orientation map is compared to an EBSD surface map and local misorientations, as well as remaining discrepancies in grain boundary positions are quantified. The new approach replaces the single orientation reconstruction scheme behind X-ray diffraction contrast tomography and extends the applicability of this diffraction imaging technique to material micro-structures exhibiting sub-grains and/or intra-granular orientation spreads of up to a few degrees. As demonstrated on textured sub-regions of the sample, the new framework can be extended to operate on experimental raw data, thereby bypassing the concept of orientation indexation based on diffraction spot peak positions. This new method enables fast, three-dimensional characterization with isotropic spatial resolution, suitable for time-lapse observations of grain microstructures evolving as a function of applied strain or temperature. PMID:26868303

  16. Biological x-ray microscopy: from biochemical mapping to lensless imaging

    NASA Astrophysics Data System (ADS)

    Jacobsen, Chris

    2005-03-01

    Cell structure has been very succesfully studied using light and electron microscopy. However, x rays ofer new insights, by imaging whole cells at 20-40 nm resolution using zone plate lenses, and in particular by combining this with spectroscopic sensitivity to organic functional groups. While spectra of single compounds can provide exquisite information on electronic states, a cell is much more complex. Pattern recognition algorithms provide a way to deal with this complexity and obtain insights into biochemical organization at a fine spatial scale, as illustrated in an ongoing study of the correlation of morphology with biochemical content in sperm. Another approach to biological imaging is to abandon the use of lenses and their resolution limits. The purest form of measurement is to collect x rays scattered by a cell with no optics-imposed losses. By using iterative phasing algorithms, this diffraction data can be phased to deliver a real-space image of a complex cell (at present, 30 nm resolution in studies of freeze-dried yeast) with a possible ultimate extension to atomic resolution imaging of proteins using x-ray free electron lasers.

  17. Optimization of the soft x-ray transmission microscopy beamline at the ALBA light source

    NASA Astrophysics Data System (ADS)

    Sorrentino, Andrea; Pereiro, Eva; Valcárcel, Ricardo; Ferrer, Salvador; Nicolas, Josep

    2013-09-01

    Mistral is the soft X-ray full field microscopy beamline at the ALBA light source. The beamline is designed to have large source acceptance and to provide constant magnification at the exit slit for photon energies between 270 and 2600 eV. The monochromator is a variation of the Petersen plane grating monochromator in which a variable line spacing grating is used to maintain the beam focused at the exit slit, independently of the fixed focus constant, and to cancel aberrations. We present the alignment strategy used to compensate errors of the optical elements, and report about the commissioning results.

  18. Schottky barrier measurements on individual GaAs nanowires by X-ray photoemission microscopy

    NASA Astrophysics Data System (ADS)

    di Mario, Lorenzo; Turchini, Stefano; Zamborlini, Giovanni; Feyer, Vitaly; Tian, Lin; Schneider, Claus M.; Rubini, Silvia; Martelli, Faustino

    2016-11-01

    We present measurements of the Schottky barrier height on individual GaAs nanowires by means of x-ray photoelectron emission microscopy (XPEEM). Values of 0.73 and 0.51 eV, averaged over the entire wires, were measured on Cu-covered n-doped and p-doped GaAs nanowires, respectively, in agreement with results obtained on bulk material. Our measurements show that XPEEM can become a feasible and reliable investigation tool of interface formation at the nanoscale and pave the way towards the study of size-dependent effects on semiconductor-based structures.

  19. Microscopy and elemental analysis in tissue samples using computed microtomography with synchrotron x-rays

    SciTech Connect

    Spanne, P.; Rivers, M.L.

    1988-01-01

    The initial development shows that CMT using synchrotron x-rays can be developed to ..mu..m spatial resolution and perhaps even better. This creates a new microscopy technique which is of special interest in morphological studies of tissues, since no chemical preparation or slicing of the sample is necessary. The combination of CMT with spatial resolution in the ..mu..m range and elemental mapping with sensitivity in the ppM range results in a new tool for elemental mapping at the cellular level. 7 refs., 1 fig.

  20. Hard x-ray microscopy with Fresnel zone plates reaches 40 nm Rayleigh resolution.

    SciTech Connect

    Chu, Y. S.; De Carlo, F.; Shen, Q.; Lee, W.K.; Wu, H.J.; Wang, C.L.; Wang, J.Y.; Liu, C.J.; Wang, C.H.; Wu, S.R.; Chien, C.C.; Hwu, Y.; Tkachuk, A.; Yun, W.; Feser, M.; Liang, K.S.; Yang, C.S.; Je, J.H.; Margaritondo, G.; X-Ray Science Division; Academia Sinica; National Tsing Hua Univ.; National Taiwan Ocean Univ.; National Synchrotron Radiation Research Center; Xradia, Inc.; National Health Research Inst.; Ecole Polytechnique Federale de Lausanne; Pohang Univ.

    2008-03-10

    Substantial improvements in the nanofabrication and characteristics of gold Fresnel zone plates yielded unprecedented resolution levels in hard-x-ray microscopy. Tests performed on a variety of specimens with 8-10 keV photons demonstrated a first-order lateral resolution below 40 nm based on the Rayleigh criterion. Combined with the use of a phase contrast technique, this makes it possible to view features in the 30 nm range; good-quality images can be obtained at video rate, down to 50 ms/frame. The important repercussions on materials science, nanotechnology, and the life sciences are discussed.

  1. Hard-x-ray microscopy with Fresnel zone plates reaches 40 nm Rayleigh resolution

    SciTech Connect

    Chu, Y. S.; Yi, J. M.; De Carlo, F.; Shen, Q.; Lee, Wah-Keat; Wu, H. J.; Wang, C. L.; Wang, J. Y.; Liu, C. J.; Wang, C. H.; Wu, S. R.; Chien, C. C.; Hwu, Y.; Tkachuk, A.; Yun, W.; Feser, M.; Liang, K. S.; Yang, C. S.; Je, J. H.; Margaritondo, G.

    2008-03-10

    Substantial improvements in the nanofabrication and characteristics of gold Fresnel zone plates yielded unprecedented resolution levels in hard-x-ray microscopy. Tests performed on a variety of specimens with 8-10 keV photons demonstrated a first-order lateral resolution below 40 nm based on the Rayleigh criterion. Combined with the use of a phase contrast technique, this makes it possible to view features in the 30 nm range; good-quality images can be obtained at video rate, down to 50 ms/frame. The important repercussions on materials science, nanotechnology, and the life sciences are discussed.

  2. Correlative Light and Scanning X-Ray Scattering Microscopy of Healthy and Pathologic Human Bone Sections

    PubMed Central

    Giannini, C.; Siliqi, D.; Bunk, O.; Beraudi, A.; Ladisa, M.; Altamura, D.; Stea, S.; Baruffaldi, F.

    2012-01-01

    Scanning small and wide angle X-ray scattering (scanning SWAXS) experiments were performed on healthy and pathologic human bone sections. Via crystallographic tools the data were transformed into quantitative images and as such compared with circularly polarized light (CPL) microscopy images. SWAXS and CPL images allowed extracting information of the mineral nanocrystalline phase embedded, with and without preferred orientation, in the collagen fibrils, mapping local changes at sub-osteon resolution. This favorable combination has been applied for the first time to biopsies of dwarfism syndrome and Paget's disease to shed light onto the cortical structure of natural bone in healthy and pathologic sections. PMID:22666538

  3. Dark-field X-ray microscopy for multiscale structural characterization

    PubMed Central

    Simons, H.; King, A.; Ludwig, W.; Detlefs, C.; Pantleon, W.; Schmidt, S.; Snigireva, I.; Snigirev, A.; Poulsen, H. F.

    2015-01-01

    Many physical and mechanical properties of crystalline materials depend strongly on their internal structure, which is typically organized into grains and domains on several length scales. Here we present dark-field X-ray microscopy; a non-destructive microscopy technique for the three-dimensional mapping of orientations and stresses on lengths scales from 100 nm to 1 mm within embedded sampling volumes. The technique, which allows ‘zooming’ in and out in both direct and angular space, is demonstrated by an annealing study of plastically deformed aluminium. Facilitating the direct study of the interactions between crystalline elements is a key step towards the formulation and validation of multiscale models that account for the entire heterogeneity of a material. Furthermore, dark-field X-ray microscopy is well suited to applied topics, where the structural evolution of internal nanoscale elements (for example, positioned at interfaces) is crucial to the performance and lifetime of macro-scale devices and components thereof. PMID:25586429

  4. 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

  5. Scanning transmission X-ray microscopy and X-ray absorption near-edge structure studies of N-doped carbon nanotubes sealed with N2 gas

    NASA Astrophysics Data System (ADS)

    Xie, Tian; Zhao, Yu; Zhong, Jun; Hu, Zheng; Sun, Xuhui

    2012-06-01

    N-doped carbon nanotubes (NCNTs) were synthesized and their electronic structures have been explored by X-ray absorption near-edge structure (XANES) spectroscopy. With a surface sensitive mode, XANES confirms the N-doping in NCNTs. However, with a more bulk sensitive detection mode of XANES, large amount of gaseous N2 have been found to be sealed in NCNTs, even in a high vacuum environment. The encapsulation of the ferrocene residues in carbon nanotubes had been revealed by scanning transmission X-ray microscopy (STXM), which may help for the N2 sealing. The results suggest that the easily sealed gas should be taken into consideration for CNT-based applications.

  6. Composition analysis of a polymer electrolyte membrane fuel cell microporous layer using scanning transmission X-ray microscopy and near edge X-ray absorption fine structure analysis

    NASA Astrophysics Data System (ADS)

    George, Michael G.; Wang, Jian; Banerjee, Rupak; Bazylak, Aimy

    2016-03-01

    The novel application of scanning transmission X-ray microscopy (STXM) to the microporous layer (MPL) of a polymer electrolyte membrane fuel cell is investigated. A spatially resolved chemical component distribution map is obtained for the MPL of a commercially available SGL 25 BC sample. This is achieved with near edge X-ray absorption fine structure spectroscopic analysis. Prior to analysis the sample is embedded in non-reactive epoxy and ultra-microtomed to a thickness of 100 nm. Polytetrafluoroethylene (PTFE), carbon particle agglomerates, and supporting epoxy resin distributions are identified and reconstructed for a scanning area of 6 μm × 6 μm. It is observed that the spatial distribution of PTFE is strongly correlated to the carbon particle agglomerations. Additionally, agglomerate structures of PTFE are identified, possibly indicating the presence of a unique mesostructure in the MPL. STXM analysis is presented as a useful technique for the investigation of chemical species distributions in the MPL.

  7. Study of hard disk and slider surfaces using X-ray photoemission electron microscopy and near-edge X-ray absorption fine structure spectroscopy

    SciTech Connect

    Anders, S.; Stammler, T.; Bhatia, C.S.; Fong, W.; Chen, C.Y.; Bogy, D.B.

    1998-04-01

    X-ray Photo Emission Electron Microscopy (X-PEEM) and Near Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy were applied to study the properties of amorphous hard carbon overcoats on disks and sliders, and the properties of the lubricant. The modification of lubricants after performing thermal desorption studies was measured by NEXAFS, and the results are compared to the thermal desorption data. The study of lubricant degradation in wear tracks is described. Sliders were investigated before and after wear test, and the modification of the slider coating as well as the transfer of lubricant to the slider was studied. The studies show that the lubricant is altered chemically during the wear. Fluorine is removed and carboxyl groups are formed.

  8. Real-Time X-Ray transmission microscopy of solidifying Al-In Alloys

    NASA Astrophysics Data System (ADS)

    Curreri, Peter A.; Kaukler, William F.

    1996-03-01

    Real-time observations of transparent analog materials have provided insight, yet the results of these observations are not necessarily representative of opaque metallic systems. In order to study the detailed dynamics of the solidification process, we develop the technologies needed for real-time Xray microscopy of solidifying metallic systems, which has not previously been feasible with the necessary resolution, speed, and contrast. In initial studies of Al-ln monotectic alloys unidirectionally solidified in an X-ray transparent furnace, in situ records of the evolution of interface morphologies, interfacial solute accumulation, and formation of the monotectic droplets were obtained for the first time: A radiomicrograph of Al-30In grown during aircraft parabolic maneuvers is presented, showing the volumetric phase distribution in this specimen. The benefits of using X-ray microscopy for postsolidification metallography include ease of specimen preparation, increased sensitivity, and three-dimensional analysis of phase distribution. Imaging of the solute boundary layer revealed that the isoconcentration lines are not parallel (as is often assumed) to the growth interface. Striations in the solidified crystal did not accurately decorate the interface position and shape. The monotectic composition alloy under some conditions grew in an uncoupled manner.

  9. Nanoscale imaging of buried topological defects with quantitative X-ray magnetic microscopy.

    PubMed

    Blanco-Roldán, C; Quirós, C; Sorrentino, A; Hierro-Rodríguez, A; Álvarez-Prado, L M; Valcárcel, R; Duch, M; Torras, N; Esteve, J; Martín, J I; Vélez, M; Alameda, J M; Pereiro, E; Ferrer, S

    2015-09-04

    Advances in nanoscale magnetism increasingly require characterization tools providing detailed descriptions of magnetic configurations. Magnetic transmission X-ray microscopy produces element specific magnetic domain images with nanometric lateral resolution in films up to ∼100 nm thick. Here we present an imaging method using the angular dependence of magnetic contrast in a series of high resolution transmission X-ray microscopy images to obtain quantitative descriptions of the magnetization (canting angles relative to surface normal and sense). This method is applied to 55-120 nm thick ferromagnetic NdCo5 layers (canting angles between 65° and 22°), and to a NdCo5 film covered with permalloy. Interestingly, permalloy induces a 43° rotation of Co magnetization towards surface normal. Our method allows identifying complex topological defects (merons or ½ skyrmions) in a NdCo5 film that are only partially replicated by the permalloy overlayer. These results open possibilities for the characterization of deeply buried magnetic topological defects, nanostructures and devices.

  10. Nanoscale imaging of buried topological defects with quantitative X-ray magnetic microscopy

    PubMed Central

    Blanco-Roldán, C.; Quirós, C.; Sorrentino, A.; Hierro-Rodríguez, A.; Álvarez-Prado, L. M.; Valcárcel, R.; Duch, M.; Torras, N.; Esteve, J.; Martín, J. I.; Vélez, M.; Alameda, J. M.; Pereiro, E.; Ferrer, S.

    2015-01-01

    Advances in nanoscale magnetism increasingly require characterization tools providing detailed descriptions of magnetic configurations. Magnetic transmission X-ray microscopy produces element specific magnetic domain images with nanometric lateral resolution in films up to ∼100 nm thick. Here we present an imaging method using the angular dependence of magnetic contrast in a series of high resolution transmission X-ray microscopy images to obtain quantitative descriptions of the magnetization (canting angles relative to surface normal and sense). This method is applied to 55–120 nm thick ferromagnetic NdCo5 layers (canting angles between 65° and 22°), and to a NdCo5 film covered with permalloy. Interestingly, permalloy induces a 43° rotation of Co magnetization towards surface normal. Our method allows identifying complex topological defects (merons or ½ skyrmions) in a NdCo5 film that are only partially replicated by the permalloy overlayer. These results open possibilities for the characterization of deeply buried magnetic topological defects, nanostructures and devices. PMID:26337838

  11. Advancement of Solidification Processing Technology Through Real Time X-Ray Transmission Microscopy: Sample Preparation

    NASA Technical Reports Server (NTRS)

    Stefanescu, D. M.; Curreri, P. A.

    1996-01-01

    Two types of samples were prepared for the real time X-ray transmission microscopy (XTM) characterization. In the first series directional solidification experiments were carried out to evaluate the critical velocity of engulfment of zirconia particles in the Al and Al-Ni eutectic matrix under ground (l-g) conditions. The particle distribution in the samples was recorded on video before and after the samples were directionally solidified. In the second series samples of the above two type of composites were prepared for directional solidification runs to be carried out on the Advanced Gradient Heating Facility (AGHF) aboard the space shuttle during the LMS mission in June 1996. X-ray microscopy proved to be an invaluable tool for characterizing the particle distribution in the metal matrix samples. This kind of analysis helped in determining accurately the critical velocity of engulfment of ceramic particles by the melt interface in the opaque metal matrix composites. The quality of the cast samples with respect to porosity and instrumented thermocouple sheath breakage or shift could be easily viewed and thus helped in selecting samples for the space shuttle experiments. Summarizing the merits of this technique it can be stated that this technique enabled the use of cast metal matrix composite samples since the particle location was known prior to the experiment.

  12. 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.

  13. 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.

  14. Refractive optical elements and optical system for high energy x-ray microscopy

    SciTech Connect

    Simon, M.; Altapova, V.; Baumbach, T.; Kluge, M.; Last, A.; Marschall, F.; Mohr, J.; Nazmov, V.; Vogt, H.

    2012-05-17

    In material science, X-ray radiation with photon energies above 25 keV is used because of its penetration into high density materials. Research of the inner structure of novel materials, such as electrodes in high power batteries for engines, require X-ray microscopes operating in the hard X-ray energy range. A flexible X-ray microscope for hard X-rays with photon energies higher than 25 keV will be realized at the synchrotron source ANKA in Karlsruhe, Germany. The device will use refractive X-ray lenses as condenser as well as objective lenses.

  15. PREFACE: 11th International Conference on X-ray Microscopy (XRM2012)

    NASA Astrophysics Data System (ADS)

    Xu, Hongjie; Wu, Ziyu; Tai, Renzhong

    2013-10-01

    The Eleventh International Conference on X-ray Microscopy (XRM2012) was held on 5-10 August 2012 at the Hope hotel in Shanghai. Historically, for the first time the XRM conference took place in China. The conference was jointly hosted by the Shanghai Synchrotron Radiation Facility (SSRF) and the National Synchrotron Radiation Laboratory (NSRL). The series of XRM conferences dates back to 1983 in Göttingen, Germany. Since the Zürich conference, XRM2008, it has been held every two years, showing its increasing popularity among the x-ray microscopy communities around the world. Research in the area of x-ray microscopy is advancing very fast with the development of synchrotron radiation techniques, especially the emergence of third generation light sources with low natural emittance which has significantly pushed forward the development of technologies and applications in this area. This has been fully demonstrated in presentations from this and previous XRM conferences. XRM2012 was attended by 295 people including 21 invited speakers, 53 contributing speakers, 55 students, and 13 industry exhibitors. Over 232 abstracts were submitted for oral or poster presentation and 56 original, peer-reviewed papers are published in these proceedings. The conference was sponsored by the Chinese Academy of Sciences (CAS) and the National Natural Science Foundation of China (11210301016/A0802), and three gold sponsors active in industrial and technological fields related to x-ray microscopy. An exhibition booth was offered free to Australia synchrotron, the host for XRM2014, to promote the next conference which will be held in Melbourne, Australia in 2014. An unforgettable memory for most conference participants might be the charming night cruise along Pujiang river which was part of the welcome reception on the first evening. The Werner Meyer-Ilse Award (WMIA) prize this year was awarded to Irene Zanette (TU-München) and Stephan Werner (HZB-Berlin), the former for her pioneering

  16. The SPARX Project: R & D Activity Towards X-Rays FEL Sources

    SciTech Connect

    Alesini, D.; Bellaveglia, M.; Bertolucci, S.; Biagini, M.E.; Boni, R.; Boscolo, M.; Castellano, M.; Clozza, A.; Di Pirro, G.; Drago, A.; Esposito, A.; Ferrario, M.; Filippetto, D.; Fusco, V.; Gallo, A.; Ghigo, A.; Guiducci, S.; Incurvati, M.; Ligi, C.; Marcellini, F.; Migliorati, M.; /Frascati /ENEA, Frascati /INFN, Milan /INFN, Rome /INFN, Rome2 /Milan Polytechnic /UCLA /SLAC

    2005-08-05

    SPARX is an evolutionary project proposed by a collaboration among ENEA-INFN-CNR-Universita di Roma Tor Vergata aiming at the construction of a FELSASE X-ray source in the Tor Vergata Campus. The first phase of the SPARX project, funded by Government Agencies, will be focused on R&D activity on critical components and techniques for future X-ray facilities as described in this paper.

  17. High-resolution dichroic imaging of magnetic flux distributions in superconductors with scanning x-ray microscopy

    SciTech Connect

    Ruoß, S. Stahl, C.; Weigand, M.; Schütz, G.; Albrecht, J.

    2015-01-12

    The penetration of magnetic flux into high-temperature superconductors has been observed using a high-resolution technique based on x-ray magnetic circular dichroism. Superconductors coated with thin soft-magnetic layers are observed in a scanning x-ray microscope under the influence of external magnetic fields. Resulting electric currents in the superconductor create an inhomogeneous magnetic field distribution above the superconductor and lead to a local reorientation of the ferromagnetic layer. Measuring the local magnetization of the ferromagnet by x-ray absorption microscopy with circular-polarized radiation allows the analysis of the magnetic flux distribution in the superconductor with a spatial resolution on the nanoscale.

  18. High resolution transmission soft X-ray microscopy of deterioration products developed in large concrete dams

    PubMed

    Kurtis; Monteiro; Brown; Meyer-Ilse

    1999-12-01

    In concrete structures, the reaction of certain siliceous aggregates with the highly alkaline concrete pore solution produces an alkali-silicate gel that can absorb water and expand. This reaction can lead to expansion, cracking, increased permeability, and decreased strength of the concrete. Massive concrete structures, such as dams, are particularly susceptible to the damage caused by the alkali-silica reaction because of the availability of water and because massive gravity dams usually do not contain steel reinforcement to restrain the expansion. Both the cement hydration products and alkali-silica reaction products are extremely sensitive to humidity. Consequently, characterization techniques that require high vacuum or drying, as many existing techniques do, are not particularly appropriate for the study of the alkali-silica reaction because artefacts are introduced. Environmental scanning electron micrographs and scanning electron micrographs with energy dispersive X-ray analysis results demonstrate the effect of drying on the morphology and chemical composition of the alkali-silicate reaction gel. Thus, the impetus for this research was the need to observe and characterize the alkali-silica reaction and its gel product on a microscopic level in a wet environment (i.e. without introducing artefacts due to drying). Only soft X-ray transmission microscopy provides the required high spatial resolution needed to observe the reaction process in situ. The alkali-silica reaction can be observed over time, in a wet condition, and at normal pressures, features unavailable with most other high resolution techniques. Soft X-rays also reveal information on the internal structure of the sample. The purpose of this paper is to present research, obtained using transmission soft X-ray microscopy, on the effect of concrete pore solution cations, namely sodium and calcium, on the product formed as a result of alkali attack. Alkali-silicate reaction (ASR) gel was obtained from

  19. X-ray microscopy for in situ characterization of 3D nanostructural evolution in the laboratory

    NASA Astrophysics Data System (ADS)

    Hornberger, Benjamin; Bale, Hrishikesh; Merkle, Arno; Feser, Michael; Harris, William; Etchin, Sergey; Leibowitz, Marty; Qiu, Wei; Tkachuk, Andrei; Gu, Allen; Bradley, Robert S.; Lu, Xuekun; Withers, Philip J.; Clarke, Amy; Henderson, Kevin; Cordes, Nikolaus; Patterson, Brian M.

    2015-09-01

    X-ray microscopy (XRM) has emerged as a powerful technique that reveals 3D images and quantitative information of interior structures. XRM executed both in the laboratory and at the synchrotron have demonstrated critical analysis and materials characterization on meso-, micro-, and nanoscales, with spatial resolution down to 50 nm in laboratory systems. The non-destructive nature of X-rays has made the technique widely appealing, with potential for "4D" characterization, delivering 3D micro- and nanostructural information on the same sample as a function of sequential processing or experimental conditions. Understanding volumetric and nanostructural changes, such as solid deformation, pore evolution, and crack propagation are fundamental to understanding how materials form, deform, and perform. We will present recent instrumentation developments in laboratory based XRM including a novel in situ nanomechanical testing stage. These developments bridge the gap between existing in situ stages for micro scale XRM, and SEM/TEM techniques that offer nanometer resolution but are limited to analysis of surfaces or extremely thin samples whose behavior is strongly influenced by surface effects. Several applications will be presented including 3D-characterization and in situ mechanical testing of polymers, metal alloys, composites and biomaterials. They span multiple length scales from the micro- to the nanoscale and different mechanical testing modes such as compression, indentation and tension.

  20. Lithographically-fabricated channel arrays for confocal x-ray fluorescence microscopy and XAFS

    NASA Astrophysics Data System (ADS)

    Woll, Arthur R.; Agyeman-Budu, David; Choudhury, Sanjukta; Coulthard, Ian; Finnefrock, Adam C.; Gordon, Robert; Hallin, Emil; Mass, Jennifer

    2014-03-01

    Confocal X-ray Fluorescence Microscopy (CXRF) employs overlapping focal regions of two x-ray optics—a condenser and collector—to directly probe a 3D volume. The minimum-achievable size of this probe volume is limited by the collector, for which polycapillaries are generally the optic of choice. Recently, we demonstrated an alternative collection optic for CXRF, consisting of an array of micron-scale collimating channels, etched in silicon, and arranged like spokes of a wheel directed towards a single source position. The optic, while successful, had a working distance of only 0.2 mm and exhibited relatively low total collection efficiency, limiting its practical application. Here, we describe a new design in which the collimating channels are formed by a staggered array of pillars whose side-walls taper away from the channel axis. This approach improves both collection efficiency and working distance, while maintaining excellent spatial resolution. We illustrate these improvements with confocal XRF data obtained at the Cornell High Energy Synchrotron Source (CHESS) and the Advanced Photon Source (APS) beamline 20-ID-B.

  1. Objective for EUV microscopy, EUV lithography, and x-ray imaging

    DOEpatents

    Bitter, Manfred; Hill, Kenneth W.; Efthimion, Philip

    2016-05-03

    Disclosed is an imaging apparatus for EUV spectroscopy, EUV microscopy, EUV lithography, and x-ray imaging. This new imaging apparatus could, in particular, make significant contributions to EUV lithography at wavelengths in the range from 10 to 15 nm, which is presently being developed for the manufacturing of the next-generation integrated circuits. The disclosure provides a novel adjustable imaging apparatus that allows for the production of stigmatic images in x-ray imaging, EUV imaging, and EUVL. The imaging apparatus of the present invention incorporates additional properties compared to previously described objectives. The use of a pair of spherical reflectors containing a concave and convex arrangement has been applied to a EUV imaging system to allow for the image and optics to all be placed on the same side of a vacuum chamber. Additionally, the two spherical reflector segments previously described have been replaced by two full spheres or, more precisely, two spherical annuli, so that the total photon throughput is largely increased. Finally, the range of permissible Bragg angles and possible magnifications of the objective has been largely increased.

  2. 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.

  3. Magnetic soft X-ray microscopy at 10nm spatial resolution

    NASA Astrophysics Data System (ADS)

    Fischer, Peter; Chao, Weilun; Im, Mi-Young; Anderson, Erik

    2011-03-01

    Magnetic soft X-ray microscopy, which combines high spatial and temporal resolution with elemental specificity by utilizing the specific features of X-ray magnetic circular dichroism effects is a unique and powerful analytical technique to image fast spin dynamics of nanoscale magnetism. The spatial resolution is determined by Fresnel zone plate lenses used as diffractive optics. FZPs are fabricated by state-of-the-art lithography techniques and the challenge is to produce a dense, circular line pattern with a high aspect ratio to achieve high efficiency. Using an overlay technique [2-3], which requires high position accuracy of the e-beam writer, FZPs with 12nm outermost zone width could be fabricated. Implementing this optic at BL 6.1.2 at the ALS in Berkeley CA, we have demonstrated that a 10nm line and space test pattern can be clearly resolved. First magnetic images of a PtCo film with a pronounced perpendicular anisotropy will be presented. Further progress to below 10nm can be anticipated in the near future. This work was supported by the U.S. Department of Energy under Contract No. DE-AC02-05-CH11231.

  4. 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.

  5. Implementation of soft x-ray microscopy with several tens nanometers spatial resolution at NSRL

    NASA Astrophysics Data System (ADS)

    Jiang, Shiping; Chen, Liang

    2009-09-01

    A transmission soft x-ray microscope (TXM), which is similar to the full-field x-ray microscopes installed on other synchrotron radiation sources in the world, was developed at National Synchrotron Radiation Laboratory (NSRL) in Hefei. An x-ray image taken with the microscope was acquired and its spatial resolution was estimated to be better than 70nm.

  6. 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.

  7. Conical foil x-ray mirrors: performance and projections.

    PubMed

    Serlemitsos, P J

    1988-04-15

    For the past decade, we have been developing at Goddard conical grazing incidence mirrors in an effort to increase the sensitivity and resolution of astronomical observations in the iron K spectral band around 7 keV. Tightly packed conical foils give us the option of trading some imaging capability for light weight, large throughput, and low cost, all crucial requirements at the higher energies where grazing angles become very small. Nearing the completion of the broad band x-ray telescope for NASA's SHEAL II mission, we have decided important design and fabrication issues including reflector substrate material and supports and most techniques for reflector preparation, mirror assembly, and alignment. We will review the design, fabrication, status, and performance of our present mirrors. Future applications along with prospects for improved spatial resolution for these mirrors will be discussed. PMID:20531595

  8. Lateral spin transfer torque induced magnetic switching at room temperature demonstrated by x-ray microscopy.

    PubMed

    Buhl, M; Erbe, A; Grebing, J; Wintz, S; Raabe, J; Fassbender, J

    2013-01-01

    Changing and detecting the orientation of nanomagnetic structures, which can be used for durable information storage, needs to be developed towards true nanoscale dimensions for keeping up the miniaturization speed of modern nanoelectronic components. Therefore, new concepts for controlling the state of nanomagnets are currently in the focus of research in the field of nanoelectronics. Here, we demonstrate reproducible switching of a purely metallic nanopillar placed on a lead that conducts a spin-polarized current at room temperature. Spin diffusion across the metal-metal (Cu to CoFe) interface between the pillar and the lead causes spin accumulation in the pillar, which may then be used to set the magnetic orientation of the pillar. In our experiments, the detection of the magnetic state of the nanopillar is performed by direct imaging via scanning transmission x-ray microscopy (STXM).

  9. Lateral spin transfer torque induced magnetic switching at room temperature demonstrated by x-ray microscopy

    PubMed Central

    Buhl, M.; Erbe, A.; Grebing, J.; Wintz, S.; Raabe, J.; Fassbender, J.

    2013-01-01

    Changing and detecting the orientation of nanomagnetic structures, which can be used for durable information storage, needs to be developed towards true nanoscale dimensions for keeping up the miniaturization speed of modern nanoelectronic components. Therefore, new concepts for controlling the state of nanomagnets are currently in the focus of research in the field of nanoelectronics. Here, we demonstrate reproducible switching of a purely metallic nanopillar placed on a lead that conducts a spin-polarized current at room temperature. Spin diffusion across the metal-metal (Cu to CoFe) interface between the pillar and the lead causes spin accumulation in the pillar, which may then be used to set the magnetic orientation of the pillar. In our experiments, the detection of the magnetic state of the nanopillar is performed by direct imaging via scanning transmission x-ray microscopy (STXM). PMID:24126435

  10. Structural characterization of colloidal crystals and inverse opals using transmission X-ray microscopy.

    PubMed

    Huang, Bo-Han; Wang, Chun-Chieh; Liao, Chen-Hong; Wu, Pu-Wei; Song, Yen-Fang

    2014-07-15

    A nondestructive tomographic technique was used to determine the crystallographic information of colloidal crystals comprising of polystyrene (PS) microspheres, as well as their silver inverse opals. The properties of the colloidal crystals, such as defects, grain size, grain boundaries, stacking sequence, and grain orientation, were determined using the full field transmission X-ray microscopy (TXM) with a spatial resolution of 50 nm. The PS microspheres (500-750 nm) which underwent a vertical electrophoresis process to form a face-centered cubic (fcc) close-packed structure with an ABCABC packing sequence. In addition, the colloidal crystal exhibited multiple grains, and an orientation variation of 6.1° in the stacking direction between two neighboring grains. PMID:24863783

  11. Transmission X-ray microscopy (TXM) reveals the nanostructure of a smectite gel.

    PubMed

    Zbik, Marek S; Martens, Wayde N; Frost, Ray L; Song, Yen-Fang; Chen, Yi-Ming; Chen, Jian-Hua

    2008-08-19

    The unusual behavior of smectites, the ability to change volume when wetted (swelling) or dried (shrinking), makes soil rich in smectites very unstable and dangerous for the building industry because of the movement of building foundations and poor slope stability. These macroscopic properties are dominated by the structural arrangement of the smectites' finest fraction. Here, we show in three dimensions how the swelling phenomenon in smectite, caused by a combination of hydratation and electrostatic forces, may expand the dry smectite volume not 10-fold, as previously thought, but to more than 1000-fold. A new technique, transmission X-ray microscopy, makes it possible to investigate the internal structure and 3-D tomographic reconstruction of clay aggregates. This reveals, for the first time, the smectite gel arrangement in the voluminous cellular tactoid structure within a natural aqueous environment. PMID:18620443

  12. Observation of thermomagnetically recorded domains with high-resolution magnetic soft x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Tsunashima, S.; Takagi, Nayuki; Yamaguchi, Atushi; Kume, Minoru; Fischer, P.; Kumazawa, M.

    2003-04-01

    Magnetic domains were thermomagnetically recorded on TbFeCo films using laser pulsed magnetic field modulation (LP-MFM) and light intensity modulation (LIM). The domains were observed with high resolution magnetic transmission X-ray microscopy (M-TXM) before and after the heat treatment in order to clarify the recording characteristics and the thermal stability of recorded domains. From the results of M-TXM images, it was found that isolated single marks whose lengths are much smaller than 100 nm can be recorded by LP-MFM but their mark lengths become often longer than designed. It was further confirmed that the heat treatment at 120 degree C for 50 hours does not influence significantly the crescent-shaped magnetic domains of 100 nm in width recorded using LP-MFM method and circular domains of 150 nm in diameter recorded using LIM method.

  13. Terminal contact elements of insect attachment devices studied by transmission X-ray microscopy.

    PubMed

    Eimüller, T; Guttmann, P; Gorb, S N

    2008-06-01

    For the first time, the terminal elements (spatulae) of setal (hairy) attachment devices of the beetle Gastrophysa viridula (Coleoptera, Chrysomelidae) and the fly Lucilia caesar (Diptera, Calliphoridae) were studied using transmission X-ray microscopy (TXM) with a lateral resolution of about 30 nm. Since images are taken under ambient conditions, we demonstrate here that this method can be applied to study the contact behaviour of biological systems, including animal tenent setae, in a fresh state. We observed that the attached spatulae show a viscoelastic behavior increasing the contact area and providing improved adaptability to the local topography of the surface. The technique can be extended to TXM tomography, which would provide three-dimensional information and a deeper insight into the details of insect attachment structures. PMID:18515726

  14. Transmission X-ray microscopy reveals the clay aggregate discrete structure in aqueous environment.

    PubMed

    Zbik, Marek S; Frost, Ray L; Song, Yen-Fang; Chen, Yi-Ming; Chen, Jian-Hua

    2008-03-15

    The utilization of new transmission X-ray microscopy (TXM) using the synchrotron photon source enable for the first time the study in three dimensions microsize clay particles in aggregates in their natural aqueous environment. This technique makes possible remarkable accurate images of nanosize mineral interparticle structure which forms a new nanocomposite. The Birdwood kaolinite/LDH aggregates observed in the TXM are much more compact than observed before in pure Birdwood kaolinite suspension and similar to aggregates formed after treatment by positively charged surfactant. Kaolinite/LDH aggregates in water reveal complex structure of larger kaolinite platelets connected together by gelled nanoparticles which are most probably LDH colloidal plates. Comparisons of the transmission electron microscope (TEM) and TXM techniques show similarities in particle morphology. The ability to study particles and aggregates in their natural aqueous environment and in 3-dimensions make this technique superior to the TEM technique. PMID:18187142

  15. Quantitative X-Ray Magnetic Microscopy: from parallel stripe domains to buried topological defects

    NASA Astrophysics Data System (ADS)

    Velez, Maria; Blanco-Roldan, C.; Quiros, C.; Valdes-Bango, F.; Alvarez-Prado, L. M.; Martin, J. I.; Alameda, J. M.; Hierro-Rodriguez, A.; Duch, M.; Torras, N.; Esteve, J.; Sorrentino, A.; Valcarcel, R.; Pereiro, E.; Ferrer, S.

    Magnetic transmission X-ray microscopy (TXM) is a powerful imaging technique that can produce element specific images of magnetic domains with nanometric lateral resolution. Here we present a novel imaging method in which the angular dependence of the magnetic contrast in a series of high resolution TXM images is used to obtain quantitative descriptions of the magnetization (canting angles and sense). This has been applied first to analyze parallel stripe domains in weak perpendicular anisotropy ferromagnetic NdCo5 layers of different thickness, and in NdCo5/Permalloy bilayers. Then, our method has been used to identify complex topological defects (merons or 1/2 skyrmions) in a NdCo5 film that are only partially replicated by the Permalloy overlayer. Meron propagation in trilayers (across the thickness) and in hexagonal networks (across bifurcations) will be discussed in terms of their topological characteristics (chirality and polarity). Work supported by Spanish Grant FIS2013-45469.

  16. Structural characterization of colloidal crystals and inverse opals using transmission X-ray microscopy.

    PubMed

    Huang, Bo-Han; Wang, Chun-Chieh; Liao, Chen-Hong; Wu, Pu-Wei; Song, Yen-Fang

    2014-07-15

    A nondestructive tomographic technique was used to determine the crystallographic information of colloidal crystals comprising of polystyrene (PS) microspheres, as well as their silver inverse opals. The properties of the colloidal crystals, such as defects, grain size, grain boundaries, stacking sequence, and grain orientation, were determined using the full field transmission X-ray microscopy (TXM) with a spatial resolution of 50 nm. The PS microspheres (500-750 nm) which underwent a vertical electrophoresis process to form a face-centered cubic (fcc) close-packed structure with an ABCABC packing sequence. In addition, the colloidal crystal exhibited multiple grains, and an orientation variation of 6.1° in the stacking direction between two neighboring grains.

  17. Data preparation and evaluation techniques for x-ray diffraction microscopy

    DOE PAGES

    Steinbrener, Jan; Nelson, Johanna; Huang, Xiaojing; Marchesini, Stefano; Shapiro, David; Turner, Joshua J.; Jacobsen, Chris

    2010-01-01

    The post-experiment processing of X-ray Diffraction Microscopy data is often time-consuming and difficult. This is mostly due to the fact that even if a preliminary result has been reconstructed, there is no definitive answer as to whether or not a better result with more consistently retrieved phases can still be obtained. In addition, we show here that the first step in data analysis, the assembly of two-dimensional diffraction patterns from a large set of raw diffraction data, is crucial to obtaining reconstructions of highest possible consistency. We have developed software that automates this process and results in consistently accurate diffractionmore » patterns. We have furthermore derived some criteria of validity for a tool commonly used to assess the consistency of reconstructions, the phase retrieval transfer function, and suggest a modified version that has improved utility for judging reconstruction quality.« less

  18. Characterization of X-ray polycapillary optics by LiF crystal radiation detectors through confocal fluorescence microscopy

    NASA Astrophysics Data System (ADS)

    Bonfigli, Francesca; Hampai, Dariush; Dabagov, Sultan B.; Montereali, Rosa Maria

    2016-08-01

    Solid-state radiation imaging detectors based on photoluminescent colour centres in lithium fluoride (LiF) crystals have been successfully tested for both advanced 2D and 3D characterizations of X-ray polycapillary optics by a table-top laboratory system. Polycapillary optics can control X-ray beams propagation and allows obtaining quasi-parallel beam (half-lens) or focused beams (full-lens). The combination of a fine-focused micro X-ray tube and a polycapillary lens can provide the high intensity radiation fluxes that are necessary for high resolution X-ray imaging. In this paper we present novel results about advanced characterization of these complex optics by 2D as well as 3D confocal laser fluorescence microscopy of X-ray irradiated LiF crystal detectors. Two dimensional high spatial resolution images on a wide field of view of transmitted X-rays through a semi-lens and 3D direct inspection of the coloured volumes produced in LiF crystals by both focused and parallel X-ray beam transmitted by a full and a semi-lens, respectively, as well as their 3D reconstructions were obtained. The results show that the photoluminescent colour centres volume in LiF crystals combined with an optical sectioning reading system provide information about tomography of transmitted X-ray beams by policapillary optics in a single exposure process. For the first time, the use of LiF crystal plates as versatile radiation imaging luminescent detectors have been used to characterize the operation of polycapillary optics as X-ray lens, in focusing and parallel mode.

  19. High-resolution and large-volume tomography reconstruction for x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Cheng, Chang-Chieh; Hwu, Yeukuang; Ching, Yu-Tai

    2016-03-01

    This paper presents a method of X-ray image acquisition for the high-resolution tomography reconstruction that uses a light source of synchrotron radiation to reconstruct a three-dimensional tomographic volume dataset for a nanoscale object. For large objects, because of the limited field-of-view, a projection image of an object should to be taken by several shots from different locations, and using an image stitching method to combine these image blocks together. In this study, the overlap of image blocks should be small because our light source is the synchrotron radiation and the X-ray dosage should be minimized as possible. We use the properties of synchrotron radiation to enable the image stitching and alignment success when the overlaps between adjacent image blocks are small. In this study, the size of overlaps can reach to 15% of the size of each image block. During the reconstruction, the mechanical stability should be considered because it leads the misalignment problem in tomography. We adopt the feature-based alignment

  20. Characterization of polymer monoliths containing embedded nanoparticles by scanning transmission X-ray microscopy (STXM).

    PubMed

    Arrua, R Dario; Hitchcock, Adam P; Hon, Wei Boon; West, Marcia; Hilder, Emily F

    2014-03-18

    The structural and chemical homogeneity of monolithic columns is a key parameter for high efficiency stationary phases in liquid chromatography. Improved characterization techniques are needed to better understand the polymer morphology and its optimization. Here the analysis of polymer monoliths by scanning transmission X-ray microscopy (STXM) is presented for the first time. Poly(butyl methacrylate-co-ethyleneglycoldimethacrylate) [poly(BuMA-co-EDMA)] monoliths containing encapsulated divinylbenzene (DVB) nanoparticles were characterized by STXM, which gives a comprehensive, quantitative chemical analysis of the monolith at a spatial resolution of 30 nm. The results are compared with other methods commonly used for the characterization of polymer monoliths [scanning electron microscopy (SEM), transmission electron microscopy (TEM), mercury porosimetry, and nitrogen adsorption]. The technique permitted chemical identification and mapping of the nanoparticles within the polymeric scaffold. Residual surfactant, which was used during the manufacture of the nanoparticles, was also detected. We show that STXM can give more in-depth chemical information for these types of materials and therefore lead to a better understanding of the link between polymer morphology and chromatographic performance.

  1. Characterization of polymer monoliths containing embedded nanoparticles by scanning transmission X-ray microscopy (STXM).

    PubMed

    Arrua, R Dario; Hitchcock, Adam P; Hon, Wei Boon; West, Marcia; Hilder, Emily F

    2014-03-18

    The structural and chemical homogeneity of monolithic columns is a key parameter for high efficiency stationary phases in liquid chromatography. Improved characterization techniques are needed to better understand the polymer morphology and its optimization. Here the analysis of polymer monoliths by scanning transmission X-ray microscopy (STXM) is presented for the first time. Poly(butyl methacrylate-co-ethyleneglycoldimethacrylate) [poly(BuMA-co-EDMA)] monoliths containing encapsulated divinylbenzene (DVB) nanoparticles were characterized by STXM, which gives a comprehensive, quantitative chemical analysis of the monolith at a spatial resolution of 30 nm. The results are compared with other methods commonly used for the characterization of polymer monoliths [scanning electron microscopy (SEM), transmission electron microscopy (TEM), mercury porosimetry, and nitrogen adsorption]. The technique permitted chemical identification and mapping of the nanoparticles within the polymeric scaffold. Residual surfactant, which was used during the manufacture of the nanoparticles, was also detected. We show that STXM can give more in-depth chemical information for these types of materials and therefore lead to a better understanding of the link between polymer morphology and chromatographic performance. PMID:24552424

  2. Seven years with the Swift Supergiant Fast X-ray Transients project

    NASA Astrophysics Data System (ADS)

    Romano, P.

    2015-09-01

    Supergiant Fast X-ray Transients (SFXTs) are HMXBs with OB supergiant companions. I review the results of the Swift SFXT project, which since 2007 has been exploiting Swift's capabilities in a systematic study of SFXTs and supergiant X-ray binaries (SGXBs) by combining follow-ups of outbursts, when detailed broad-band spectroscopy is possible, with long-term monitoring campaigns, when the out-of-outburst fainter states can be observed. This strategy has led us to measure their duty cycles as a function of luminosity, to extract their differential luminosity distributions in the soft X-ray domain, and to compare, with unprecedented detail, the X-ray variability in these different classes of sources. I also discuss the "seventh year crisis", the challenges that the recent Swift observations are making to the prevailing models attempting to explain the SFXT behavior.

  3. Analytic 3D imaging of mammalian nucleus at nanoscale using coherent x-rays and optical fluorescence microscopy.

    PubMed

    Song, Changyong; Takagi, Masatoshi; Park, Jaehyun; Xu, Rui; Gallagher-Jones, Marcus; Imamoto, Naoko; Ishikawa, Tetsuya

    2014-09-01

    Despite the notable progress that has been made with nano-bio imaging probes, quantitative nanoscale imaging of multistructured specimens such as mammalian cells remains challenging due to their inherent structural complexity. Here, we successfully performed three-dimensional (3D) imaging of mammalian nuclei by combining coherent x-ray diffraction microscopy, explicitly visualizing nuclear substructures at several tens of nanometer resolution, and optical fluorescence microscopy, cross confirming the substructures with immunostaining. This demonstrates the successful application of coherent x-rays to obtain the 3D ultrastructure of mammalian nuclei and establishes a solid route to nanoscale imaging of complex specimens.

  4. Qualitative detection of single submicron and nanoparticles in human skin by scanning transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Graf, Christina; Meinke, Martina; Gao, Qi; Hadam, Sabrina; Raabe, Jörg; Sterry, Wolfram; Blume-Peytavi, Ulrike; Lademann, Jürgen; Rühl, Eckart; Vogt, Annika

    2009-03-01

    First results on single particle detection in human skin samples by x-ray microscopy are reported. 94+/-6 and 161+/-13 nm gold core particles with silica shells and 298+/-11 nm silica particles coated with a gold shell on ultramicrotome sections of human skin were determined. The particles were applied on fresh intact skin samples, which were sectioned prior to imaging. After screening the sections by conventional microscopy techniques, defined areas of interest were qualitatively investigated by scanning transmission x-ray microscopy at the Swiss Light Source. In studies on the percutaneous penetration of 161+/-13 nm particles on human skin samples, x-ray microscopy yielded high-resolution images of single particles spreading on the superficial layer of the stratum corneum and on the epithelium in superficial parts of hair follicles. No deeper penetration was observed. The present work using x-ray microscopy provides the unique opportunity to study qualitative penetration processes and membrane-particle interactions on the level of single particles. This goes beyond present approaches using optical microscopy. Further improvement of this approach will allow one to study particles with different physicochemical properties and surface modifications, including responses of the exposed tissue.

  5. Recent investigations of silk fibers utilizing x-ray scattering and atomic force microscopy

    NASA Astrophysics Data System (ADS)

    Miller, Lance D.

    1998-12-01

    Silks from the mulberry silkworm, Bombyx mori, and the golden-orb spider, Nephila clavipes, are materials that possess respectable properties. Even pitted against the high performance fibers of Kevlar, polyethylene, and carbon, the advantages of some of nature's fibers are clear. The tensile strength of the golden-orb spider dragline is of the same order of magnitude as many synthetic fibers, yet the dragline's compressive strength as a percentage of its tensile strength is greater. The spider's ampullate glands, responsible for the manufacture of the dragline, also excel. The spider spins its fiber from a liquid crystalline solution that is water based versus the solutions at high temperatures containing volatile solvents that are required for current synthetic fibers. Understanding the morphology of silks will provide the basis for improved manufacturing and better performing synthetic fibers. The studies presented here have centered on the use of small-angle x-ray scattering, SAXS, to describe the large-scale morphology of silk fibers. We have determined minimum scattering dimensions on the order of 150-300 nm. A detailed analysis of the Porod scattering region has revealed correlation lengths of the same magnitude. Both of these dimensions are similar to with direct atomic force microscopy, AFM, measurements of nanofibers found in samples of abraded or peeled silk. The incorporation of discrete Fourier transform theory and AFM topographic information has yielded results in general agreement with measured SAXS patterns. This incorporation allows the materials scientist a way of visualizing the relationship between a material and its resulting scattering function. We have also found that x-ray scattering gives insight to new periodic distances of the morphology of golden-orb dragline. All of these studies yield a more complete view of the silk morphology and give a new method of model building from scattering experiments.

  6. Development of in-line furnace for in-situ nanoscale resolution x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Eng, Christopher; Chen-Wiegart, Yu-Chen K.; Wang, Jun

    2013-09-01

    Full field transmission x-ray microscopy (TXM) is a newly developed x-ray imaging technique to provide quantitative and non-destructive 3D characterization of the complex microstructure of materials at nanometer resolution. A key missing component is an in situ apparatus enabling the imaging of the complex structural evolution of the materials and to correlate the structural change with a material's functionality under real operating conditions. This work describes the design of an environmental cell which satisfies the requirements for in situ TXM studies. The limited space within the TXM presents a spatial constraint which prohibits the use of conventional heaters, as well as requiring consideration in designing for safe and controlled operation of the system and alignment of the cell with the beam. A gravity drip-fed water cooling jacket was installed in place around the heating module to maintain critical components of the microscope at safe operating temperatures. A motion control system consisting of pulse width modulated DC motor driven XYZ translation stages was developed to facilitate fine alignment of the cell. Temperature of the sample can be controlled remotely and accurately through a controller to temperatures as high as 1200 K. Heating zone measurement was carried out and shows a 500 x 500 x 500 μm3 homogeneous zone volume for sample area, which is a critical parameter to ensure accurate observation of structural evolution at nanometer scale with a sample in size of tens of microns. Application on Ni particles for in situ oxidation experiment and dehydrogenation of aluminum hydride is also discussed.

  7. Probing platinum degradation in polymer electrolyte membrane fuel cells by synchrotron X-ray microscopy.

    PubMed

    Berejnov, Viatcheslav; Martin, Zulima; West, Marcia; Kundu, Sumit; Bessarabov, Dmitri; Stumper, Jürgen; Susac, Darija; Hitchcock, Adam P

    2012-04-14

    Synchrotron-based scanning transmission X-ray spectromicroscopy (STXM) was used to characterize the local chemical environment at and around the platinum particles in the membrane (PTIM) which form in operationally tested (end-of-life, EOL) catalyst coated membranes (CCMs) of polymer electrolyte membrane fuel cells (PEM-FC). The band of metallic Pt particles in operationally tested CCM membranes was imaged using transmission electron microscopy (TEM). The cathode catalyst layer in the beginning-of-life (BOL) CCMs was fabricated using commercially available catalysts created from Pt precursors with and without nitrogen containing ligands. The surface composition of these catalyst powders was measured by X-ray Photoelectron Spectroscopy (XPS). The local chemical environment of the PTIM in EOL CCMs was found to be directly related to the Pt precursor used in CCM fabrication. STXM chemical mapping at the N 1s edge revealed a characteristic spectrum at and around the dendritic Pt particles in CCMs fabricated with nitrogen containing Pt-precursors. This N 1s spectrum was identical to that of the cathode and different from the membrane. For CCM samples fabricated without nitrogen containing Pt-precursors the N 1s spectrum at the Pt particles was indistinguishable from that of the adjacent membrane. We interpret these observations to indicate that nitrogenous ligands in the nitrogen containing precursors, or decomposition product(s) from that source, are transported together with the dissolved Pt from the cathode into the membrane as a result of the catalyst degradation process. This places constraints on possible mechanisms for the PTIM band formation process.

  8. Element distribution and iron speciation in mature wheat grains (Triticum aestivum L.) using synchrotron X-ray fluorescence microscopy mapping and X-ray absorption near-edge structure (XANES) imaging.

    PubMed

    De Brier, Niels; Gomand, Sara V; Donner, Erica; Paterson, David; Smolders, Erik; Delcour, Jan A; Lombi, Enzo

    2016-08-01

    Several studies have suggested that the majority of iron (Fe) and zinc (Zn) in wheat grains are associated with phytate, but a nuanced approach to unravel important tissue-level variation in element speciation within the grain is lacking. Here, we present spatially resolved Fe-speciation data obtained directly from different grain tissues using the newly developed synchrotron-based technique of X-ray absorption near-edge spectroscopy imaging, coupling this with high-definition μ-X-ray fluorescence microscopy to map the co-localization of essential elements. In the aleurone, phosphorus (P) is co-localized with Fe and Zn, and X-ray absorption near-edge structure imaging confirmed that Fe is chelated by phytate in this tissue layer. In the crease tissues, Zn is also positively related to P distribution, albeit less so than in the aleurone. Speciation analysis suggests that Fe is bound to nicotianamine rather than phytate in the nucellar projection, and that more complex Fe structures may also be present. In the embryo, high Zn concentrations are present in the root and shoot primordium, co-occurring with sulfur and presumably bound to thiol groups. Overall, Fe is mainly concentrated in the scutellum and co-localized with P. This high resolution imaging and speciation analysis reveals the complexity of the physiological processes responsible for element accumulation and bioaccessibility. PMID:27038325

  9. Element distribution and iron speciation in mature wheat grains (Triticum aestivum L.) using synchrotron X-ray fluorescence microscopy mapping and X-ray absorption near-edge structure (XANES) imaging.

    PubMed

    De Brier, Niels; Gomand, Sara V; Donner, Erica; Paterson, David; Smolders, Erik; Delcour, Jan A; Lombi, Enzo

    2016-08-01

    Several studies have suggested that the majority of iron (Fe) and zinc (Zn) in wheat grains are associated with phytate, but a nuanced approach to unravel important tissue-level variation in element speciation within the grain is lacking. Here, we present spatially resolved Fe-speciation data obtained directly from different grain tissues using the newly developed synchrotron-based technique of X-ray absorption near-edge spectroscopy imaging, coupling this with high-definition μ-X-ray fluorescence microscopy to map the co-localization of essential elements. In the aleurone, phosphorus (P) is co-localized with Fe and Zn, and X-ray absorption near-edge structure imaging confirmed that Fe is chelated by phytate in this tissue layer. In the crease tissues, Zn is also positively related to P distribution, albeit less so than in the aleurone. Speciation analysis suggests that Fe is bound to nicotianamine rather than phytate in the nucellar projection, and that more complex Fe structures may also be present. In the embryo, high Zn concentrations are present in the root and shoot primordium, co-occurring with sulfur and presumably bound to thiol groups. Overall, Fe is mainly concentrated in the scutellum and co-localized with P. This high resolution imaging and speciation analysis reveals the complexity of the physiological processes responsible for element accumulation and bioaccessibility.

  10. [Cryo-microscopy, an alternative to the X-ray crystallography?].

    PubMed

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

    Recent technological advances have revolutionized the field of structural biologists. Specifically, dramatic progress related to the development of new electron microscopes and image capture (direct electron detection camera) and the provision of new image analysis software has led to a breakthrough in terms of resolution attained using cryo-electron transmission microscopy. It is thus possible to calculate relatively quickly high-resolution structures of biological molecules whom structural study still resists to more conventional methods such as X-ray diffraction or nuclear magnetic resonance (NMR). These structures thus obtained may also bring complementary structural information to those already described by other methods. Some of these new structures resolved through cryo-electron microscopy revealed for the first time the precise operation of essential mechanisms necessary for the good physiological process of a cell. The ability to solve these structures at atomic resolution detail is essential for the development of new drugs that target these proteins of therapeutic interest. Thanks to these advanced techniques that we summarize in this revew, biological and medical issues have now become accessible, whereas this approach was inconceivable only five yeras ago. ‡. PMID:27615185

  11. 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.

  12. 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.

  13. Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy.

    PubMed

    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.

  14. Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy.

    PubMed

    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

  15. 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

  16. Integrated circuit authentication using photon-limited x-ray microscopy.

    PubMed

    Markman, Adam; Javidi, Bahram

    2016-07-15

    A counterfeit integrated circuit (IC) may contain subtle changes to its circuit configuration. These changes may be observed when imaged using an x-ray; however, the energy from the x-ray can potentially damage the IC. We have investigated a technique to authenticate ICs under photon-limited x-ray imaging. We modeled an x-ray image with lower energy by generating a photon-limited image from a real x-ray image using a weighted photon-counting method. We performed feature extraction on the image using the speeded-up robust features (SURF) algorithm. We then authenticated the IC by comparing the SURF features to a database of SURF features from authentic and counterfeit ICs. Our experimental results with real and counterfeit ICs using an x-ray microscope demonstrate that we can correctly authenticate an IC image captured using orders of magnitude lower energy x-rays. To the best of our knowledge, this Letter is the first one on using a photon-counting x-ray imaging model and relevant algorithms to authenticate ICs to prevent potential damage.

  17. Integrated circuit authentication using photon-limited x-ray microscopy.

    PubMed

    Markman, Adam; Javidi, Bahram

    2016-07-15

    A counterfeit integrated circuit (IC) may contain subtle changes to its circuit configuration. These changes may be observed when imaged using an x-ray; however, the energy from the x-ray can potentially damage the IC. We have investigated a technique to authenticate ICs under photon-limited x-ray imaging. We modeled an x-ray image with lower energy by generating a photon-limited image from a real x-ray image using a weighted photon-counting method. We performed feature extraction on the image using the speeded-up robust features (SURF) algorithm. We then authenticated the IC by comparing the SURF features to a database of SURF features from authentic and counterfeit ICs. Our experimental results with real and counterfeit ICs using an x-ray microscope demonstrate that we can correctly authenticate an IC image captured using orders of magnitude lower energy x-rays. To the best of our knowledge, this Letter is the first one on using a photon-counting x-ray imaging model and relevant algorithms to authenticate ICs to prevent potential damage. PMID:27420519

  18. In-situ observation of nickel oxidation using synchrotron based full-field transmission X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Kiss, Andrew M.; Harris, William M.; Wang, Steve; Vila-Comamala, Joan; Deriy, Alex; Chiu, Wilson K. S.

    2013-02-01

    An in situ imaging-based approach is reported to study chemical reactions using full-field transmission x-ray microscopy (TXM). Ni particles were oxidized at temperatures between 400 and 850 °C in the TXM to directly observe their morphology change while the chemical composition is monitored by x-ray absorption near edge spectroscopy. Reaction rates and activation energies are calculated from the image data. The goal of this effort is to better understand Ni oxidation in electrode materials. The approach developed will be an effective technique for directly studying chemical reactions of particles and their behavior at the nano-scale.

  19. Zone-doubled Fresnel zone plates for high-resolution hard X-ray full-field transmission microscopy

    PubMed Central

    Vila-Comamala, Joan; Pan, Yongsheng; Lombardo, Jeffrey J.; Harris, William M.; Chiu, Wilson K. S.; David, Christian; Wang, Yuxin

    2012-01-01

    Full-field transmission X-ray microscopy is a unique non-destructive technique for three-dimensional imaging of specimens at the nanometer scale. Here, the use of zone-doubled Fresnel zone plates to achieve a spatial resolution better than 20 nm in the hard X-ray regime (8–10 keV) is reported. By obtaining a tomographic reconstruction of a Ni/YSZ solid-oxide fuel cell, the feasibility of performing three-dimensional imaging of scientifically relevant samples using such high-spatial-resolution Fresnel zone plates is demonstrated. PMID:22898949

  20. Multi-Scaled Microstructures in Natural Rubber Characterized by Synchrotron X-ray Scattering and Optical Microscopy

    SciTech Connect

    Toki , S.; Hsiao, B; Amnuaypornsri , S; Sakdapipanich, J; Tanaka, Y

    2008-01-01

    Multi-scaled microstructures induced by natural impurities (i.e., proteins, phospholipids, carbohydrates) in natural rubber (NR) were investigated by synchrotron small-angle X-ray scattering (SAXS), wide-angle X-ray diffraction (WAXD), and optical microscopy using several kinds of untreated and chemically treated un-vulcanized samples. These microstructures include large aggregates (size less than 50 m), well-defined crystals (size less than a few 10 m), and micelles (size much less than 10 m). In un-vulcanized NR samples, even though the concentrations of natural impurities are relatively low, the dispersion of these microstructures significantly affects the mechanical properties

  1. In situ alkali-silica reaction observed by x-ray microscopy

    SciTech Connect

    Kurtis, K.E.; Monteiro, P.J.M.; Brown, J.T.; Meyer-Ilse, W.

    1997-04-01

    In concrete, alkali metal ions and hydroxyl ions contributed by the cement and reactive silicates present in aggregate can participate in a destructive alkali-silica reaction (ASR). This reaction of the alkalis with the silicates produces a gel that tends to imbibe water found in the concrete pores, leading to swelling of the gel and eventual cracking of the affected concrete member. Over 104 cases of alkali-aggregate reaction in dams and spillways have been reported around the world. At present, no method exists to arrest the expansive chemical reaction which generates significant distress in the affected structures. Most existing techniques available for the examination of concrete microstructure, including ASR products, demand that samples be dried and exposed to high pressure during the observation period. These sample preparation requirements present a major disadvantage for the study of alkali-silica reaction. Given the nature of the reaction and the affect of water on its products, it is likely that the removal of water will affect the morphology, creating artifacts in the sample. The purpose of this research is to observe and characterize the alkali-silica reaction, including each of the specific reactions identified previously, in situ without introducing sample artifacts. For observation of unconditioned samples, x-ray microscopy offers an opportunity for such an examination of the alkali-silica reaction. Currently, this investigation is focusing on the effect of calcium ions on the alkali-silica reaction.

  2. Visualization of asymmetric wetting ridges on soft solids with X-ray microscopy

    PubMed Central

    Park, Su Ji; Weon, Byung Mook; Lee, Ji San; Lee, Junho; Kim, Jinkyung; Je, Jung Ho

    2014-01-01

    One of the most questionable issues in wetting is the force balance that includes the vertical component of liquid surface tension. On soft solids, the vertical component leads to a microscopic protrusion of the contact line, that is, a ‘wetting ridge’. The wetting principle determining the tip geometry of the ridge is at the heart of the issues over the past half century. Here we reveal a universal wetting principle from the ridge tips directly visualized with high spatio-temporal resolution of X-ray microscopy. We find that the cusp of the ridge is bent with an asymmetric tip, whose geometry is invariant during ridge growth or by surface softness. This singular asymmetry is deduced by linking the macroscopic and microscopic contact angles to Young and Neuman laws, respectively. Our finding shows that this dual-scale approach would be contributable to a general framework in elastowetting, and give hints to issues in cell-substrate interaction and elasto-capillary problems. PMID:25007777

  3. Electron microscopy and x-ray diffraction evidence for two Z-band structural states.

    PubMed

    Perz-Edwards, Robert J; Reedy, Michael K

    2011-08-01

    In vertebrate muscles, Z-bands connect adjacent sarcomeres, incorporate several cell signaling proteins, and may act as strain sensors. Previous electron microscopy (EM) showed Z-bands reversibly switch between a relaxed, "small-square" structure, and an active, "basketweave" structure, but the mechanism of this transition is unknown. Here, we found the ratio of small-square to basketweave in relaxed rabbit psoas muscle varied with temperature, osmotic pressure, or ionic strength, independent of activation. By EM, the A-band and both Z-band lattice spacings varied with temperature and pressure, not ionic strength; however, the basketweave spacing was consistently 10% larger than small-square. We next sought evidence for the two Z-band structures in unfixed muscles using x-ray diffraction, which indicated two Z-reflections whose intensity ratios and spacings correspond closely to the EM measurements for small-square and basketweave if the EM spacings are adjusted for 20% shrinkage due to EM processing. We conclude that the two Z-reflections arise from the small-square and basketweave forms of the Z-band as seen by EM. Regarding the mechanism of transition during activation, the effects of Ca(2+) in the presence of force inhibitors suggested that the interconversion of Z-band forms was correlated with tropomyosin movement on actin. PMID:21806939

  4. Submicrometre-Resolution Polychromatic Three-dimensional X-ray Microscopy

    SciTech Connect

    Larson, Ben C; Levine, Lyle E.

    2013-01-01

    The ability to study the structure, microstructure and evolution of materials with increasing spatial resolution is fundamental to achieving a full understanding of the underlying science of materials. Polychromatic three-dimensional X-ray microscopy (3DXM) is a recently developed nondestructive diffraction technique that enables crystallographic phase identification, determination of local crystal orientations, grain morphologies, grain interface types and orientations, and in favorable cases direct determination of the deviatoric elastic strain tensor with submicrometre spatial resolution in all three dimensions. With the added capability of an energy-scanning incident beam monochromator, the determination of absolute lattice parameters is enabled, allowing specification of the complete elastic strain tensor with three- dimensional spatial resolution. The methods associated with 3DXM are described and key applications of 3DXM are discussed, including studies of deformation in single-crystal and polycrystalline metals and semiconductors, indentation deformation, thermal grain growth in polycrystalline aluminium, the metal insulator transition in nanoplatelet VO 2 , interface strengths in metal matrix composites, high-pressure science, Sn whisker growth, and electromigra- tion processes. Finally, the outlook for future developments associated with this technique is described.

  5. Real-Time X-Ray Transmission Microscopy for Fundamental Studies Solidification

    NASA Technical Reports Server (NTRS)

    Curreri, Peter A.; Kaukler, William F.; Sen, Subhayu; Peters, Palmer

    1998-01-01

    High resolution real-time X-ray Transmission Microscopy, XTM, has been applied to obtain information fundamental to solidification of optically opaque metallic systems. We have previously reported the measurement of solute profile in the liquid, phase growth, and detailed solid-liquid interfacial morphology of aluminum based alloys with exposure times less than 2 seconds. Recent advances in XTM furnace design have provided an increase in real-time magnification (during solidification) for the XTM from 4OX to 16OX. The increased magnification has enabled for the first time the XTM imaging of real-time growth of fibers and particles with diameters of 5 micrometers. We have applied this system to study of the kinetics of formation and morphological evolution of secondary fibers and particles in Al-Bi monotectic alloys to observe a previously unreported velocity dependent thermo-capillary depletion mechanism for Bi rich liquid which can penetrate many fiber diameters into the solid-liquid interface. In this talk we will discuss application of the XTM to the study the fundamentals of monotectic and eutectic solidification, the enhancement of XTM data with precise solid liquid interfacial temperature and thermal gradient measurement techniques, and the application of this technology to the study of the fundamentals of solidification in microgravity,

  6. Architectural plasticity of AMPK revealed by electron microscopy and X-ray crystallography.

    PubMed

    Ouyang, Yan; Zhu, Li; Li, Yifang; Guo, Miaomiao; Liu, Yang; Cheng, Jin; Zhao, Jing; Wu, Yi

    2016-01-01

    Mammalian AMP-activated protein kinase (AMPK) acts as an important sensor of cellular energy homeostasis related with AMP/ADP to ATP ratio. The overall architecture of AMPK has been determined in either homotrimer or monomer form by electron microscopy (EM) and X-ray crystallography successively. Accordingly proposed models have consistently revealed a key role of the α subunit linker in sensing adenosine nucleoside binding on the γ subunit and mediating allosteric regulation of kinase domain (KD) activity, whereas there are vital differences in orienting N-terminus of α subunit and locating carbohydrate-binding module (CBM) of β subunit. Given that Mg(2+), an indispensable cofactor of AMPK was present in the EM sample preparation buffer however absent when forming crystals, here we carried out further reconstructions without Mg(2+) to expectably inspect if this ion may contribute to this difference. However, no essential alteration has been found in this study compared to our early work. Further analyses indicate that the intra-molecular movement of the KD and CBM are most likely due to the flexible linkage of the disordered linkers with the rest portion as well as a contribution from the plasticity in the inter-molecular assembly mode, which might ulteriorly reveal an architectural complication of AMPK. PMID:27063142

  7. 3D localization of electrophysiology catheters from a single x-ray cone-beam projection

    SciTech Connect

    Robert, Normand Polack, George G.; Sethi, Benu; Rowlands, John A.; Crystal, Eugene

    2015-10-15

    Purpose: X-ray images allow the visualization of percutaneous devices such as catheters in real time but inherently lack depth information. The provision of 3D localization of these devices from cone beam x-ray projections would be advantageous for interventions such as electrophysiology (EP), whereby the operator needs to return a device to the same anatomical locations during the procedure. A method to achieve real-time 3D single view localization (SVL) of an object of known geometry from a single x-ray image is presented. SVL exploits the change in the magnification of an object as its distance from the x-ray source is varied. The x-ray projection of an object of interest is compared to a synthetic x-ray projection of a model of said object as its pose is varied. Methods: SVL was tested with a 3 mm spherical marker and an electrophysiology catheter. The effect of x-ray acquisition parameters on SVL was investigated. An independent reference localization method was developed to compare results when imaging a catheter translated via a computer controlled three-axes stage. SVL was also performed on clinical fluoroscopy image sequences. A commercial navigation system was used in some clinical image sequences for comparison. Results: SVL estimates exhibited little change as x-ray acquisition parameters were varied. The reproducibility of catheter position estimates in phantoms denoted by the standard deviations, (σ{sub x}, σ{sub y}, σ{sub z}) = (0.099 mm,  0.093 mm,  2.2 mm), where x and y are parallel to the detector plane and z is the distance from the x-ray source. Position estimates (x, y, z) exhibited a 4% systematic error (underestimation) when compared to the reference method. The authors demonstrated that EP catheters can be tracked in clinical fluoroscopic images. Conclusions: It has been shown that EP catheters can be localized in real time in phantoms and clinical images at fluoroscopic exposure rates. Further work is required to characterize

  8. Contrast transfer functions for Zernike phase contrast in full-field transmission hard X-ray microscopy.

    PubMed

    Yang, Yang; Cheng, Yin; Heine, Ruth; Baumbach, Tilo

    2016-03-21

    Full-field transmission hard X-ray microscopy (TXM) has been widely applied to study morphology and structures with high spatial precision and to dynamic processes. Zernike phase contrast (ZPC) in hard X-ray TXM is often utilized to get an in-line phase contrast enhancement for weak-absorbing materials with little contrast differences. Here, following forward image formation, we derive and simplify the contrast transfer functions (CTFs) of the Zernike phase imaging system in TXM based on a linear space-shift-invariant imaging mode under certain approximations. The CTFs in ZPC in their simplified forms show a high similarity to the one in free-space propagation X-ray imaging systems. PMID:27136800

  9. 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. PMID:25392009

  10. Fast-scanning high-flux microprobe for biological X-ray fluorescence microscopy and microXAS

    SciTech Connect

    Barrea, R.A.; Gore, D.; Kujala, N.; Karanfil, C.; Kozyrenko, S.; Heurich, R.; Vukonich, M.; Huang, R.; Paunesku, T.; Woloschak, G.; Irving, T.C.

    2010-07-23

    There is a growing interest in the biomedical community in obtaining information concerning the distribution and local chemical environment of metals in tissues and cells. Recently, biological X-ray fluorescence microscopy (XFM) has emerged as the tool of choice to address these questions. A fast-scanning high-flux X-ray microprobe, built around a recently commissioned pair of 200 mm-long Rh-coated silicon Kirkpatrick-Baez mirrors, has been constructed at BioCAT beamline 18ID at the Advanced Photon Source. The new optical system delivers a flux of 1.3 x 10{sup 12} photons s{sup -1} into a minimum focal spot size of {approx}3-5 {micro}m FWHM. A set of Si drift detectors and bent Laue crystal analyzers may be used in combination with standard ionization chambers for X-ray fluorescence measurements. BioCAT's scanning software allows fast continuous scans to be performed while acquiring and storing full multichannel analyzer spectra per pixel on-the-fly with minimal overhead time (<20 ms per pixel). Together, the high-flux X-ray microbeam and the rapid-scanning capabilities of the BioCAT beamline allow the collection of XFM and micro X-ray absorption spectroscopy (microXAS) measurements from as many as 48 tissue sections per day. This paper reports the commissioning results of the new instrument with representative XFM and microXAS results from tissue samples.

  11. Feasibility study of high-resolution coherent diffraction microscopy using synchrotron x rays focused by Kirkpatrick-Baez mirrors

    SciTech Connect

    Takahashi, Yukio; Nishino, Yoshinori; Ishikawa, Tetsuya; Mimura, Hidekazu; Tsutsumi, Ryosuke; Kubo, Hideto; Yamauchi, Kazuto

    2009-04-15

    High-flux coherent x rays are necessary for the improvement of the spatial resolution in coherent x-ray diffraction microscopy (CXDM). In this study, high-resolution CXDM using Kirkpatrick-Baez (KB) mirrors is proposed, and the mirrors are designed for experiments of the transmission scheme at SPring-8. Both the photon density and spatial coherence of synchrotron x rays focused by the KB mirrors are investigated by wave optical simulation. The KB mirrors can produce nearly diffraction-limited two-dimensional focusing x rays of approx1 mum in size at 8 keV. When the sample size is less than approx1 mum, the sample can be illuminated with full coherent x rays by adjusting the cross-slit size set between the source and the mirrors. From the estimated photon density at the sample position, the feasibility of CXDM with a sub-1-nm spatial resolution is suggested. The present ultraprecise figuring process enables us to fabricate mirrors for carrying out high-resolution CXDM experiments.

  12. Ultrastructural imaging and molecular modeling of live bacteria using soft x-ray contact microscopy with nanoseconds laser-plasma radiation

    NASA Astrophysics Data System (ADS)

    Kado, Masataka; Richardson, Martin C.; Gaebel, Kai; Torres, David S.; Rajyaguru, Jayshree; Muszynski, Michael J.

    1995-09-01

    X-ray images of the various live bacteria, such as Staphylococcus and Streptococcus, and micromolecule such as chromosomal DNA from Escherichis coli, and Lipopolysacchride 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 50nm spatial resolutions are achieved and images are able to be discussed on the biological view.

  13. Large-area soft x-ray projection lithography using multilayer mirrors structured by RIE

    NASA Astrophysics Data System (ADS)

    Rahn, Steffen; Kloidt, Andreas; Kleineberg, Ulf; Schmiedeskamp, Bernt; Kadel, Klaus; Schomburg, Werner K.; Hormes, F. J.; Heinzmann, Ulrich

    1993-01-01

    SXPL (soft X-ray projection lithography) is one of the most promising applications of X-ray reflecting optics using multilayer mirrors. Within our collaboration, such multilayer mirrors were fabricated, characterized, laterally structured and then used as reflection masks in a projecting lithography procedure. Mo/Si-multilayer mirrors were produced by electron beam evaporation in UHV under thermal treatment with an in-situ X-ray controlled thickness in the region of 2d equals 14 nm. The reflectivities measured at normal incidence reached up to 54%. Various surface analysis techniques have been applied in order to characterize and optimize the X-ray mirrors. The multilayers were patterned by reactive ion etching (RIE) with CF(subscript 4), using a photoresist as the etch mask, thus producing X-ray reflection masks. The masks were tested in the synchrotron radiation laboratory of the electron accelerator ELSA at the Physikalisches Institut of Bonn University. A double crystal X-ray monochromator was modified so as to allow about 0.5 cm(superscript 2) of the reflection mask to be illuminated by white synchrotron radiation. The reflected patterns were projected (with an energy of 100 eV) onto the resist (Hoechst AZ PF 514), which was mounted at an average distance of about 7 mm. In the first test-experiments, structure sizes down to 8 micrometers were nicely reproduced over the whole of the exposed area. Smaller structures were distorted by Fresnel-diffraction. The theoretically calculated diffraction images agree very well with the observed images.

  14. Soft-x-ray projection lithography experiments using Schwarzschild imaging optics

    SciTech Connect

    Tichenor, D.A.; Kubiak, G.D.; Malinowski, M.E.; Stulen, R.H.; Haney, S.J.; Berger, K.W.; Brown, L.A. ); Sweatt, W.C. ); Bjorkholm, J.E.; Freeman, R.R.; Himel, M.D.; MacDowell, A.A.; Tennant, D.M.; Wood II, O.R. ); Bokor, J.; Jewell, T.E.; Mansfield, W.M.; Waskiewicz, W.K.; White, D.L.; Windt, D.L. )

    1993-12-01

    Soft-x-ray projection imaging is demonstrated by the use of 14-nm radiation from a laser plasma source and a single-surface multilayer-coated ellipsoidal condenser. Aberrations in the condenser and the Schwarzschild imaging objective are characterized and correlated with imaging performance. A new Schwarzschild housing, designed for improved alignment stability, is described.

  15. 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.

  16. 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.

  17. Feasibility tests of transmission x-ray photoelectron emission microscopy of wet samples

    NASA Astrophysics Data System (ADS)

    De Stasio, Gelsomina; Gilbert, B.; Nelson, T.; Hansen, R.; Wallace, J.; Mercanti, D.; Capozi, M.; Baudat, P. A.; Perfetti, P.; Margaritondo, G.; Tonner, B. P.

    2000-01-01

    We performed feasibility tests of photoelectron emission spectromicroscopy of wet samples in the water window (285-532 eV) soft x-ray spectral region. Water was successfully confined in an ultrahigh vacuum compatible compartment with x-ray transparent sides. This water cell was placed in the MEPHISTO spectromicroscope in a transmission geometry, and complete x-ray absorption spectra of the water window region were acquired. We also show micrographs of test samples, mounted outside of the compartment, and imaged through the water. This technique can be used to study liquid chemistry and, at least to the micron level, the microstructure of wet samples. Possibilities include cells in water or buffer, proteins in solution, oils of tribological interest, liquid crystals, and other samples not presently accessible to the powerful x-ray photoelectron emission spectromicroscopy technique.

  18. Science with the EXTraS Project: Exploring the X-Ray Transient and Variable Sky

    NASA Astrophysics Data System (ADS)

    De Luca, A.; Salvaterra, R.; Tiengo, A.; D'Agostino, D.; Watson, M. G.; Haberl, F.; Wilms, J.

    The EXTraS project ("Exploring the X-ray Transient and variable Sky") will characterise the temporal behaviour of the largest ever sample of objects in the soft X-ray range (0.1-12 keV) with a complex, systematic and consistent analysis of all data collected by the European Photon Imaging Camera (EPIC) instrument onboard the ESA XMM-Newton X-ray observatory since its launch. We will search for, and characterize variability (both periodic and aperiodic) in hundreds of thousands of sources spanning more than nine orders of magnitude in time scale and six orders of magnitude in flux. We will also search for fast transients, missed by standard image analysis. Our analysis will be completed by multiwavelength characterization of new discoveries and phenomenological classification of variable sources. All results and products will be made available to the community in a public archive, serving as a reference for a broad range of astrophysical investigations.

  19. Characterization and possible repair of defects in Soft X-ray Projection Lithography masks

    SciTech Connect

    Hawryluk, A.M.

    1993-07-01

    Soft X-ray Projection Lithography (SXPL) is one promising technique for the mass production of integrated circuits with minimum features sizes below 100 nm. Mask fabrication, inspection and repair processes are critically important to all forms of lithography, including SXPL which requires a reflection mask (a substrate coated with a x-ray multilayer coating and patterned with thin metallization layer). Processes for the repair of defects in the metallization patterns have been developed, but at present, there exist no processes for the repair of defects in the multilayer coatings deposited in LLNL`s magnetron sputter deposition facility, which produces state of the art x-ray multilayer mirrors. We also propose one possible process for the repair of defects in these multilayer coatings.

  20. Direct observation of unstained wet biological samples by scanning-electron generation X-ray microscopy.

    PubMed

    Ogura, Toshihiko

    2010-01-01

    Analytical tools of nanometre-scale resolution are indispensable in the fields of biology, physics and chemistry. One suitable tool, the soft X-ray microscope, provides high spatial resolution of visible light for wet specimens. For biological specimens, X-rays of water-window wavelength between carbon (284 eV; 4.3 nm) and oxygen (540 eV; 2.3 nm) absorption edges provide high-contrast imaging of biological samples in water. Among types of X-ray microscope, the transmission X-ray microscope using a synchrotron radiation source with diffractive zone plates offers the highest spatial resolution, approaching 15-10nm. However, even higher resolution is required to measure proteins and protein complexes in biological specimens; therefore, a new type of X-ray microscope with higher resolution that uses a simple light source is desirable. Here we report a novel scanning-electron generation X-ray microscope (SGXM) that demonstrates direct imaging of unstained wet biological specimens. We deposited wet yeasts in the space between two silicon nitride (Si(3)N(4)) films. A scanning electron beam of accelerating voltage 5 keV and current 1.6 nA irradiates the titanium (Ti)-coated Si(3)N(4) film, and the soft X-ray signal from it is detected by an X-ray photodiode (PD) placed below the sample. The SGXM can theoretically achieve better than 5 nm resolution. Our method can be utilized easily for various wet biological samples of bacteria, viruses, and protein complexes.

  1. Versatile atomic force microscopy setup combined with micro-focused X-ray beam

    SciTech Connect

    Slobodskyy, T. Tholapi, R.; Liefeith, L.; Hansen, W.; Zozulya, A. V. Fester, M.; Sprung, M.

    2015-06-15

    Micro-focused X-ray beams produced by third generation synchrotron sources offer new perspective of studying strains and processes at nanoscale. Atomic force microscope setup combined with a micro-focused synchrotron beam allows precise positioning and nanomanipulation of nanostructures under illumination. In this paper, we report on integration of a portable commercial atomic force microscope setup into a hard X-ray synchrotron beamline. Details of design, sample alignment procedure, and performance of the setup are presented.

  2. 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.

  3. 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.

  4. Reconstructing the projected gravitational potential of Abell 1689 from X-ray measurements

    NASA Astrophysics Data System (ADS)

    Tchernin, Céline; Majer, Charles L.; Meyer, Sven; Sarli, Eleonora; Eckert, Dominique; Bartelmann, Matthias

    2015-02-01

    Context. Galaxy clusters can be used as cosmological probes, but to this end, they need to be thoroughly understood. Combining all cluster observables in a consistent way will help us to understand their global properties and their internal structure. Aims: We provide proof of the concept that the projected gravitational potential of galaxy clusters can directly be reconstructed from X-ray observations. We also show that this joint analysis can be used to locally test the validity of the equilibrium assumptions in galaxy clusters. Methods: We used a newly developed reconstruction method, based on Richardson-Lucy deprojection, that allows reconstructing projected gravitational potentials of galaxy clusters directly from X-ray observations. We applied this algorithm to the well-studied cluster Abell 1689 and compared the gravitational potential reconstructed from X-ray observables to the potential obtained from gravitational lensing measurements. We also compared the X-ray deprojected profiles obtained by the Richardson-Lucy deprojection algorithm with the findings from the more conventional onion-peeling technique. Results: Assuming spherical symmetry and hydrostatic equilibrium, the potentials recovered from gravitational lensing and from X-ray emission agree very well beyond 500 kpc. Owing to the fact that the Richardson-Lucy deprojection algorithm allows deprojecting each line of sight independently, this result may indicate that non-gravitational effects and/or asphericity are strong in the central regions of the clusters. Conclusions: We demonstrate the robustness of the potential reconstruction method based on the Richardson-Lucy deprojection algorithm and show that gravitational lensing and X-ray emission lead to consistent gravitational potentials. Our results illustrate the power of combining galaxy-cluster observables in a single, non-parametric, joint reconstruction of consistent cluster potentials that can be used to locally constrain the physical state

  5. 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.

  6. A Comparison of Image Quality Evaluation Techniques for Transmission X-Ray Microscopy

    SciTech Connect

    Bolgert, Peter J; /Marquette U. /SLAC

    2012-08-31

    Beamline 6-2c at Stanford Synchrotron Radiation Lightsource (SSRL) is capable of Transmission X-ray Microscopy (TXM) at 30 nm resolution. Raw images from the microscope must undergo extensive image processing before publication. Since typical data sets normally contain thousands of images, it is necessary to automate the image processing workflow as much as possible, particularly for the aligning and averaging of similar images. Currently we align images using the 'phase correlation' algorithm, which calculates the relative offset of two images by multiplying them in the frequency domain. For images containing high frequency noise, this algorithm will align noise with noise, resulting in a blurry average. To remedy this we multiply the images by a Gaussian function in the frequency domain, so that the algorithm ignores the high frequency noise while properly aligning the features of interest (FOI). The shape of the Gaussian is manually tuned by the user until the resulting average image is sharpest. To automatically optimize this process, it is necessary for the computer to evaluate the quality of the average image by quantifying its sharpness. In our research we explored two image sharpness metrics, the variance method and the frequency threshold method. The variance method uses the variance of the image as an indicator of sharpness while the frequency threshold method sums up the power in a specific frequency band. These metrics were tested on a variety of test images, containing both real and artificial noise. To apply these sharpness metrics, we designed and built a MATLAB graphical user interface (GUI) called 'Blur Master.' We found that it is possible for blurry images to have a large variance if they contain high amounts of noise. On the other hand, we found the frequency method to be quite reliable, although it is necessary to manually choose suitable limits for the frequency band. Further research must be performed to design an algorithm which

  7. 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.

  8. Imaging Spin Dynamics on the Nanoscale using X-Ray Microscopy

    NASA Astrophysics Data System (ADS)

    Stoll, Hermann; Noske, Matthias; Weigand, Markus; Richter, Kornel; Krüger, Benjamin; Reeve, Robert; Hänze, Max; Adolff, Christian; Stein, Falk-Ulrich; Meier, Guido; Kläui, Mathias; Schütz, Gisela

    2015-04-01

    The dynamics of emergent magnetic quasiparticles, such as vortices, domain walls, and bubbles are studied by scanning transmission x-ray microscopy (STXM), combining magnetic (XMCD) contrast with about 25 nm lateral resolution as well as 70 ps time resolution. Essential progress in the understanding of magnetic vortex dynamics is achieved by vortex core reversal observed by sub-GHz excitation of the vortex gyromode, either by ac magnetic fields or spin transfer torque. The basic switching scheme for this vortex core reversal is the generation of a vortex-antivortex pair. Much faster vortex core reversal is obtained by exciting azimuthal spin wave modes with (multi-GHz) rotating magnetic fields or orthogonal monopolar field pulses in x and y direction, down to 45 ps in duration. In that way unidirectional vortex core reversal to the vortex core 'down' or 'up' state only can be achieved with switching times well below 100 ps. Coupled modes of interacting vortices mimic crystal properties. The individual vortex oscillators determine the properties of the ensemble, where the gyrotropic mode represents the fundamental excitation. By self-organized state formation we investigate distinct vortex core polarization configurations and understand these eigenmodes in an extended Thiele model. Analogies with photonic crystals are drawn. Oersted fields and spin-polarized currents are used to excite the dynamics of domain walls and magnetic bubbles. From the measured phase and amplitude of the displacement of domain walls we deduce the size of the non-adiabatic spin-transfer torque. For sensing applications, the displacement of domain walls is studied and a direct correlation between domain wall velocity and spin structure is found. Finally the synchronous displacement of multiple domain walls using perpendicular field pulses is demonstrated as a possible paradigm shift for magnetic memory and logic applications.

  9. X-ray tomographic microscopy analysis of the dendrite orientation transition in Al-Zn

    NASA Astrophysics Data System (ADS)

    Friedli, Jonathan; Fife, Julie L.; Di Napoli, Paolo; Rappaz, Michel

    2012-07-01

    Recently, Gonzales and Rappaz [Met. Mat. Trans. A37:2797, 2006] showed the influence of an increasing zinc content on the growth directions of aluminum dendrites. langle100rangle and langle110rangle dendrites were observed below 25wt.% and above 55wt.% zinc, respectively, whereas textured seaweeds and langle320rangle dendrites were observed at intermediate compositions. Considering the complexity of these structures, it is necessary to first characterize them in further details and second, to model them using the phase field method. The so-called Dendrite Orientation Transition (DOT) was thus reinvestigated in quenched Bridgman solidification samples. The combination of X-ray tomographic microscopy and electron backscattered diffraction (EBSD) analysis on a whole range of compositions, from 5 to 90wt.% Zn, allowed insights with unprecedented details about texture, growth directions and mechanisms of the aforementioned structures. We show that seaweeds rather than dendrites are found at all intermediate compositions. Their growth was confirmed to be constrained within a (100) symmetry plane. However, new findings indicate that the observed macroscopic texture does not necessarily correspond to the actual growth directions of the microstructure. Further, it seems to operate by an alternating growth direction mechanism and could be linked to the competition between the langle100rangle and langle110rangle characters of regular dendrites observed at the limits of the DOT. These characters, as well as 3D seaweeds, are observed in phase-field simulations of equiaxed growth and directional solidification, respectively. This study emphasizes the importance of accurate experimental data to validate numerical models and details the progress that such combinations provide for the understanding of growth mechanisms.

  10. Fast Simulation of X-ray Projections of Spline-based Surfaces using an Append Buffer

    PubMed Central

    Maier, Andreas; Hofmann, Hannes G.; Schwemmer, Chris; Hornegger, Joachim; Keil, Andreas; Fahrig, Rebecca

    2012-01-01

    Many scientists in the field of x-ray imaging rely on the simulation of x-ray images. As the phantom models become more and more realistic, their projection requires high computational effort. Since x-ray images are based on transmission, many standard graphics acceleration algorithms cannot be applied to this task. However, if adapted properly, simulation speed can be increased dramatically using state-of-the-art graphics hardware. A custom graphics pipeline that simulates transmission projections for tomographic reconstruction was implemented based on moving spline surface models. All steps from tessellation of the splines, projection onto the detector, and drawing are implemented in OpenCL. We introduced a special append buffer for increased performance in order to store the intersections with the scene for every ray. Intersections are then sorted and resolved to materials. Lastly, an absorption model is evaluated to yield an absorption value for each projection pixel. Projection of a moving spline structure is fast and accurate. Projections of size 640×480 can be generated within 254 ms. Reconstructions using the projections show errors below 1 HU with a sharp reconstruction kernel. Traditional GPU-based acceleration schemes are not suitable for our reconstruction task. Even in the absence of noise, they result in errors up to 9 HU on average, although projection images appear to be correct under visual examination. Projections generated with our new method are suitable for the validation of novel CT reconstruction algorithms. For complex simulations, such as the evaluation of motion-compensated reconstruction algorithms, this kind of x-ray simulation will reduce the computation time dramatically. Source code is available at http://conrad.stanford.edu/ PMID:22975431

  11. Techniques for deriving tissue structure from multiple projection dual-energy x-ray absorptiometry

    NASA Technical Reports Server (NTRS)

    Charles, Jr., Harry K. (Inventor); Beck, Thomas J. (Inventor); Feldmesser, Howard S. (Inventor); Magee, Thomas C. (Inventor)

    2004-01-01

    Techniques for deriving bone properties from images generated by a dual-energy x-ray absorptiometry apparatus include receiving first image data having pixels indicating bone mineral density projected at a first angle of a plurality of projection angles. Second image data and third image data are also received. The second image data indicates bone mineral density projected at a different second angle. The third image data indicates bone mineral density projected at a third angle. The third angle is different from the first angle and the second angle. Principal moments of inertia for a bone in the subject are computed based on the first image data, the second image data and the third image data. The techniques allow high-precision, high-resolution dual-energy x-ray attenuation images to be used for computing principal moments of inertia and strength moduli of individual bones, plus risk of injury and changes in risk of injury to a patient.

  12. The Role of Project Science in the Chandra X-Ray Observatory

    NASA Technical Reports Server (NTRS)

    O'Dell, Stephen L.; Weisskopf, Martin C.

    2006-01-01

    The Chandra X-Ray Observatory, one of NASA's Great Observatories, has an outstanding record of scientific and technical success. This success results from the efforts of a team comprising NASA, its contractors, the Smithsonian Astrophysical Observatory, the instrument groups, and other elements of the scientific community, including thousands of scientists who utilize this powerful facility for astrophysical research. We discuss the role of NASA Project Science in the formulation, development, calibration, and operation of the Chandra X-ray Observatory. In addition to representing the scientific community within the Project, Project Science performed what we term "science systems engineering". This activity encompasses translation of science requirements into technical requirements and assessment of the scientific impact of programmatic and technical trades. We briefly describe several examples of science systems engineering conducted by Chandra Project Science.

  13. Hard X-Ray Emission from X-Ray Bursters

    NASA Technical Reports Server (NTRS)

    Halpern, Jules P.; Kaaret, Philip

    1999-01-01

    The scientific goal of this project is to study the hard x-ray emission from x-ray bursters. One target of opportunity observation was made for this investigation during 1997. We obtained 38ks of data on the source 4UI705-44. The project is closely related to "Monitoring x-ray emission from x-ray bursters", and "Long-Term Hard X-Ray Monitoring of X-Ray Bursters."

  14. X-ray contact microscopy using a plasma source generated by long and short (120ns and 10ns) excimer laser pulses

    SciTech Connect

    Cotton, R.; Bollanti, S.; Di Lazzaro, P.

    1995-12-31

    Soft X-ray contact microscopy (SXCM), using a pulsed X-ray source, offers the possibility of imaging the ultrastructure of living biological systems at sub-50nm resolution. The authors have developed a pulsed plasma X-ray source for this application, generated by the large volume XeCl laser Hercules. Various unstable optical resonator configurations were employed to achieve a high laser intensity to increase the conversion efficiency to water window X-rays (280--530 eV). Optimum plasma conditions for SXCM are discussed, including the effect of pulse duration on image resolution. Soft X-ray contact images of Chlamydomonas dysosmos (unicellular alga) and the cyanobacteria Leptolyngbya are shown. In addition, the potential of producing a movie film of the development of X-ray images within the photoresist (acting as the recording medium) is discussed, following the resist development while viewing by atomic force microscopy.

  15. Defect-Assisted Hard-X-Ray Microscopy with Capillary Optics.

    PubMed

    Korecki, Paweł; Sowa, Katarzyna M; Jany, Benedykt R; Krok, Franciszek

    2016-06-10

    Polycapillary x-ray focusing devices are built from hundreds of thousands of bent microcapillaries that are stacked into hexagonal arrays. We show that intrinsic point defects of the optics (e.g., missing or larger capillaries) lead to the formation of multiple x-ray images of an object positioned in the focal plane. These images can be recorded in parallel, and can provide spatial resolution that is limited by the defect size and not by the focal spot size. In a proof-of-principle experiment, we demonstrate submicron resolution, which has not yet been achieved with polycapillary focusing optics. Tailored optics with a controlled distribution of "defects" could be used for multimodal nanoscale x-ray imaging with laboratory setups.

  16. Dark field X-ray microscopy: the effects of condenser/detector aperture.

    PubMed

    Vogt, S; Chapman, H N; Jacobsen, C; Medenwaldt, R

    2001-03-01

    In order to visualize the functionality of a biological cell, it is often desirable to label specific proteins. In this work we concentrate on the optical theory of visualizing colloidal gold labels with soft X-ray microscopes, where scattering from small gold spheres used as labels dominates the image. Using numerical simulations of bright and dark field imaging, we compare different configurations of condenser and objective lenses in transmission X-ray microscopes, and configurations of detector and objective lens in scanning transmission X-ray microscopes. It is verified that the contrast of small, closely spaced features is strongly affected by changes in these configurations; the optimum situation is to have the condenser aperture (in TXM) or detector aperture (in STXM) equal to 3/2 that of the objective numerical aperture. PMID:11310539

  17. Compact high-resolution differential interference contrast soft x-ray microscopy

    SciTech Connect

    Bertilson, Michael C.; Hofsten, Olov von; Lindblom, Magnus; Hertz, Hans M.; Vogt, Ulrich

    2008-02-11

    We demonstrate high-resolution x-ray differential interference contrast (DIC) in a compact soft x-ray microscope. Phase contrast imaging is enabled by the use of a diffractive optical element objective which is matched to the coherence conditions in the microscope setup. The performance of the diffractive optical element objective is evaluated in comparison with a normal zone plate by imaging of a nickel siemens star pattern and linear grating test objects. Images obtained with the DIC optic exhibit typical DIC enhancement in addition to the normal absorption contrast. Contrast transfer functions based on modulation measurements in the obtained images show that the DIC optic gives a significant increase in contrast without reducing the spatial resolution. The phase contrast operation mode now available for our compact soft x-ray microscope will be a useful tool for future studies of samples with low absorption contrast.

  18. The X-Ray Transform Projection of 3D Mother Wavelet Function

    PubMed Central

    Yang, Xiangyu; Guo, Jiqiang; Lu, Li; Zeng, Li

    2013-01-01

    As we all know, any practical computed tomography (CT) projection data more or less contains noises. Hence, it will be inconvenient for the postprocessing of a reconstructed 3D image even when the noise in the projection data is white. The reason is that the noise in the reconstructed image may be nonwhite. X-ray transform can be applied to the three dimensional (3D) CT, depicting the relationship between material density and ray projection. In this paper, nontensor product relationship between the two dimensional (2D) mother wavelet and 3D mother wavelet is obtained by taking X-ray transform projection of 3D mother wavelet. We proved that the projection of the 3D mother wavelet is a 2D mother wavelet if the 3D mother wavelet satisfies certain conditions. So, the 3D wavelet transform of a 3D image can be implemented by the 2D wavelet transform of its X-ray transform projection and it will contribute to the reduction complexity and computation time during image processing. What is more, it can also avoid noise transfer and amplification during the processing of CT image reconstruction. PMID:24376470

  19. 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.

  20. The use of high energy laser-plasma sources in soft X-ray contact microscopy of living biological samples

    NASA Astrophysics Data System (ADS)

    Batani, D.; Botto, C.; Moret, M.; Milani, M.; Lucchini, G.; Eidmann, K.; Cotelli, F.; Lora Lamia Donin, C.; Poletti, G.; Ford, T.; Stead, A.

    2002-11-01

    In this paper the results of an experiment on soft X-ray contact microscopy using a laser-plasma source are presented. A resolution of 50 nm has been achieved imaging pig sperm cells, while other specimens, such as algae and yeast cells, showed internal details, proving the technique to be a powerful tool for biological investigations. Original biological information has been obtained and the conditions for optimal image formation have been studied.

  1. An X-ray diffraction and electron microscopy study of the extraction of erythrocyte membranes with the bile salt, cholate.

    PubMed

    Finean, J B; Gunn, T K; Hutchinson, A; Mills, D

    1984-10-17

    Studies by X-ray diffraction and electron microscopy of slowly frozen samples of control and cholate-extracted preparations of erythrocyte membranes have demonstrated changes in structural parameters which can readily be related to the extraction of cytoskeletal proteins. In the frozen state, these components appear to be condensed to about 10% of the total membrane thickness. The observations illustrate some of the advantages and limitations in the use of slowly frozen membrane preparations in studies of membrane structure.

  2. Development of achromatic full-field hard x-ray microscopy with two monolithic imaging mirrors

    NASA Astrophysics Data System (ADS)

    Matsuyama, S.; Kino, H.; Yasuda, S.; Kohmura, Y.; Okada, H.; Ishikawa, T.; Yamauchi, K.

    2015-09-01

    Advanced Kirkpatrick-Baez mirror optics using two monolithic imaging mirrors was developed to realize an achromatic, high-resolution, and a high-stability full-field X-ray microscope. The mirror consists of an elliptical section and a hyperbolic section on a quartz glass substrate, in which the geometry follows the Wolter (type I) optics rules. A preliminary test was performed at SPring-8 using X-rays monochromatized to 9.881 keV. A 100-nm feature on a Siemens star chart could be clearly observed.

  3. X-ray Phase Imaging Microscopy with Two-Dimensional Knife-Edge Filters

    NASA Astrophysics Data System (ADS)

    Choi, Jaeho; Park, Yong-Sung

    2012-04-01

    A novel scheme of X-ray differential phase imaging was implemented with an array source and a two-dimensional Foucault knife-edge (2DFK). A pinhole array lens was employed to manipulate the X-ray beam on the Fourier space. An emerging biaxial scanning procedure was also demonstrated with the periodic 2DFK. The differential phase images (DPIs) of the midrib in a leaf of a rose bush were visualized to verify the phase imaging of biological specimens by the proposed method. It also has features of depicting multiple-stack phase images, and rendering morphological DPIs, because it acquires pure phase information.

  4. 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

  5. In situ spatial and time-resolved studies of electrochemical reactions by scanning transmission X-ray microscopy.

    PubMed

    Guay, Daniel; Stewart-Ornstein, Jacob; Zhang, Xuerong; Hitchcock, Adam P

    2005-06-01

    The first in situ measurements with scanning transmission X-ray microscopy (STXM) of an active electrochemical cell are reported. An electrochemical wet cell, consisting of an electrodeposited polyaniline thin film on a thin Au film covered by an overlayer of 1 M HCl solution sitting between two X-ray transparent silicon nitride windows, was assembled. X-ray absorption images and spatial and time-resolved spectra of this system under potential control were examined using the beamline 5.3.2 STXM at the Advanced Light Source. The chemical state of the polyaniline film was reversibly converted between reduced (leucoemeraldine) and oxidized (emeraldine chloride) states by changing the applied potential. The electrochemical changes were monitored by spatially resolved C 1s and N 1s X-ray absorption spectroscopy and chemical-state selective imaging. Comparison of differences between images at two energies at different potentials provided electrochemical contrast with a resolution better than 50 nm, thereby monitoring that component of the polyaniline film that was electrochemically active. Kinematic studies in the subsecond regime are demonstrated.

  6. Three-dimensional imaging of chemical phase transformations at the nanoscale with full-field transmission X-ray microscopy.

    PubMed

    Meirer, Florian; Cabana, Jordi; Liu, Yijin; Mehta, Apurva; Andrews, Joy C; Pianetta, Piero

    2011-09-01

    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

  7. Laboratory-based cryogenic soft x-ray tomography with correlative cryo-light and electron microscopy.

    PubMed

    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 subcellular structures of Saccharomyces cerevisiae cells. The microscope is shown to achieve better than 50 nm half-pitch spatial resolution with a Siemens star test sample. For whole biological cells, the microscope can image specimens up to 5 μm thick. Structures as small as 90 nm can be detected in tomographic reconstructions 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 enable greater access to three-dimensional ultrastructure determination of biological whole cells without chemical fixation or physical sectioning.

  8. 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.

  9. Reverse projection retrieval in edge illumination x-ray phase contrast computed tomography

    NASA Astrophysics Data System (ADS)

    Hagen, Charlotte K.; Endrizzi, Marco; Diemoz, Paul C.; Olivo, Alessandro

    2016-06-01

    Edge illumination (EI) x-ray phase contrast computed tomography (CT) can provide three-dimensional distributions of the real and imaginary parts of the complex refractive index (n=1-δ +\\text{i}β ) of the sample. Phase retrieval, i.e. the separation of attenuation and refraction data from projections that contain a combination of both, is a key step in the image reconstruction process. In EI-based x-ray phase contrast CT, this is conventionally performed on the basis of two projections acquired in opposite illumination configurations (i.e. with different positions of the pre-sample mask) at each CT angle. Displacing the pre-sample mask at each projection makes the scan susceptible to motor-induced misalignment and prevents a continuous sample rotation. We present an alternative method for the retrieval of attenuation and refraction data that does not require repositioning the pre-sample mask. The method is based on the reverse projection relation published by Zhu et al (2010 Proc. Natl Acad. Sci. USA 107 13576–81) for grating interferometry-based x-ray phase contrast CT. We use this relation to derive a simplified acquisition strategy that allows acquiring data with a continuous sample rotation, which can reduce scan time when combined with a fast read-out detector. Besides discussing the theory and the necessary alignment of the experimental setup, we present tomograms obtained with reverse projection retrieval and demonstrate their agreement with those obtained with the conventional EI retrieval.

  10. Reverse projection retrieval in edge illumination x-ray phase contrast computed tomography

    NASA Astrophysics Data System (ADS)

    Hagen, Charlotte K.; Endrizzi, Marco; Diemoz, Paul C.; Olivo, Alessandro

    2016-06-01

    Edge illumination (EI) x-ray phase contrast computed tomography (CT) can provide three-dimensional distributions of the real and imaginary parts of the complex refractive index (n=1-δ +\\text{i}β ) of the sample. Phase retrieval, i.e. the separation of attenuation and refraction data from projections that contain a combination of both, is a key step in the image reconstruction process. In EI-based x-ray phase contrast CT, this is conventionally performed on the basis of two projections acquired in opposite illumination configurations (i.e. with different positions of the pre-sample mask) at each CT angle. Displacing the pre-sample mask at each projection makes the scan susceptible to motor-induced misalignment and prevents a continuous sample rotation. We present an alternative method for the retrieval of attenuation and refraction data that does not require repositioning the pre-sample mask. The method is based on the reverse projection relation published by Zhu et al (2010 Proc. Natl Acad. Sci. USA 107 13576-81) for grating interferometry-based x-ray phase contrast CT. We use this relation to derive a simplified acquisition strategy that allows acquiring data with a continuous sample rotation, which can reduce scan time when combined with a fast read-out detector. Besides discussing the theory and the necessary alignment of the experimental setup, we present tomograms obtained with reverse projection retrieval and demonstrate their agreement with those obtained with the conventional EI retrieval.

  11. Development of single shot soft x-ray contact microscopy system for nano-scale dynamics measurement of living biological specimen

    NASA Astrophysics Data System (ADS)

    Kishimoto, Maki; Kado, Masataka; Ishino, Masahiko; Tamotsu, Satoshi; Yasuda, Keiko; Shinohara, Kunio

    2012-07-01

    We have been developing a picosecond single shot soft x-ray contact microscopy system for observing the nanometer-scale inner structure of the living biological specimen in a hydrated condition. The microscopy system consists of an intense IR pump laser system for generating laser-induced plasma as a soft x-ray source and x-ray microscope chamber. The pump laser system employs OPCPA (Optical Parametric Chirped Pulse Amplification) technique to obtain a high contrast pump laser pulse, and we can generate water-window x-rays effectively by combining it to an ultra-thin metal target. The x-ray microscope chamber is composed of a vacuum chamber, a focusing lens, a metal film target, an in-vacuum type sample holder. The pump laser pulse is focused on the metal film target with a focusing lens. The soft x-rays from the laser-induced plasma illuminates bio-specimens on the PMMA photo resist set in the in-vacuum sample holder. The photo resist is developed and the x-ray transmission image recorded on the photo resist is read out by AFM. We took x-ray images of hydrated Leydig cells from mouse testicle and demonstrated that the developed x-ray microscopy system has a spatial resolution of about 100 nm.

  12. Asymmetric and Stochastic Behavior in Magnetic Vortices Studied by Soft X-ray Microscopy

    NASA Astrophysics Data System (ADS)

    Im, Mi-Young

    Asymmetry and stochasticity in spin processes are not only long-standing fundamental issues but also highly relevant to technological applications of nanomagnetic structures to memory and storage nanodevices. Those nontrivial phenomena have been studied by direct imaging of spin structures in magnetic vortices utilizing magnetic transmission soft x-ray microscopy (BL6.1.2 at ALS). Magnetic vortices have attracted enormous scientific interests due to their fascinating spin structures consisting of circularity rotating clockwise (c = + 1) or counter-clockwise (c = -1) and polarity pointing either up (p = + 1) or down (p = -1). We observed a symmetry breaking in the formation process of vortex structures in circular permalloy (Ni80Fe20) disks. The generation rates of two different vortex groups with the signature of cp = + 1 and cp =-1 are completely asymmetric. The asymmetric nature was interpreted to be triggered by ``intrinsic'' Dzyaloshinskii-Moriya interaction (DMI) arising from the spin-orbit coupling due to the lack of inversion symmetry near the disk surface and ``extrinsic'' factors such as roughness and defects. We also investigated the stochastic behavior of vortex creation in the arrays of asymmetric disks. The stochasticity was found to be very sensitive to the geometry of disk arrays, particularly interdisk distance. The experimentally observed phenomenon couldn't be explained by thermal fluctuation effect, which has been considered as a main reason for the stochastic behavior in spin processes. We demonstrated for the first time that the ultrafast dynamics at the early stage of vortex creation, which has a character of classical chaos significantly affects the stochastic nature observed at the steady state in asymmetric disks. This work provided the new perspective of dynamics as a critical factor contributing to the stochasticity in spin processes and also the possibility for the control of the intrinsic stochastic nature by optimizing the design of

  13. Variable magnification with Kirkpatrick-Baez optics for synchrotron X-ray microscopy

    DOE PAGES

    Jach, Terrence; Bakulin, Alex S.; Durbin, Stephen M.; Pedulla, Joseph; Macrander, Albert

    2006-05-01

    In this study, we describe the distinction between the operation of a short focal length x-ray microscope forming a real image with a laboratory source (convergent illumination) and with a highly collimated intense beam from a synchrotron light source (Kohler illumination).

  14. 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.

  15. Soft x-ray microscopy - a powerful analytical tool to image magnetism down to fundamental length and times scales

    SciTech Connect

    Fischer, Peter

    2008-08-01

    The magnetic properties of low dimensional solid state matter is of the utmost interest both scientifically as well as technologically. In addition to the charge of the electron which is the base for current electronics, by taking into account the spin degree of freedom in future spintronics applications open a new avenue. Progress towards a better physical understanding of the mechanism and principles involved as well as potential applications of nanomagnetic devices can only be achieved with advanced analytical tools. Soft X-ray microscopy providing a spatial resolution towards 10nm, a time resolution currently in the sub-ns regime and inherent elemental sensitivity is a very promising technique for that. This article reviews the recent achievements of magnetic soft X-ray microscopy by selected examples of spin torque phenomena, stochastical behavior on the nanoscale and spin dynamics in magnetic nanopatterns. The future potential with regard to addressing fundamental magnetic length and time scales, e.g. imaging fsec spin dynamics at upcoming X-ray sources is pointed out.

  16. Revealing the Role of Catalysts in Carbon Nanotubes and Nanofibers by Scanning Transmission X-ray Microscopy

    PubMed Central

    Gao, Jing; Zhong, Jun; Bai, Lili; Liu, Jinyin; Zhao, Guanqi; Sun, Xuhui

    2014-01-01

    The identification of effective components on the atomic scale in carbon nanomaterials which improve the performance in various applications remains outstanding challenges. Here the catalyst residues in individual carbon nanotube (CNT) and carbon nanofiber (CNF) were clearly imaged with a concurrent characterization of their electronic structure by nanoscale scanning transmission X-ray microscopy. Except for prominent catalyst nanoparticle at the tip, tiny catalyst clusters along the tube (fiber) were detected, indicating a migration of the catalysts with the growth of CNTs (CNFs). The observation provides the direct evidence on the atomic metal in CNT for oxygen reduction reported in the literature. Interaction between catalysts (Fe, Ni) and CNTs (CNFs) at the tip was also identified by comparing the X-ray absorption spectra. A deep understanding of catalyst residues such as Fe or Ni in carbon nanomaterials is very vital to growth mechanism development and practical applications. PMID:24398972

  17. Residual solvent content in conducting polymer-blend films mapped with scanning transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Meier, Robert; Schindler, Markus; Müller-Buschbaum, Peter; Watts, Benjamin

    2011-11-01

    Near-edge x-ray absorption fine-structure spectra prove the presence of solvent molecules in conducting polymer films and are used to calculate the absolute solvent uptake of, e.g., 5 vol.% in poly(vinylcarbazole) (PVK) films, which were prepared by solution casting with cyclohexanone as solvent. Nanoscale scanning transmission x-ray microscopy (STXM) reveals a thickness-independent solvent content in a PVK gradient sample due to the formation of an enrichment layer of residual solvent. In polymer-blend films of PVK and poly(3-hexylthiophene) (P3HT), STXM probes a lateral residual solvent uptake, which depends on the composition of the phase-separation domains. For all measurements, oxygen-containing solvent molecules in oxygen-free conducting polymer films are used as marker material, and a significant amount of residual solvent is found in all types of investigated samples.

  18. Studies of SmCo5/Fe nanocomposite magnetic bilayers with magnetic soft x-ray transmission microscopy

    SciTech Connect

    Shahzad, F.; Siddiqi, S. A.; Im, M.-Y.; Avallone, A.; Fischer, P.; Hussain, Z.; Siddiqi, I.; Hellman, F.; Zhao, J.

    2009-12-04

    A hard/soft SmCo{sub 5}/Fe nanocomposite magnetic bilayer system has been fabricated on X-ray transparent 100-200 nm thin Si{sub 3}N{sub 4} membranes by magnetron sputtering. The microscopic magnetic domain pattern and its behavior during magnetization reversal in the hard and soft magnetic phases have been individually studied by element specific magnetic soft x-ray microscopy at a spatial resolution of better than 25nm. We observe that the domain patterns for soft and hard phases switch coherently throughout the full hysteresis cycle upon applying external magnetic fields. We derived local M(H) curves from the images for Fe and SmCo5 separately and found switching for both hard and soft phases same.

  19. 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.

  20. 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.

  1. Pressure-induced densification in GeO{sub 2} glass: A transmission x-ray microscopy study

    SciTech Connect

    Lin, Yu Zeng, Qiaoshi; Yang, Wenge; Mao, Wendy L.

    2013-12-23

    Nanoscale transmission x-ray microscopy measurements have been performed to determine the effect of pressure (P) on the volume (V) change in GeO{sub 2} glass up to 38.5 GPa. The P-V data show a continuous increase upon compression, indicating that the density-driven structural transformation is a gradual process. Over the pressure range studied, a transition is observed at approximately 10–13 GPa, where the material displays distinct compression behaviors. The pressure-induced densification that involves the coordination number change has been discussed. Using this newly developed high-pressure imaging technique with tens of nanometer resolution, we have provided a direct and unequivocal way for measuring density of amorphous materials to much higher pressures with accuracy rivaling x-ray diffraction of crystalline solids.

  2. Penetrating view of nano-structures in Aleochara verna spermatheca and flagellum by hard X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Zhang, Kai; Li, De-E.; Hong, You-Li; Zhu, Pei-Ping; Yuan, Qing-Xi; Huang, Wan-Xia; Gao, Kun; Zhou, Hong-Zhang; Wu, Zi-Yu

    2013-07-01

    A penetrating view of the three-dimensional nanostructure of female spermatheca and male flagellum in the species Aleochara verna is obtained with 100-nm resolution using a hard X-ray microscope, which provides a fast noninvasive imaging technology for insect morphology. Through introducing Zernike phase contrast and heavy metal staining, images taken at 8 keV displayed sufficient contrast for observing nanoscale fine structures, such as the spermatheca cochleate duct and the subapex of the flagellum, which have some implications for the study of the sperm transfer process and genital evolution in insects. This work shows that both the spatial resolution and the contrast characteristic of hard X-ray microscopy are quite promising for insect morphology studies and, particularly, provide an attractive alternative to the destructive techniques used for investigating internal soft tissues.

  3. Imaging Drosophila brain by combining cryo-soft X-ray microscopy of thick vitreous sections and cryo-electron microscopy of ultrathin vitreous sections.

    PubMed

    Leforestier, Amélie; Levitz, Pierre; Preat, Thomas; Guttmann, Peter; Michot, Laurent J; Tchénio, Paul

    2014-11-01

    Cryo-soft X-ray microscopy is an emerging imaging tool complementary to cryo-electron microscopy, allowing to image frozen hydrated specimens ten to hundred times thicker, but at lower resolution. We describe how the method, so far restricted to isolated small cells or cell monolayers, can be extended to large cells and tissue. We image the synapses of the Kenyon cells in frozen hydrated Drosophila brains combining cryo-soft X-ray microscopy of thick vitreous sections, and cryo-electron microscopy of ultrathin vitreous sections. We show how to obtain frozen hydrated sections of thicknesses ranging from 40 nm up to 2.5 μm, by tuning the sectioning speed of the cryo-microtome. A fluorescent stereo-microscope mounted on the cryo-microtome allowed us to target the regions of interest after GFP-labeling of synapses. Thick cryo-sections were imaged by cryo-soft X-ray microscopy at a resolution better than 25 nm, while ultrathin cryo-sections of the same regions were explored in parallel at the nanometre level of resolution by cryo-electron microscopy.

  4. Phase retrieval using polychromatic illumination for transmission X-ray microscopy.

    PubMed

    Liu, Yijin; Andrews, Joy C; Wang, Junyue; Meirer, Florian; Zhu, Peiping; Wu, Ziyu; Pianetta, Piero

    2011-01-17

    An alternative method for quantitative phase retrieval in a transmission X-ray microscope system at sub-50-nm resolution is presented. As an alternative to moving the sample in the beam direction in order to analyze the propagation-introduced phase effect, we have illuminated the TXM using X-rays of different energy without any motor movement in the TXM system. Both theoretical analysis and experimental studies have confirmed the feasibility and the advantage of our method, because energy tuning can be performed with very high energy resolution using a double crystal monochromator at a synchrotron beam line, and there is zero motor error in TXM system in our approach. High-spatial-resolution phase retrieval is accomplished using the proposed method. PMID:21263593

  5. High-reflectivity Cr/Sc multilayer condenser for compact soft x-ray microscopy

    SciTech Connect

    Stollberg, H.; Yulin, S.; Takman, P. A. C.; Hertz, H. M.

    2006-12-15

    The condenser is a critical component in compact water-window x-ray microscopes as it influences the exposure time via its efficiency and the resolution via its numerical aperture. Normal-incidence multilayer mirrors can reach large geometrical collection efficiencies and match the numerical aperture of the zone plate but require advanced processing for high total reflectivity. In the present article we demonstrate large-diameter normal-incidence spherical Cr/Sc multilayer condensers with high and uniform reflectivity. Dc-magnetron sputtering was used to deposit 300 bilayers of Cr/Sc with a predetermined d-spacing matching the {lambda}=3.374 nm operating wavelength on spherical substrates. The mirrors show a uniform reflectivity of {approx}3% over the full 58 mm diameter condenser area. With these mirrors an improvement in exposure time by a factor of 10 was achieved, thereby improving the performance of the compact x-ray microscope significantly.

  6. 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.

  7. Phase retrieval using polychromatic illumination for transmission X-ray microscopy

    PubMed Central

    Liu, Yijin; Andrews, Joy C.; Wang, Junyue; Meirer, Florian; Zhu, Peiping; Wu, Ziyu; Pianetta, Piero

    2011-01-01

    An alternative method for quantitative phase retrieval in a transmission X-ray microscope system at sub-50-nm resolution is presented. As an alternative to moving the sample in the beam direction in order to analyze the propagation-introduced phase effect, we have illuminated the TXM using X-rays of different energy without any motor movement in the TXM system. Both theoretical analysis and experimental studies have confirmed the feasibility and the advantage of our method, because energy tuning can be performed with very high energy resolution using a double crystal monochromator at a synchrotron beam line, and there is zero motor error in TXM system in our approach. High-spatial-resolution phase retrieval is accomplished using the proposed method. PMID:21263593

  8. Confocal soft X-ray scanning transmission microscopy: setup, alignment procedure and limitations.

    PubMed

    Späth, Andreas; Raabe, Jörg; Fink, Rainer H

    2015-01-01

    Zone-plate-based scanning transmission soft X-ray microspectroscopy (STXM) is a well established technique for high-contrast imaging of sufficiently transparent specimens (e.g. ultrathin biological tissues, polymer materials, archaeometric specimens or magnetic thin films) with spatial resolutions in the regime of 20 nm and high spectroscopic or chemical sensitivity. However, due to the relatively large depth of focus of zone plates, the resolution of STXM along the optical axis so far stays unambiguously behind for thicker X-ray transparent specimens. This challenge can be addressed by the implementation of a second zone plate in the detection pathway of the beam, resulting in a confocal arrangement. Within this paper a first proof-of-principle study for a confocal STXM (cSTXM) and an elaborate alignment procedure in transmission and fluorescence geometry are presented. Based on first confocal soft X-ray micrographs of well known specimens, the advantage and limitation of cSTXM as well as further development potentials for future applications are discussed.

  9. A controlled dispersion parallel wavelength x ray spectrometer for electron microscopy

    NASA Astrophysics Data System (ADS)

    Fiori, C. E.; Wight, S. A.; Romig, A. D., Jr.

    1991-04-01

    A new technique is described for the detection of x rays in electron column instruments used in microanalysis. In electron column instruments, the point source of x rays is produced by the interaction of a focused electron beam with the sample. Neither of the conventional methods, wavelength dispersive (WDS) nor energy dispersive (EDS) based spectrometry, is optimized for low Z element quantitative analysis. In WDS applications, where the analyte elements are Be through P, chemical effects complicate the x ray measurement process. Peak positions and shapes are altered, sometimes very strongly, by the electron configurations of the analyte atoms and neighboring atoms. In these cases, the ideal spectrometer would profile the peak and some small amount of continuum on either side of the peak such that an accurate peak area could be calculated. Present WDS spectrometers are serial in nature and cannot directly measure peak areas, often causing errors in the determination of light element concentrations. Bastin and co-workers have developed an elegant method to provide accurate area determinations, using the serial spectrometer, by a three point procedure. The parallel wavelength dispersive spectrometer (PWDS) proposed here is ideally suited for those applications.

  10. Confocal soft X-ray scanning transmission microscopy: setup, alignment procedure and limitations

    PubMed Central

    Späth, Andreas; Raabe, Jörg; Fink, Rainer H.

    2015-01-01

    Zone-plate-based scanning transmission soft X-ray microspectroscopy (STXM) is a well established technique for high-contrast imaging of sufficiently transparent specimens (e.g. ultrathin biological tissues, polymer materials, archaeometric specimens or magnetic thin films) with spatial resolutions in the regime of 20 nm and high spectroscopic or chemical sensitivity. However, due to the relatively large depth of focus of zone plates, the resolution of STXM along the optical axis so far stays unambiguously behind for thicker X-ray transparent specimens. This challenge can be addressed by the implementation of a second zone plate in the detection pathway of the beam, resulting in a confocal arrangement. Within this paper a first proof-of-principle study for a confocal STXM (cSTXM) and an elaborate alignment procedure in transmission and fluorescence geometry are presented. Based on first confocal soft X-ray micrographs of well known specimens, the advantage and limitation of cSTXM as well as further development potentials for future applications are discussed. PMID:25537596

  11. Cryo X-ray microscopy with high spatial resolution in amplitude and phase contrast.

    PubMed

    Schneider, G

    1998-11-01

    The resolution of transmission X-ray microscopes (TXMs) using zone plate optics is presently about 30 nm. Theory and experiments presented here show that this resolution can be obtained in radiation sensitive hydrated biological material by using shock frozen samples. For this purpose the interaction of X-rays with matter and the image formation with zone plates is described. For the first time the influence of the limited apertures of the condenser and the zone plate objective are in included in calculations of the image contrast, the photon density and radiation dose required for the object illumination. Model considerations show that lowest radiation dose and high image contrast are obtained in optimized phase contrast which exploits absorption as well as phase shift. The damaging effect of the absorbed X-rays is quantitatively evaluated by radiation-induced kinetics showing that cryogenic samples are structurally stable. To verify these theoretical models the TXM was modified to allow imaging of frozen-hydrated samples at atmospheric pressure. Details inside cells and algae as small as 35 nm are visible at 2.4 nm wavelength in amplitude contrast mode. At this resolution the cryogenic samples show no structural changes. As predicted, optimized phase contrast shows structures inside the frozen-hydrated objects with high contrast. Stereo-pair images of algae reveal the 3D organization of the organelles. Element analysis and micro-tomography of whole cryogenic cells are possible. PMID:9836467

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

    NASA Astrophysics Data System (ADS)

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

    2015-10-01

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

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

    PubMed Central

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

    2015-01-01

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

  14. Preliminary Experience With A Charged Selenium Plate Projection X-Ray System

    NASA Astrophysics Data System (ADS)

    Papin, Patrick J.; Mankovich, Nicholas J.; Barbaric, Zoran; Huang, H. K.

    1984-06-01

    Electrostatic imaging techniques provide the means to record x-ray images without the use of film. The conventional screen-film photon receptor is replaced by a charged selenium-oxide plate. After exposure, the plate is scanned with multiple electrometer probes forming a 1024x1024x12 bit digital image from the latent electrostatic image. This imaging modality represents an early entry into the era of true digital radiography, evolving toward a filmless diagnostic imaging facility. This paper discusses the architecture of an experimental charged selenium plate projection digital x-ray system. As well as some preliminary results of the characteristics of a amorphous selenium plate photon receptor exposed to visible light.

  15. The Chandra ACIS Timing Survey Project: glimpsing a sample of faint X-ray pulsators

    NASA Astrophysics Data System (ADS)

    Israel, G. L.; Esposito, P.; Rodríguez Castillo, G. A.; Sidoli, L.

    2016-11-01

    We report on the discovery of 41 new pulsating sources in the data of the Chandra Advanced CCD Imaging Spectrometer, which is sensitive to X-ray photons in the 0.3-10 keV band. The archival data of the first 15 yr of Chandra observations were retrieved and analysed by means of fast Fourier transforms, employing a peak-detection algorithm able to screen candidate signals in an automatic fashion. We carried out the search for new X-ray pulsators in light curves with more than 50 photons, for a total of about 190 000 light curves out of about 430 000 extracted. With these numbers, the ChAndra Timing Survey at Brera And Roma astronomical observatories (CATS @ BAR) - as we called the project - represents the largest ever systematic search for coherent signals in the classic X-ray band. More than 50 per cent of the signals were confirmed by further Chandra (for those sources with two or more pointings), XMM-Newton or ROSAT data. The period distribution of the new X-ray pulsators above ˜2000 s resembles that of cataclysmic variables, while there is a paucity of sources with shorter period and low fluxes. Since there is not an obvious bias against these detections, a possible interpretation is in terms of a magnetic gating mechanism in accreting neutron stars. Finally, we note that CATS @ BAR is a living project and the detection algorithm will continue to be routinely applied to the new Chandra data as they become public. Based on the results obtained so far, we expect to discover about three new pulsators every year.

  16. High resolution imaging of the ultrastructure of living algal cells using soft x-ray contact microscopy

    SciTech Connect

    Ford, T.W.; Cotton, R.A.; Page, A.M.; Tomie, T.; Majima, T.; Stead, A.D.

    1995-12-31

    Soft x-ray contact microscopy provides the biologist with a technique for examining the ultrastructure of living cells at a much higher resolution than that possible by various forms of light microscopy. Readout of the developed photoresist using atomic force microscopy (AFM) produces a detailed map of the carbon densities generated in the resist following exposure of the specimen to water-window soft x-rays (2--4nm) produced by impact of a high energy laser onto a suitable target. The established high resolution imaging method of transmission electron microscopy (TEM) has inherent problems in the chemical pre-treatment required for producing the ultrathin sections necessary for this technique. Using the unicellular green alga Chlamydomonas the ultrastructural appearance of the cells following SXCM and TEM has been compared. While SXCM confirms the basic structural organization of the cell as seen by TEM (e.g., the organization of the thylakoid membranes within the chloroplast; flagellar insertion into the cytoplasm), there are important differences. These are in the appearance of the cell covering and the presence of carbon-dense spherical cellular inclusions.

  17. Development of achromatic full-field hard x-ray microscopy and its application to x-ray absorption near edge structure spectromicroscopy

    NASA Astrophysics Data System (ADS)

    Matsuyama, S.; Emi, Y.; Kino, H.; Kohmura, Y.; Yabashi, M.; Ishikawa, T.; Yamauchi, K.

    2014-09-01

    An achromatic and high-resolution hard X-ray microscope was developed, in which advanced Kirkpatrick-Baez mirror optics with four total-reflection mirrors was employed as an objective. A fine test pattern with a 100 nm feature size could successfully be resolved. Full-field imaging, in combination with X-ray absorption near edge structure (XANES) spectroscopy, was used to characterize tungsten particles. XANES spectra were obtained over the entire observation area, showing good agreement with the XANES spectrum of pure tungsten.

  18. 3D ablation catheter localisation using individual C-arm x-ray projections

    NASA Astrophysics Data System (ADS)

    Haase, C.; Schäfer, D.; Dössel, O.; Grass, M.

    2014-11-01

    Cardiac ablation procedures during electrophysiology interventions are performed under x-ray guidance with a C-arm imaging system. Some procedures require catheter navigation in complex anatomies like the left atrium. Navigation aids like 3D road maps and external tracking systems may be used to facilitate catheter navigation. As an alternative to external tracking a fully automatic method is presented here that enables the calculation of the 3D location of the ablation catheter from individual 2D x-ray projections. The method registers a high resolution, deformable 3D attenuation model of the catheter to a 2D x-ray projection. The 3D localization is based on the divergent beam projection of the catheter. On an individual projection, the catheter tip is detected in 2D by image filtering and a template matching method. The deformable 3D catheter model is adapted using the projection geometry provided by the C-arm system and 2D similarity measures for an accurate 2D/3D registration. Prior to the tracking and registration procedure, the deformable 3D attenuation model is automatically extracted from a separate 3D cone beam CT reconstruction of the device. The method can hence be applied to various cardiac ablation catheters. In a simulation study of a virtual ablation procedure with realistic background, noise, scatter and motion blur an average 3D registration accuracy of 3.8 mm is reached for the catheter tip. In this study four different types of ablation catheters were used. Experiments using measured C-arm fluoroscopy projections of a catheter in a RSD phantom deliver an average 3D accuracy of 4.5 mm.

  19. 3D ablation catheter localisation using individual C-arm x-ray projections.

    PubMed

    Haase, C; Schäfer, D; Dössel, O; Grass, M

    2014-11-21

    Cardiac ablation procedures during electrophysiology interventions are performed under x-ray guidance with a C-arm imaging system. Some procedures require catheter navigation in complex anatomies like the left atrium. Navigation aids like 3D road maps and external tracking systems may be used to facilitate catheter navigation. As an alternative to external tracking a fully automatic method is presented here that enables the calculation of the 3D location of the ablation catheter from individual 2D x-ray projections. The method registers a high resolution, deformable 3D attenuation model of the catheter to a 2D x-ray projection. The 3D localization is based on the divergent beam projection of the catheter. On an individual projection, the catheter tip is detected in 2D by image filtering and a template matching method. The deformable 3D catheter model is adapted using the projection geometry provided by the C-arm system and 2D similarity measures for an accurate 2D/3D registration. Prior to the tracking and registration procedure, the deformable 3D attenuation model is automatically extracted from a separate 3D cone beam CT reconstruction of the device. The method can hence be applied to various cardiac ablation catheters. In a simulation study of a virtual ablation procedure with realistic background, noise, scatter and motion blur an average 3D registration accuracy of 3.8 mm is reached for the catheter tip. In this study four different types of ablation catheters were used. Experiments using measured C-arm fluoroscopy projections of a catheter in a RSD phantom deliver an average 3D accuracy of 4.5 mm.

  20. Synchrotron-based in situ soft X-ray microscopy of Ag corrosion in aqueous chloride solution

    NASA Astrophysics Data System (ADS)

    Bozzini, B.; D'Urzo, L.; Gianoncelli, A.; Kaulich, B.; Kiskinova, M.; Prasciolu, M.; Tadjeddine, A.

    2009-09-01

    In this paper we report an in situ X-ray microscopy study of a model metal electrochemistry system, incorporating faradaic reactivity: the anodic corrosion and cathodic electrodeposition of Ag in aqueous systems. The information at sub-μm scale about morpho-chemical evolution of the electrified interface, provided by this novel electroanalytical approach fosters fundamental understanding of important issues concerning material fabrication and stability, which are crucial in developing the next generation electrochemical technologies, such as fuel cells and biosensors. The key methodology challenge faced in this pilot electrochemical experiments is combining a three-electrode configuration and wet environment, which required metal electrodes suitable for transmitting soft X-rays and a sealed cell allowing working in high vacuum. This has been solved via lithographic fabrication route fabricating 75 nm thick Ag electrodes and using Si3N4 membranes as X-ray windows and electrode support. Imaging in the STXM mode with phase contrast allowed us to monitor the corrosion morphologies and metal outgrowth features. Localised thickness variation and the build-up of reaction products of electron density different from that of the starting material have been detected with high sensitivity.

  1. TXM-Wizard: a program for advanced data collection and evaluation in full-field transmission X-ray microscopy.

    PubMed

    Liu, Yijin; Meirer, Florian; Williams, Phillip A; Wang, Junyue; Andrews, Joy C; Pianetta, Piero

    2012-03-01

    Transmission X-ray microscopy (TXM) has been well recognized as a powerful tool for non-destructive investigation of the three-dimensional inner structure of a sample with spatial resolution down to a few tens of nanometers, especially when combined with synchrotron radiation sources. Recent developments of this technique have presented a need for new tools for both system control and data analysis. Here a software package developed in MATLAB for script command generation and analysis of TXM data is presented. The first toolkit, the script generator, allows automating complex experimental tasks which involve up to several thousand motor movements. The second package was designed to accomplish computationally intense tasks such as data processing of mosaic and mosaic tomography datasets; dual-energy contrast imaging, where data are recorded above and below a specific X-ray absorption edge; and TXM X-ray absorption near-edge structure imaging datasets. Furthermore, analytical and iterative tomography reconstruction algorithms were implemented. The compiled software package is freely available. PMID:22338691

  2. Dear-Mama: A photon counting X-ray imaging project for medical applications

    NASA Astrophysics Data System (ADS)

    Blanchot, G.; Chmeissani, M.; Díaz, A.; Díaz, F.; Fernández, J.; García, E.; García, J.; Kainberger, F.; Lozano, M.; Maiorino, M.; Martínez, R.; Montagne, J. P.; Moreno, I.; Pellegrini, G.; Puigdengoles, C.; Sentís, M.; Teres, L.; Tortajada, M.; Ullán, M.

    2006-12-01

    Dear-Mama ( Detection of Early Markers in Mammography) is an EU funded project devoted to develop an X-ray Medical imaging device based on room temperature solid-state pixel detector coupled to photon counting readout electronics via bump bonding. The technology being used leads to signal-to-noise ratio enhancement and thus the ability to detect low contrast anomalies such as micro-calcifications. The Dear-Mama machine is currently being evaluated and preliminary results show an excellent MTF response. Dear-Mama consortium is made up from six European institutions, the project runs from December 2001 to March 2006.

  3. Method and apparatus for multiple-projection, dual-energy x-ray absorptiometry scanning

    NASA Technical Reports Server (NTRS)

    Charles, Jr., Harry K. (Inventor); Beck, Thomas J. (Inventor); Feldmesser, Howard S. (Inventor); Magee, Thomas C. (Inventor)

    2007-01-01

    Methods and apparatuses for advanced, multiple-projection, dual-energy X-ray absorptiometry scanning systems include combinations of a conical collimator; a high-resolution two-dimensional detector; a portable, power-capped, variable-exposure-time power supply; an exposure-time control element; calibration monitoring; a three-dimensional anti-scatter-grid; and a gantry-gantry base assembly that permits up to seven projection angles for overlapping beams. Such systems are capable of high precision bone structure measurements that can support three dimensional bone modeling and derivations of bone strength, risk of injury, and efficacy of countermeasures among other properties.

  4. Image reconstruction from limited angle projections collected by multisource interior x-ray imaging systems

    NASA Astrophysics Data System (ADS)

    Liu, Baodong; Wang, Ge; Ritman, Erik L.; Cao, Guohua; Lu, Jianping; Zhou, Otto; Zeng, Li; Yu, Hengyong

    2011-10-01

    A multisource x-ray interior imaging system with limited angle scanning is investigated to study the possibility of building an ultrafast micro-CT for dynamic small animal imaging, and two methods are employed to perform interior reconstruction from a limited number of projections collected by the multisource interior x-ray system. The first is total variation minimization with the steepest descent search (TVM-SD) and the second is total difference minimization with soft-threshold filtering (TDM-STF). Comprehensive numerical simulations and animal studies are performed to validate the associated reconstructed methods and demonstrate the feasibility and application of the proposed system configuration. The image reconstruction results show that both of the two reconstruction methods can significantly improve the image quality and the TDM-SFT is slightly superior to the TVM-SD. Finally, quantitative image analysis shows that it is possible to make an ultrafast micro-CT using a multisource interior x-ray system scheme combined with the state-of-the-art interior tomography.

  5. Image reconstruction from limited angle projections collected by multisource interior x-ray imaging systems.

    PubMed

    Liu, Baodong; Wang, Ge; Ritman, Erik L; Cao, Guohua; Lu, Jianping; Zhou, Otto; Zeng, Li; Yu, Hengyong

    2011-10-01

    A multisource x-ray interior imaging system with limited angle scanning is investigated to study the possibility of building an ultrafast micro-CT for dynamic small animal imaging, and two methods are employed to perform interior reconstruction from a limited number of projections collected by the multisource interior x-ray system. The first is total variation minimization with the steepest descent search (TVM-SD) and the second is total difference minimization with soft-threshold filtering (TDM-STF). Comprehensive numerical simulations and animal studies are performed to validate the associated reconstructed methods and demonstrate the feasibility and application of the proposed system configuration. The image reconstruction results show that both of the two reconstruction methods can significantly improve the image quality and the TDM-SFT is slightly superior to the TVM-SD. Finally, quantitative image analysis shows that it is possible to make an ultrafast micro-CT using a multisource interior x-ray system scheme combined with the state-of-the-art interior tomography.

  6. An assessment of the resolution limitation due to radiation-damage in X-ray diffraction microscopy

    DOE PAGES

    Howells, M. R.; Beetz, T.; Chapman, H. N.; Cui, C.; Holton, J. M.; Jacobsen, C. J.; Kirz, J.; Lima, E.; Marchesini, S.; Miao, H.; et al

    2008-11-17

    X-ray diffraction microscopy (XDM) is a new form of x-ray imaging that is being practiced at several third-generation synchrotron-radiation x-ray facilities. Nine years have elapsed since the technique was first introduced and it has made rapid progress in demonstrating high-resolution three-dimensional imaging and promises few-nm resolution with much larger samples than can be imaged in the transmission electron microscope. Both life- and materials-science applications of XDM are intended, and it is expected that the principal limitation to resolution will be radiation damage for life science and the coherent power of available x-ray sources for material science. In this paper wemore » address the question of the role of radiation damage. We use a statistical analysis based on the so-called "dose fractionation theorem" of Hegerl and Hoppe to calculate the dose needed to make an image of a single life-science sample by XDM with a given resolution. We find that for simply-shaped objects the needed dose scales with the inverse fourth power of the resolution and present experimental evidence to support this finding. To determine the maximum tolerable dose we have assembled a number of data taken from the literature plus some measurements of our own which cover ranges of resolution that are not well covered otherwise. The conclusion of this study is that, based on the natural contrast between protein and water and "Rose-criterion" image quality, one should be able to image a frozen-hydrated biological sample using XDM at a resolution of about 10 nm.« less

  7. An assessment of the resolution limitation due to radiation-damage in X-ray diffraction microscopy

    SciTech Connect

    Howells, M. R.; Beetz, T.; Chapman, H. N.; Cui, C.; Holton, J. M.; Jacobsen, C. J.; Kirz, J.; Lima, E.; Marchesini, S.; Miao, H.; Sayre, D.; Shapiro, D. A.; Spence, J. C.H.; Starodub, D.

    2008-11-17

    X-ray diffraction microscopy (XDM) is a new form of x-ray imaging that is being practiced at several third-generation synchrotron-radiation x-ray facilities. Nine years have elapsed since the technique was first introduced and it has made rapid progress in demonstrating high-resolution three-dimensional imaging and promises few-nm resolution with much larger samples than can be imaged in the transmission electron microscope. Both life- and materials-science applications of XDM are intended, and it is expected that the principal limitation to resolution will be radiation damage for life science and the coherent power of available x-ray sources for material science. In this paper we address the question of the role of radiation damage. We use a statistical analysis based on the so-called "dose fractionation theorem" of Hegerl and Hoppe to calculate the dose needed to make an image of a single life-science sample by XDM with a given resolution. We find that for simply-shaped objects the needed dose scales with the inverse fourth power of the resolution and present experimental evidence to support this finding. To determine the maximum tolerable dose we have assembled a number of data taken from the literature plus some measurements of our own which cover ranges of resolution that are not well covered otherwise. The conclusion of this study is that, based on the natural contrast between protein and water and "Rose-criterion" image quality, one should be able to image a frozen-hydrated biological sample using XDM at a resolution of about 10 nm.

  8. In-situ synchrotron x-ray transmission microscopy of the sintering of multilayers

    NASA Astrophysics Data System (ADS)

    Yan, Zilin; Guillon, Olivier; Martin, Christophe L.; Wang, Steve; Lee, Chul-Seung; Bouvard, Didier

    2013-06-01

    This letter reports on in-situ characterization of the high temperature sintering of multilayer ceramic capacitors by high-resolution synchrotron x-ray imaging. Microstructural evolution was obtained in real time by a continuous recording of 2-dimensional radiographs. Anisotropic strains were measured for different layers. Quantification of defects was conducted with 3-dimensional nano-computed tomography. These in-situ observations prove that electrode discontinuities occur at the early stage of sintering and originate from initial heterogeneities linked to the particulate nature of the starting powders.

  9. Measuring inside damage of individual multi-walled carbon nanotubes using scanning transmission X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Liu, Jinyin; Bai, Lili; Wang, Jian; Zhao, Guanqi; Sun, Xuhui; Zhong, Jun

    2014-06-01

    The electronic structure of individual multi-walled carbon nanotubes (MWCNTs) has been probed using scanning transmission X-ray microscopy (STXM). Although transmission electron microscope (TEM) images show that the exterior of the MWCNTs are clean and straight; the inside structure of some of the MWCNTs is much less well ordered, as revealed by STXM. The amorphization of the interior tubes can be introduced in the growth or modification processes. Moreover, TEM measurement with high dose may also lead to the inside damage. Our results reveal that the structure of individual MWCNTs can be complex and suggest that electronic structure measurements are an important tool for characterizing carbon nanomaterials.

  10. Observation of field-induced domain wall propagation in magnetic nanowires by magnetic transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Bryan, M. T.; Fry, P. W.; Fischer, P. J.; Allwood, D. A.

    2008-04-01

    Magnetic transmission x-ray microscopy (M-TXM) is used to image domain walls in magnetic ring structures formed by a 300nm wide, 24nm thick Ni81Fe19 nanowire. Both transverse- and vortex-type domain walls are observed after application of different field sequences. Domain walls can be observed by comparing images obtained from opposite field sequences or else domain wall propagation observed by comparing successive images in a particular field sequence. This demonstrates the potential use of M-TXM in developing and understanding planar magnetic nanowire behavior.

  11. Observation of Thermomagnetically Recorded Magnetic Domains in TbFeCo Films with Soft X-Ray Microscopy

    NASA Astrophysics Data System (ADS)

    Takagi, Naoyuki; Fischer, Peter; Tsunashima, Shigeru; Kumazawa, Masayuki; Ishida, Hiroki; Yamaguchi, Atsushi; Noguchi, Hitoshi; Kume, Minoru

    2001-04-01

    We observed thermomagnetically recorded domains of various sizes with magnetic transmission X-ray microscopy (M-TXM) in order to clarify the recording characteristics. The domains were recorded on TbFeCo films by laser-pumped magnetic field modulation (LP-MFM) using a 635 nm laser diode. Typical images of magnetic domains in TbFeCo films were taken at the Fe L3-edge, and it was confirmed that the crescent-shaped domains could be recorded with high quality for mark lengths down to 100 nm.

  12. Measuring inside damage of individual multi-walled carbon nanotubes using scanning transmission X-ray microscopy

    SciTech Connect

    Liu, Jinyin; Bai, Lili; Zhao, Guanqi; Sun, Xuhui E-mail: jzhong@suda.edu.cn; Zhong, Jun E-mail: jzhong@suda.edu.cn; Wang, Jian

    2014-06-16

    The electronic structure of individual multi-walled carbon nanotubes (MWCNTs) has been probed using scanning transmission X-ray microscopy (STXM). Although transmission electron microscope (TEM) images show that the exterior of the MWCNTs are clean and straight; the inside structure of some of the MWCNTs is much less well ordered, as revealed by STXM. The amorphization of the interior tubes can be introduced in the growth or modification processes. Moreover, TEM measurement with high dose may also lead to the inside damage. Our results reveal that the structure of individual MWCNTs can be complex and suggest that electronic structure measurements are an important tool for characterizing carbon nanomaterials.

  13. Observation of field-induced domain wall propagation in magnetic nanowires by magnetic transmission X-ray microscopy

    SciTech Connect

    Bryan, M. T.; Fry, P. W.; Fischer, P.; Allwood, D. A.

    2007-12-01

    Magnetic transmission X-ray microscopy (M-TXM) is used to image domain walls in magnetic ring structures formed by a 300 nm wide, 24 nm thick Ni{sub 81}Fe{sub 19} nanowire. Both transverse and vortex type domain walls are observed after application of different field sequences. Domain walls can be observed by comparing images obtained from opposite field sequences, or else domain wall propagation observed by comparing successive images in a particular field sequence. This demonstrates the potential use of M-TXM in developing and understanding planar magnetic nanowire behavior.

  14. The application of x-ray diffraction and electron microscopy to the study of human peripheral nerve obtained by biopsy.

    PubMed

    FINEAN, J B; WOOLF, A L

    1961-03-01

    Human peripheral nerves obtained by biopsy from patients suffering from neuromuscular disorders have been studied by x-ray diffraction and electron microscopy. Few abnormal diffraction patterns have yet been recorded and their significance is not yet established. Electron micrographs have revealed wide variations in the numbers of myelinated fibres included in the nerve trunks and have facilitated a detailed study of the Schwann cell-axon relationships in the large numbers of unmyelinated fibres always present. Some indications of demyelination have been encountered.

  15. Scanning X-ray strain microscopy of inhomogeneously strained Ge micro-bridges

    PubMed Central

    Etzelstorfer, Tanja; Süess, Martin J.; Schiefler, Gustav L.; Jacques, Vincent L. R.; Carbone, Dina; Chrastina, Daniel; Isella, Giovanni; Spolenak, Ralph; Stangl, Julian; Sigg, Hans; Diaz, Ana

    2014-01-01

    Strained semiconductors are ubiquitous in microelectronics and microelectromechanical systems, where high local stress levels can either be detrimental for their integrity or enhance their performance. Consequently, local probes for elastic strain are essential in analyzing such devices. Here, a scanning X-ray sub-microprobe experiment for the direct measurement of deformation over large areas in single-crystal thin films with a spatial resolution close to the focused X-ray beam size is presented. By scanning regions of interest of several tens of micrometers at different rocking angles of the sample in the vicinity of two Bragg reflections, reciprocal space is effectively mapped in three dimensions at each scanning position, obtaining the bending, as well as the in-plane and out-of-plane strain components. Highly strained large-area Ge structures with applications in optoelectronics are used to demonstrate the potential of this technique and the results are compared with finite-element-method models for validation. PMID:24365924

  16. THE CHANDRA CARINA COMPLEX PROJECT: DECIPHERING THE ENIGMA OF CARINA'S DIFFUSE X-RAY EMISSION

    SciTech Connect

    Townsley, Leisa K.; Broos, Patrick S.; Garmire, Gordon P.; Chu, You-Hua; Gruendl, Robert A.; Gagne, Marc; Hamaguchi, Kenji; Montmerle, Thierry; Naze, Yael; Oey, M. S.; Park, Sangwook; Petre, Robert; Pittard, Julian M.

    2011-05-01

    We present a 1.42 deg{sup 2} mosaic of diffuse X-ray emission in the Great Nebula in Carina from the Chandra X-ray Observatory Advanced CCD Imaging Spectrometer camera. After removing >14,000 X-ray point sources from the field, we smooth the remaining unresolved emission, tessellate it into segments of similar apparent surface brightness, and perform X-ray spectral fitting on those tessellates to infer the intrinsic properties of the X-ray-emitting plasma. By modeling faint resolved point sources, we estimate the contribution to the extended X-ray emission from unresolved point sources and show that the vast majority of Carina's unresolved X-ray emission is truly diffuse. Line-like correlated residuals in the X-ray spectral fits suggest that substantial X-ray emission is generated by charge exchange at the interfaces between Carina's hot, rarefied plasma and its many cold neutral pillars, ridges, and clumps.

  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. In situ azimuthal rotation device for linear dichroism measurements in scanning transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Hernández-Cruz, D.; Hitchcock, A. P.; Tyliszczak, T.; Rousseau, M.-E.; Pézolet, M.

    2007-03-01

    A novel miniature rotation device used in conjunction with a scanning transmission x-ray microscope is described. It provides convenient in situ sample rotation to enable measurements of linear dichroism at high spatial resolution. The design, fabrication, and mechanical characterization are presented. This device has been used to generate quantitative maps of the spatial distribution of the orientation of proteins in several different spider and silkworm silks. Specifically, quantitative maps of the dichroic signal at the C 1s→π*amide transition in longitudinal sections of the silk fibers give information about the spatial orientation, degree of alignment, and spatial distribution of protein peptide bonds. A new approach for analyzing the dichroic signal to extract orientation distributions, in addition to magnitudes of aligned components, is presented and illustrated with results from Nephila clavipes dragline spider silk measured using the in situ rotation device.

  19. 3D X-ray Strain Microscopy in Two-Phase Composites at Submicron Length Scale

    SciTech Connect

    Barabash, Rozaliya; Bei, Hongbin; Ice, Gene E; Gao, Yanfei; Barabash, Oleg M

    2011-01-01

    Author note: Part of this research summary is based on findings first reported in Refs. [3-5, 18]. Renewed interest in composite materials is driven by the fact that their mechanical properties can be superior to those of individual constituent phases. Interfaces between the phases are the key elements responsible for the unique micro-mechanisms of plastic deformation in composites. In this study the depth-dependent residual strain distributed in the two phases and partitioned across the composite interfaces is directly measured at submicron length-scale using X-ray microdiffraction and compared to a detailed simulation within the framework of micromechanical stress analysis. Interface strength is determined from the analysis of the so-called slip zone caused by the near-surface stress relaxation. Two examples are discussed including NiAl/Mo and Ni/Mo composites.

  20. X-ray propagation microscopy of biological cells using waveguides as a quasipoint source

    SciTech Connect

    Giewekemeyer, K.; Krueger, S. P.; Kalbfleisch, S.; Bartels, M.; Salditt, T.; Beta, C.

    2011-02-15

    We have used x-ray waveguides as highly confining optical elements for nanoscale imaging of unstained biological cells using the simple geometry of in-line holography. The well-known twin-image problem is effectively circumvented by a simple and fast iterative reconstruction. The algorithm which combines elements of the classical Gerchberg-Saxton scheme and the hybrid-input-output algorithm is optimized for phase-contrast samples, well-justified for imaging of cells at multi-keV photon energies. The experimental scheme allows for a quantitative phase reconstruction from a single holographic image without detailed knowledge of the complex illumination function incident on the sample, as demonstrated for freeze-dried cells of the eukaryotic amoeba Dictyostelium discoideum. The accessible resolution range is explored by simulations, indicating that resolutions on the order of 20 nm are within reach applying illumination times on the order of minutes at present synchrotron sources.

  1. Following Dynamic Processes by X-ray Tomographic Microscopy with Sub-second Temporal Resolution

    SciTech Connect

    Mokso, R.; Marone, F.; Mikuljan, G.; Isenegger, A.; Haberthuer, D.; Schittny, J. C.; Stampanoni, M.

    2011-09-09

    Several non-destructive imaging techniques offer the possibility to observe rapid phenomena in real time, yet most of these techniques fail when it comes to bulky samples and micrometer precision in three dimensions. Therefore there is clearly a need to develop approaches that address such conditions. We identified the large potential that lies in synchrotron-based x-rays as a probe and developed a direct-space tomographic instrument suitable to provide sub-second temporal resolution with several-micrometers spatial resolution. Selected applications from the field of biology and material science are shown in order to demonstrate the unique capabilities in generating three-dimensional images with very high quality making image segmentation and analysis possible for samples that could, until now, only be studied in two dimensions due to the occurrence of rapid structural changes.

  2. A new detector system for low energy X-ray fluorescence coupled with soft X-ray microscopy: First tests and characterization

    NASA Astrophysics Data System (ADS)

    Gianoncelli, Alessandra; Bufon, Jernej; Ahangarianabhari, Mahdi; Altissimo, Matteo; Bellutti, Pierluigi; Bertuccio, Giuseppe; Borghes, Roberto; Carrato, Sergio; Cautero, Giuseppe; Fabiani, Sergio; Giacomini, Gabriele; Giuressi, Dario; Kourousias, George; Menk, Ralf Hendrik; Picciotto, Antonino; Piemonte, Claudio; Rachevski, Alexandre; Rashevskaya, Irina; Stolfa, Andrea; Vacchi, Andrea; Zampa, Gianluigi; Zampa, Nicola; Zorzi, Nicola

    2016-04-01

    The last decades have witnessed substantial efforts in the development of several detector technologies for X-ray fluorescence (XRF) applications. In spite of the increasing trend towards performing, cost-effective and reliable XRF systems, detectors for soft X-ray spectroscopy still remain a challenge, requiring further study, engineering and customization in order to yield effective and efficient systems. In this paper we report on the development, first characterization and tests of a novel multielement detector system based on low leakage current silicon drift detectors (SDD) coupled to ultra low noise custom CMOS preamplifiers for synchrotron-based low energy XRF. This new system exhibits the potential for improving the count rate by at least an order of magnitude resulting in ten-fold shorter dwell time at an energy resolution similar to that of single element silicon drift detectors.

  3. Metal artifacts reduction in x-ray CT based on segmentation and forward-projection.

    PubMed

    Nawaz, Shoukat; Fu, Jian; Fan, Dekai

    2014-01-01

    X-ray computed tomography (CT) is a powerful clinical diagnosis tool and has been used widely in many clinical and biological settings. Metal artifacts, caused by high density implants, are commonly encountered in clinical CT applications, thereby affecting the detection of abnormal structures and undermining CT's diagnostic value. In this paper, we developed a metal artifact reduction approach based on image segmentation and forward-projection. We further demonstrate the usefulness of our approach by using a biomedical specimen consisting of muscles, bones and metals. Our aim is to remove the inaccurate metal artifact pixels in the original CT slices and exactly reconstruct the soft-tissue using the forward projections with no metal information. During the reconstruction, artifacts are reduced by replacing the metal projection using the forward projection. The presented work is of interest for CT biomedical applications.

  4. Projection effects in X-ray cores of cooling flow galaxy clusters

    NASA Astrophysics Data System (ADS)

    Ettori, Stefano

    2002-03-01

    Recent analyses of Newton-XMM and Chandra data of the cores of X-ray bright clusters of galaxies show that modelling with a multi-phase gas in which several temperatures and densities are in equilibrium might not be appropriate. Instead, a single-phase model seems able to reproduce properly the spectra collected in annuli from the central region. The measured single-phase temperature profiles indicate a steep positive gradient in the central 100-200kpc and the gas density shows a flat profile in the central few 10s of kpc. Given this observational evidence, we estimate the contribution to the projected-on-the-sky rings from the cluster emissivity as function of the shell volume fraction sampled. We show that the observed projected X-ray emission mimics the multi-phase status of the plasma even though the input distribution is single-phase. This geometrical projection affects (i) analyses of data where insufficient spatial resolution is accessible, (ii) the central bin when its dimension is comparable to the extension of any flatness in the central gas density profile.

  5. High-Energy Nanoscale-Resolution X-ray Microscopy Based on Refractive Optics on a Long Beamline

    SciTech Connect

    Snigireva, I.; Vaughan, G. B. M.; Snigirev, A.

    2011-09-09

    The long length and good coherence properties of ID11 at the ESRF have led to the development of x-ray microscopy based on compound refractive lenses (CRLs). For the highest resolution full-field microscopy, the sample is placed {approx}40 m from the source, which can be micro-focused by a transfocator as a condenser. Due to the long length of the beamline and consequent long sample-detector distance, a CRL objective can be placed up to a meter behind the sample and still allow for magnification of 60x on a detector located at 99 m--enough to achieve easily 100-nm resolution with a typical high-resolution detector.

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

    PubMed

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

    2016-09-01

    penetration by nanoradiators. In conclusion, the combined use of a synchrotron X-ray microbeam-irradiated three-dimensional ROS gel and confocal laser scanning fluorescence microscopy provides a simple dosimetry method for track analysis of X-ray photoelectric nanoradiator radiation, suggesting extensive cellular damage with dose-enhancement beyond a single cell containing IONs.

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

    PubMed

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

    2016-09-01

    penetration by nanoradiators. In conclusion, the combined use of a synchrotron X-ray microbeam-irradiated three-dimensional ROS gel and confocal laser scanning fluorescence microscopy provides a simple dosimetry method for track analysis of X-ray photoelectric nanoradiator radiation, suggesting extensive cellular damage with dose-enhancement beyond a single cell containing IONs. PMID:27577774

  8. The EXTraS project: Exploring the X-ray Transient and variable Sky

    NASA Astrophysics Data System (ADS)

    Tiengo, Andrea

    Modern soft X-ray observatories can yield unique insights into time domain astrophysics. Indeed, a huge amount of information is stored - and largely unexploited - in data archives. The EXTraS project will harvest the hitherto unexplored temporal domain information buried in the serendipitous data collected by the European Photon Imaging Camera (EPIC) instrument onboard the ESA XMM-Newton mission in more than 13 yr of observations. This will include a search for fast transients, missed by standard image analysis, as well as a search and characterization of variability (both periodical and aperiodical) in hundreds of thousands of sources spanning more than nine orders of magnitude in time scale (from <1 s to >10 yr) and six orders of magnitude in flux (from 10(-9) to 10(-15) erg cm(-2) s(-1) in 0.2-12 keV). X-ray results will be complemented by multiwavelength characterization of all previously undetected sources. Phenomenological classification of variable sources will also be performed. All our results will be made available to the community in a public catalogue, together with new analysis tools. The EXTraS project, funded within the EU/FP7-Cooperation Space framework, is carried out by a collaboration including INAF (Italy), IUSS (Italy), CNR/IMATI (Italy), University of Leicester (UK), MPE (Germany) and ECAP (Germany).

  9. Hard x-ray contact microscopy with 250 nm spatial resolution using a LiF film detector and a tabletop microsource

    SciTech Connect

    Almaviva, S.; Bonfigli, F.; Franzini, I.; Lai, A.; Montereali, R. M.; Pelliccia, D.; Cedola, A.; Lagomarsino, S.

    2006-07-31

    An innovative route for deep-submicrometer spatial resolution hard x-ray microscopy with tabletop x-ray source is proposed. A film of lithium fluoride (LiF) was used as imaging detector in contact mode. We present here the x-ray images recorded on LiF films of a Fresnel zone plate with submicrometer gold structures and of an onion cataphyll. The images were read with an optical confocal microscope in fluorescence mode. The measured spatial resolution was about 250 nm, i.e., close to the resolution limit of the confocal microscope. The advantages and drawbacks, and the possible improvements, of this route are discussed.

  10. Hard x-ray contact microscopy with 250 nm spatial resolution using a LiF film detector and a tabletop microsource

    NASA Astrophysics Data System (ADS)

    Almaviva, S.; Bonfigli, F.; Franzini, I.; Lai, A.; Montereali, R. M.; Pelliccia, D.; Cedola, A.; Lagomarsino, S.

    2006-07-01

    An innovative route for deep-submicrometer spatial resolution hard x-ray microscopy with tabletop x-ray source is proposed. A film of lithium fluoride (LiF) was used as imaging detector in contact mode. We present here the x-ray images recorded on LiF films of a Fresnel zone plate with submicrometer gold structures and of an onion cataphyll. The images were read with an optical confocal microscope in fluorescence mode. The measured spatial resolution was about 250nm, i.e., close to the resolution limit of the confocal microscope. The advantages and drawbacks, and the possible improvements, of this route are discussed.

  11. Experimental analysis of high-resolution soft x-ray microscopy

    SciTech Connect

    Chao, Weilun; Anderson, Erik H.; Denbeaux, Gregory; Harteneck, Bruce; Pearson, Angelic L.; Olynick, Deirdre; Schneider, Gerd; Attwood, David

    2001-09-06

    The soft x-ray, full-field microscope XM-1 at Lawrence Berkeley National Laboratory's (LBNL) Advanced Light Source has already demonstrated its capability to resolve 25-nm features. This was accomplished using a micro zone plate (MZP) with an outer zone width of 25 nm. Limited by the aspect ratio of the resist used in the fabrication, the gold-plating thickness of that zone plate is around 40 nm. However, some applications, in particular, biological imaging, prefer improved efficiency, which can be achieved by high-aspect-ratio zone plates. We accomplish this by using a bilayer-resist process in the zone plate fabrication. As our first attempt, a 40-nm-outer-zone-width MZP with a nickel-plating thickness of 150 nm (aspect ratio of 4:1) was successfully fabricated. Relative to the 25-nm MZP, this zone plate is ten times more efficient. Using this high-efficiency MZP, a line test pattern with half period of 30 nm is resolved by the microscope at photon energy of 500 eV. Furthermore, with a new multilayer mirror, the XM-1 can now perform imaging up to 1.8 keV. An image of a line test pattern with half period of 40 nm has a measured modulation of 90%. The image was taken at 1.77 keV with the high-efficiency MZP with an outer zone width of 35 nm and a nickel-plating thickness of 180 nm (aspect ratio of 5:1). XM-1 provides a gateway to high-resolution imaging at high energy. To measure frequency response of the XM-1, a partially annealed gold ''island'' pattern was chosen as a test object. After comparison with the SEM image of the pattern, the microscope has the measured cutoff of 19 nm, close to the theoretical one of 17 nm. The normalized frequency response, which is the ratio of the power density of the soft x-ray image to that of the SEM image, is shown in this paper.

  12. Visualizing chemical states and defects induced magnetism of graphene oxide by spatially-resolved-X-ray microscopy and spectroscopy

    PubMed Central

    Wang, Y. F.; Singh, Shashi B.; Limaye, Mukta V.; Shao, Y. C.; Hsieh, S. H.; Chen, L. Y.; Hsueh, H. C.; Wang, H. T.; Chiou, J. W.; Yeh, Y. C.; Chen, C. W.; Chen, C. H.; Ray, Sekhar C.; Wang, J.; Pong, W. F.; Takagi, Y.; Ohigashi, T.; Yokoyama, T.; Kosugi, N.

    2015-01-01

    This investigation studies the various magnetic behaviors of graphene oxide (GO) and reduced graphene oxides (rGOs) and elucidates the relationship between the chemical states that involve defects therein and their magnetic behaviors in GO sheets. Magnetic hysteresis loop reveals that the GO is ferromagnetic whereas photo-thermal moderately reduced graphene oxide (M-rGO) and heavily reduced graphene oxide (H-rGO) gradually become paramagnetic behavior at room temperature. Scanning transmission X-ray microscopy and corresponding X-ray absorption near-edge structure spectroscopy were utilized to investigate thoroughly the variation of the C 2p(π*) states that are bound with oxygen-containing and hydroxyl groups, as well as the C 2p(σ*)-derived states in flat and wrinkle regions to clarify the relationship between the spatially-resolved chemical states and the magnetism of GO, M-rGO and H-rGO. The results of X-ray magnetic circular dichroism further support the finding that C 2p(σ*)-derived states are the main origin of the magnetism of GO. Based on experimental results and first-principles calculations, the variation in magnetic behavior from GO to M-rGO and to H-rGO is interpreted, and the origin of ferromagnetism is identified as the C 2p(σ*)-derived states that involve defects/vacancies rather than the C 2p(π*) states that are bound with oxygen-containing and hydroxyl groups on GO sheets. PMID:26481557

  13. New insights into globoids of protein storage vacuoles in wheat aleurone using synchrotron soft X-ray microscopy

    PubMed Central

    Regvar, Marjana; Eichert, Diane; Kaulich, Burkhard; Gianoncelli, Alessandra; Pongrac, Paula; Vogel-Mikuš, Katarina; Kreft, Ivan

    2011-01-01

    Mature developed seeds are physiologically and biochemically committed to store nutrients, principally as starch, protein, oils, and minerals. The composition and distribution of elements inside the aleurone cell layer reflect their biogenesis, structural characteristics, and physiological functions. It is therefore of primary importance to understand the mechanisms underlying metal ion accumulation, distribution, storage, and bioavailability in aleurone subcellular organelles for seed fortification purposes. Synchrotron radiation soft X-ray full-field imaging mode (FFIM) and low-energy X-ray fluorescence (LEXRF) spectromicroscopy were applied to characterize major structural features and the subcellular distribution of physiologically important elements (Zn, Fe, Na, Mg, Al, Si, and P). These direct imaging methods reveal the accumulation patterns between the apoplast and symplast, and highlight the importance of globoids with phytic acid mineral salts and walls as preferential storage structures. C, N, and O chemical topographies are directly linked to the structural backbone of plant substructures. Zn, Fe, Na, Mg, Al, and P were linked to globoid structures within protein storage vacuoles with variable levels of co-localization. Si distribution was atypical, being contained in the aleurone apoplast and symplast, supporting a physiological role for Si in addition to its structural function. These results reveal that the immobilization of metals within the observed endomembrane structures presents a structural and functional barrier and affects bioavailability. The combination of high spatial and chemical X-ray microscopy techniques highlights how in situ analysis can yield new insights into the complexity of the wheat aleurone layer, whose precise biochemical composition, morphology, and structural characteristics are still not unequivocally resolved. PMID:21447756

  14. 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.

  15. Chemical Heterogeneity of Organic Soil Colloids Investigated by Scanning Transmission X-ray Microscopy and C-1s NEXAFS Microspectroscopy

    SciTech Connect

    Schumacher,M.; Christl, I.; Scheinost, A.; Jacobsen, C.; Kretzschmar, R.

    2005-01-01

    Colloid release and deposition in soils and sorption of inorganic and organic pollutants to soil colloids are strongly influenced by the composition and chemical heterogeneity of colloidal soil particles. To investigate the chemical heterogeneity of organic soil colloids at the particle scale, we used synchrotron scanning transmission X-ray microscopy (STXM) and C-1s near-edge X-ray absorption fine structure (NEXAFS) spectroscopy on 49 individual particles isolated from the surface horizons of three forest soils. Stacks of 130 images of each particle were collected at different X-ray energies between 280 and 310 eV. From these image arrays, NEXAFS spectra were obtained for each pixel and analyzed by principle component analysis and cluster analysis (PCA-CA) to characterize the intraparticle heterogeneity of the organic components. The results demonstrate that the organic matter associated with water-dispersible soil colloids is chemically heterogeneous at the single-particle scale. PCA-CA identified at least two distinct regions within single particles. However, the spectral variations between these regions were much smaller than the variations of averaged NEXAFS spectra representing different particles from the same soil horizon, implying that interparticle heterogeneity is much larger than intraparticle heterogeneity. Especially the contents of aromatic and carboxyl carbon exhibited a large variability. Overall, the NEXAFS spectra of water-dispersible soil colloids were similar to the NEXAFS spectrum of the humic acid fraction, but differed clearly from the fulvic acid and dissolved organic matter fractions extracted from the same soil horizon using conventional techniques.

  16. New insights into globoids of protein storage vacuoles in wheat aleurone using synchrotron soft X-ray microscopy.

    PubMed

    Regvar, Marjana; Eichert, Diane; Kaulich, Burkhard; Gianoncelli, Alessandra; Pongrac, Paula; Vogel-Mikus, Katarina; Kreft, Ivan

    2011-07-01

    Mature developed seeds are physiologically and biochemically committed to store nutrients, principally as starch, protein, oils, and minerals. The composition and distribution of elements inside the aleurone cell layer reflect their biogenesis, structural characteristics, and physiological functions. It is therefore of primary importance to understand the mechanisms underlying metal ion accumulation, distribution, storage, and bioavailability in aleurone subcellular organelles for seed fortification purposes. Synchrotron radiation soft X-ray full-field imaging mode (FFIM) and low-energy X-ray fluorescence (LEXRF) spectromicroscopy were applied to characterize major structural features and the subcellular distribution of physiologically important elements (Zn, Fe, Na, Mg, Al, Si, and P). These direct imaging methods reveal the accumulation patterns between the apoplast and symplast, and highlight the importance of globoids with phytic acid mineral salts and walls as preferential storage structures. C, N, and O chemical topographies are directly linked to the structural backbone of plant substructures. Zn, Fe, Na, Mg, Al, and P were linked to globoid structures within protein storage vacuoles with variable levels of co-localization. Si distribution was atypical, being contained in the aleurone apoplast and symplast, supporting a physiological role for Si in addition to its structural function. These results reveal that the immobilization of metals within the observed endomembrane structures presents a structural and functional barrier and affects bioavailability. The combination of high spatial and chemical X-ray microscopy techniques highlights how in situ analysis can yield new insights into the complexity of the wheat aleurone layer, whose precise biochemical composition, morphology, and structural characteristics are still not unequivocally resolved.

  17. Visualizing chemical states and defects induced magnetism of graphene oxide by spatially-resolved-X-ray microscopy and spectroscopy.

    PubMed

    Wang, Y F; Singh, Shashi B; Limaye, Mukta V; Shao, Y C; Hsieh, S H; Chen, L Y; Hsueh, H C; Wang, H T; Chiou, J W; Yeh, Y C; Chen, C W; Chen, C H; Ray, Sekhar C; Wang, J; Pong, W F; Takagi, Y; Ohigashi, T; Yokoyama, T; Kosugi, N

    2015-10-20

    This investigation studies the various magnetic behaviors of graphene oxide (GO) and reduced graphene oxides (rGOs) and elucidates the relationship between the chemical states that involve defects therein and their magnetic behaviors in GO sheets. Magnetic hysteresis loop reveals that the GO is ferromagnetic whereas photo-thermal moderately reduced graphene oxide (M-rGO) and heavily reduced graphene oxide (H-rGO) gradually become paramagnetic behavior at room temperature. Scanning transmission X-ray microscopy and corresponding X-ray absorption near-edge structure spectroscopy were utilized to investigate thoroughly the variation of the C 2p(π*) states that are bound with oxygen-containing and hydroxyl groups, as well as the C 2p(σ*)-derived states in flat and wrinkle regions to clarify the relationship between the spatially-resolved chemical states and the magnetism of GO, M-rGO and H-rGO. The results of X-ray magnetic circular dichroism further support the finding that C 2p(σ*)-derived states are the main origin of the magnetism of GO. Based on experimental results and first-principles calculations, the variation in magnetic behavior from GO to M-rGO and to H-rGO is interpreted, and the origin of ferromagnetism is identified as the C 2p(σ*)-derived states that involve defects/vacancies rather than the C 2p(π*) states that are bound with oxygen-containing and hydroxyl groups on GO sheets.

  18. Trace metals and their relation to bacterial infections studied by X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Maser, J.; Wagner, D.; Lai, B.; Cai, Z.; Legnini, D.; Moric, I.; Bermudez, L.

    2003-03-01

    Bacterial pathogens survive in different environments in the human host by responding with expression of virulence factors that enable them to adapt to changing conditions. Trace elements regulate the expression of many virulence genes in bacteria and are thus important for their survival in the host. Mycobacteria are intracellular pathogens that can cause diseases such as tuberculosis or secondary infections in immunocompromised patients. We have used a hard x-ray microprobe to study the trace element distribution in the mycobacterial phagosome after infection of macrophages. We have studied phagosomes with virulent (M. avium) and nonvirulent (M. smegmatis) mycobacteria. In this article, we will show that the iron concentration in phagosomes with macrophages infected with nonvirulent M. smegmatis is reduced 24 hours after infection but increased in phagosomes in cells infected with virulent M. avium. In addition, we will show the effect activation of macrophages with tumor necrosis factor (TNF-α) or interferon (IFN-γ) has on the iron concentration in M. avium.

  19. 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.

  20. Low-energy X-ray fluorescence microscopy opening new opportunities for bio-related research

    PubMed Central

    Kaulich, Burkhard; Gianoncelli, Alessandra; Beran, Alfred; Eichert, Diane; Kreft, Ivan; Pongrac, Paula; Regvar, Marjana; Vogel-Mikuš, Katarina; Kiskinova, Maya

    2009-01-01

    Biological systems are unique matter with very complex morphology and highly heterogeneous chemical composition dominated by light elements. Discriminating qualitatively at the sub-micrometer level the lateral distribution of constituent elements, and correlating it to the sub-cellular biological structure, continues to be a challenge. The low-energy X-ray fluorescence microspectroscopy, recently implemented in TwinMic scanning transmission mode, has opened up new opportunities for mapping the distribution of the light elements, complemented by morphology information provided by simultaneous acquisition of absorption and phase contrast images. The important new information that can be obtained in bio-related research domains is demonstrated by two pilot experiments with specimens of interest for marine biology and food science. They demonstrate the potential to yield important insights into the structural and compositional enrichment, distribution and correlation of essential trace elements in the lorica of Tintinnopsis radix, and the lateral distribution of trace nutrients in the seeds of wheat Triticum aestivum. PMID:19570794

  1. X-ray tomographic microscopy for non-destructive inspection and advanced materials characterization. Final report, May 22, 1992--May 21, 1994

    SciTech Connect

    1995-04-27

    This was a CRADA to transfer the x-ray tomographic microscope technology to the Quality Technology Center of General Electric Air Craft Engines Division in Ohio. The x-ray tomographic microscope (XTM) is a high resolution, three-dimensional imaging system that can be used to image materials microstructures noninvasively. The apparatus consists of an x-ray source, x-ray collimators, sample positioning stages, a fluorescent screen to convert x-rays to visible light, an optical lens, and a thermoelectrically cooled charge coupled device detector. The details of the microscope`s design have been described elsewhere. In practice, the sample to be imaged is positioned on a rotating stage. The sample is initially translated out of the x-ray path, and an image is obtained of the incident x-ray beam (the reference image). Next, the sample is placed between the x-ray path and the scintillator, and another image, the projection image, is acquired. The ratios of the logarithms of the reference image and the projection image provide values of the integrated x-ray attenuation through the sample. By rotating the sample in discrete angular increments through 180 degrees, enough data can be obtained to reconstruct the two-dimensional projection images into a three-dimensional image of the mineral density distribution in the sample. This reconstruction procedure, known as reconstruction from projections, is usually performed with the technique of Fourier-filtered back-projection. Using the present microscope, a 1 cubic centimeter volume can be imaged with five micrometer volume elements in about one hour or less.

  2. Ordering in bio-inorganic hybrid nanomaterials probed by in situ scanning transmission X-ray microscopy.

    PubMed

    Lee, Jonathan R I; Bagge-Hansen, Michael; Tunuguntla, Ramya; Kim, Kyunghoon; Bangar, Mangesh; Willey, Trevor M; Tran, Ich C; Kilcoyne, David A; Noy, Aleksandr; van Buuren, Tony

    2015-06-01

    Phospholipid bilayer coated Si nanowires are one-dimensional (1D) composites that provide versatile bio-nanoelectronic functionality via incorporation of a wide variety of biomolecules into the phospholipid matrix. The physiochemical behaviour of the phospholipid bilayer is strongly dependent on its structure and, as a consequence, substantial modelling and experimental efforts have been directed at the structural characterization of supported bilayers and unsupported phospholipid vesicles; nonetheless, the experimental studies conducted to date have exclusively involved volume-averaged techniques, which do not allow for the assignment of spatially resolved structural variations that could critically impact the performance of the 1D phospholipid-Si NW composites. In this manuscript, we use scanning transmission X-ray microscopy (STXM) to probe bond orientation and bilayer thickness as a function of position with a spatial resolution of ∼30 nm for Δ9-cis 1,2-dioleoyl-sn-glycero-3-phosphocholine layers prepared Si NWs. When coupled with small angle X-ray scattering measurements, the STXM data reveal structural motifs of the Si NWs that give rise to multi-bilayer formation and enable assignment of the orientation of specific bonds known to affect the order and rigidity of phospholipid bilayers.

  3. Microwave soft x-ray microscopy for nanoscale magnetization dynamics in the 5-10 GHz frequency range.

    PubMed

    Bonetti, Stefano; Kukreja, Roopali; Chen, Zhao; Spoddig, Detlef; Ollefs, Katharina; Schöppner, Christian; Meckenstock, Ralf; Ney, Andreas; Pinto, Jude; Houanche, Richard; Frisch, Josef; Stöhr, Joachim; Dürr, Hermann A; Ohldag, Hendrik

    2015-09-01

    We present a scanning transmission x-ray microscopy setup combined with a novel microwave synchronization scheme for studying high frequency magnetization dynamics at synchrotron light sources. The sensitivity necessary to detect small changes in the magnetization on short time scales and nanometer spatial dimensions is achieved by combining the excitation mechanism with single photon counting electronics that is locked to the synchrotron operation frequency. Our instrument is capable of creating direct images of dynamical phenomena in the 5-10 GHz range, with high spatial resolution. When used together with circularly polarized x-rays, the above capabilities can be combined to study magnetic phenomena at microwave frequencies, such as ferromagnetic resonance (FMR) and spin waves. We demonstrate the capabilities of our technique by presenting phase resolved images of a ∼6 GHz nanoscale spin wave generated by a spin torque oscillator, as well as the uniform ferromagnetic precession with ∼0.1° amplitude at ∼9 GHz in a micrometer-sized cobalt strip. PMID:26429444

  4. X-ray fluorescent microscopy reveals large-scale relocalization and extracellular translocation of cellular copper during angiogenesis.

    SciTech Connect

    Finney, L.; Mandava, S.; Ursos, L.; Zhang, W.; Rodi, D.; Vogt, S.; Legnini, D.; Maser, J.; Ikpatt, F.; Olopade, O. I.; Glesne, D.; Univ. of Chicago

    2007-02-13

    Although copper has been reported to influence numerous proteins known to be important for angiogenesis, the enhanced sensitivity of this developmental process to copper bioavailability has remained an enigma, because copper metalloproteins are prevalent and essential throughout all cells. Recent developments in x-ray optics at third-generation synchrotron sources have provided a resource for highly sensitive visualization and quantitation of metalloproteins in biological samples. Here, we report the application of x-ray fluorescence microscopy (XFM) to in vitro models of angiogenesis and neurogenesis, revealing a surprisingly dramatic spatial relocalization specific to capillary formation of 80-90% of endogenous cellular copper stores from intracellular compartments to the tips of nascent endothelial cell filopodia and across the cell membrane. Although copper chelation had no effect on process formation, an almost complete ablation of network formation was observed. XFM of highly vascularized ductal carcinomas showed copper clustering in putative neoangiogenic areas. This use of XFM for the study of a dynamic developmental process not only sheds light on the copper requirement for endothelial tube formation but highlights the value of synchrotron-based facilities in biological research.

  5. Mesoscopic structural phase progression in photo-excited VO2 revealed by time-resolved x-ray diffraction microscopy

    DOE PAGES

    Zhu, Yi; Cai, Zhonghou; Chen, Pice; Zhang, Qingteng; Highland, Matthew J.; Jung, II Woong; Walko, Donald A.; Dufresne, Eric M.; Jaewoo, Jeong; Samant, Mahesh G.; et al

    2016-02-26

    Dynamical phase separation during a solid-solid phase transition poses a challenge for understanding the fundamental processes in correlated materials. Critical information underlying a phase transition, such as localized phase competition, is difficult to reveal by measurements that are spatially averaged over many phase seperated regions. The ability to simultanousely track the spatial and temporal evolution of such systems is essential to understanding mesoscopic processes during a phase transition. Using state-of- the-art time-resolved hard x-ray diffraction microscopy, we directly visualize the structural phase progression in a VO2 film upon photoexcitation. Following a homogenous in-plane optical excitation, the phase transformation is initiatedmore » at discrete sites and completed by the growth of one lattice structure into the other, instead of a simultaneous isotropic lattice symmetry change. The time-dependent x-ray diffraction spatial maps show that the in-plane phase progression in laser-superheated VO2 is via a displacive lattice transformation as a result of relaxation from an excited monoclinic phase into a rutile phase. The speed of the phase front progression is quantitatively measured, which is faster than the process driven by in-plane thermal diffusion but slower than the sound speed in VO2. Lastly, the direct visualization of localized structural changes in the time domain opens a new avenue to study mesoscopic processes in driven systems.« less

  6. In-situ transmission x-ray microscopy study of photon-induced oxidation of silver nanowires

    NASA Astrophysics Data System (ADS)

    Yu, Le; Sun, Yugang; Wang, Yuxin; Cai, Zhonghou; Han, Ping; Cheng, X. M.

    Oxidation of metal nanoparticles usually follows a Kirkendall process to transform solid nanoparticles to hollow metal oxide nanoshells. However the morphological trajectory of nanoparticles and the mass diffusion kinetics involved in the nanoscale Kirkendall process are complex. In this presentation we report the use of in-situ transmission x-ray microscopy (TXM) to directly image individual silver nanowires under oxidation atmosphere, which are created from radiolysis of air under illumination of the focused synchrotron x-ray beam. The in-situ results clearly show the morphological transformation from solid silver nanowires to hollow nanotubes in the course of oxidation reaction of silver. Quantitative analysis of the time-resolved TXM images provides unprecedented details on reaction kinetics and mass diffusion kinetics associated with the oxidation process. Work at Bryn Mawr College is supported by NSF Grant #1207085. Use of the Advanced Photon Source and the Center for Nanoscale Materials at Argonne National Laboratory was supported by the U. S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

  7. Sorption and distribution of copper in unsaturated Pseudomonas putida CZ1 biofilms as determined by X-ray fluorescence microscopy.

    PubMed

    Chen, Guangcun; Chen, Xincai; Yang, Yuanqiang; Hay, Anthony G; Yu, Xiaohan; Chen, Yingxu

    2011-07-01

    The spatial and temporal distribution of metals in unsaturated Pseudomonas putida CZ1 biofilms was determined using synchrotron-based X-ray fluorescence microscopy (XRF). It was found that Fe, Mn, and Ca were mainly distributed near the air-biofilm interface of a biofilm grown on 40 mM citrate, while there were two Fe-, Mn-, and Ca-rich layers within a biofilm grown on 10 mM citrate. The sorption of copper by biofilm grown in medium containing 10 mM citrate was rapid, with copper being found throughout the biofilm after only 1 h of exposure. Copper initially colocalized with Fe and Mn element layers in the biofilm and then precipitated in a 40-μm-thick layer near the air-biofilm interface when exposed for 12 h. Cu K-edge X-ray absorption near edge structure (XANES) analysis revealed that Cu was primarily bound with citrate within the biofilm, and the precipitate formed in the biofilm exposed to copper for 12 h was most similar to copper phosphate. LIVE/DEAD staining revealed that cells at the biofilm-membrane interface were mostly alive even when the copper concentration reached 80.5 mg copper g(-1) biomass. This suggests that the biofilm matrix provided significant protection for cells in this area. These results significantly improve our understanding of metal acquisition, transportation, and immobilization in unsaturated biofilm systems. PMID:21642411

  8. Ordering in bio-inorganic hybrid nanomaterials probed by in situ scanning transmission X-ray microscopy

    DOE PAGES

    Lee, Jonathan R. I.; Bagge-Hansen, Michael; Tunuguntla, Ramya; Kim, Kyunghoon; Bangar, Mangesh; Willey, Trevor M.; Tran, Ich C.; Kilcoyne, David A.; Noy, Aleksandr; van Buuren, Tony

    2015-04-15

    Here, phospholipid bilayer coated Si nanowires are one-dimensional (1D) composites that provide versatile bio-nanoelectronic functionality via incorporation of a wide variety of biomolecules into the phospholipid matrix. The physiochemical behaviour of the phospholipid bilayer is strongly dependent on its structure and, as a consequence, substantial modelling and experimental efforts have been directed at the structural characterization of supported bilayers and unsupported phospholipid vesicles; nonetheless, the experimental studies conducted to date have exclusively involved volume-averaged techniques, which do not allow for the assignment of spatially resolved structural variations that could critically impact the performance of the 1D phospholipid-Si NW composites. Inmore » this manuscript, we use scanning transmission X-ray microscopy (STXM) to probe bond orientation and bilayer thickness as a function of position with a spatial resolution of ~30 nm for Δ9-cis 1,2-dioleoyl-sn-glycero-3-phosphocholine layers prepared Si NWs. When coupled with small angle X-ray scattering measurements, the STXM data reveal structural motifs of the Si NWs that give rise to multi-bilayer formation and enable assignment of the orientation of specific bonds known to affect the order and rigidity of phospholipid bilayers.« less

  9. Mesoscopic structural phase progression in photo-excited VO2 revealed by time-resolved x-ray diffraction microscopy

    NASA Astrophysics Data System (ADS)

    Zhu, Yi; Cai, Zhonghou; Chen, Pice; Zhang, Qingteng; Highland, Matthew J.; Jung, Il Woong; Walko, Donald A.; Dufresne, Eric M.; Jeong, Jaewoo; Samant, Mahesh G.; Parkin, Stuart S. P.; Freeland, John W.; Evans, Paul G.; Wen, Haidan

    2016-02-01

    Dynamical phase separation during a solid-solid phase transition poses a challenge for understanding the fundamental processes in correlated materials. Critical information underlying a phase transition, such as localized phase competition, is difficult to reveal by measurements that are spatially averaged over many phase separated regions. The ability to simultaneously track the spatial and temporal evolution of such systems is essential to understanding mesoscopic processes during a phase transition. Using state-of-the-art time-resolved hard x-ray diffraction microscopy, we directly visualize the structural phase progression in a VO2 film upon photoexcitation. Following a homogenous in-plane optical excitation, the phase transformation is initiated at discrete sites and completed by the growth of one lattice structure into the other, instead of a simultaneous isotropic lattice symmetry change. The time-dependent x-ray diffraction spatial maps show that the in-plane phase progression in laser-superheated VO2 is via a displacive lattice transformation as a result of relaxation from an excited monoclinic phase into a rutile phase. The speed of the phase front progression is quantitatively measured, and is faster than the process driven by in-plane thermal diffusion but slower than the sound speed in VO2. The direct visualization of localized structural changes in the time domain opens a new avenue to study mesoscopic processes in driven systems.

  10. Mesoscopic structural phase progression in photo-excited VO2 revealed by time-resolved x-ray diffraction microscopy

    PubMed Central

    Zhu, Yi; Cai, Zhonghou; Chen, Pice; Zhang, Qingteng; Highland, Matthew J.; Jung, Il Woong; Walko, Donald A.; Dufresne, Eric M.; Jeong, Jaewoo; Samant, Mahesh G.; Parkin, Stuart S. P.; Freeland, John W.; Evans, Paul G.; Wen, Haidan

    2016-01-01

    Dynamical phase separation during a solid-solid phase transition poses a challenge for understanding the fundamental processes in correlated materials. Critical information underlying a phase transition, such as localized phase competition, is difficult to reveal by measurements that are spatially averaged over many phase separated regions. The ability to simultaneously track the spatial and temporal evolution of such systems is essential to understanding mesoscopic processes during a phase transition. Using state-of-the-art time-resolved hard x-ray diffraction microscopy, we directly visualize the structural phase progression in a VO2 film upon photoexcitation. Following a homogenous in-plane optical excitation, the phase transformation is initiated at discrete sites and completed by the growth of one lattice structure into the other, instead of a simultaneous isotropic lattice symmetry change. The time-dependent x-ray diffraction spatial maps show that the in-plane phase progression in laser-superheated VO2 is via a displacive lattice transformation as a result of relaxation from an excited monoclinic phase into a rutile phase. The speed of the phase front progression is quantitatively measured, and is faster than the process driven by in-plane thermal diffusion but slower than the sound speed in VO2. The direct visualization of localized structural changes in the time domain opens a new avenue to study mesoscopic processes in driven systems. PMID:26915398

  11. Effect of processing on the microstructure of finger millet by X-ray diffraction and scanning electron microscopy.

    PubMed

    Dharmaraj, Usha; Parameswara, P; Somashekar, R; Malleshi, Nagappa G

    2014-03-01

    Finger millet is one of the important minor cereals, and carbohydrates form its major chemical constituent. Recently, the millet is processed to prepare hydrothermally treated (HM), decorticated (DM), expanded (EM) and popped (PM) products. The present research aims to study the changes in the microstructure of carbohydrates using X-ray diffraction and scanning electron microscopy. Processing the millet brought in significant changes in the carbohydrates. The native millet exhibited A-type pattern of X-ray diffraction with major peaks at 2θ values of 15.3, 17.86 and 23.15°, whereas, all other products showed V-type pattern with single major peak at 2θ values ranging from 19.39 to 19.81°. The corresponding lattice spacing and the number of unit cells in a particular direction of reflection also reduced revealing that crystallinity of starch has been decreased depending upon the processing conditions. Scanning electron microscopic studies also revealed that the orderly pattern of starch granules changed into a coherent mass due to hydrothermal treatment, while high temperature short time treatment rendered a honey-comb like structure to the product. However, the total carbohydrates and non-starch polysaccharide contents almost remained the same in all the products except for DM and EM, but the individual carbohydrate components changed significantly depending on the type of processing.

  12. Microwave soft x-ray microscopy for nanoscale magnetization dynamics in the 5–10 GHz frequency range

    DOE PAGES

    Bonetti, Stefano; Kukreja, Roopali; Chen, Zhao; Spoddig, Detlef; Ollefs, Katharina; Schöppner, Christian; Meckenstock, Ralf; Ney, Andreas; Pinto, Jude; Houanche, Richard; et al

    2015-09-10

    In this study, we present a scanning transmission x-ray microscopy setup combined with a novel microwave synchronization scheme in order to study high frequency magnetization dynamics at synchrotron light sources. The sensitivity necessary to detect small changes of the magnetization on short time scales and nanometer spatial dimensions is achieved by combination of the developed excitation mechanism with a single photon counting electronics that is locked to the synchrotron operation frequency. The required mechanical stability is achieved by a compact design of the microscope. Our instrument is capable of creating direct images of dynamical phenomena in the 5-10 GHz range,more » with 35 nm resolution. When used together with circularly polarized x-rays, the above capabilities can be combined to study magnetic phenomena at microwave frequencies, such as ferromagnetic resonance (FMR) and spin waves. We demonstrate the capabilities of our technique by presenting phase resolved images of a –6 GHz nanoscale spin wave generated by a spin torque oscillator, as well as the uniform ferromagnetic precession with ~0.1° amplitude at –9 GHz in a micrometer-sized cobalt strip.« less

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

    PubMed

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

    2015-04-01

    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. PMID:25849399

  14. Microwave soft x-ray microscopy for nanoscale magnetization dynamics in the 5-10 GHz frequency range

    NASA Astrophysics Data System (ADS)

    Bonetti, Stefano; Kukreja, Roopali; Chen, Zhao; Spoddig, Detlef; Ollefs, Katharina; Schöppner, Christian; Meckenstock, Ralf; Ney, Andreas; Pinto, Jude; Houanche, Richard; Frisch, Josef; Stöhr, Joachim; Dürr, Hermann A.; Ohldag, Hendrik

    2015-09-01

    We present a scanning transmission x-ray microscopy setup combined with a novel microwave synchronization scheme for studying high frequency magnetization dynamics at synchrotron light sources. The sensitivity necessary to detect small changes in the magnetization on short time scales and nanometer spatial dimensions is achieved by combining the excitation mechanism with single photon counting electronics that is locked to the synchrotron operation frequency. Our instrument is capable of creating direct images of dynamical phenomena in the 5-10 GHz range, with high spatial resolution. When used together with circularly polarized x-rays, the above capabilities can be combined to study magnetic phenomena at microwave frequencies, such as ferromagnetic resonance (FMR) and spin waves. We demonstrate the capabilities of our technique by presenting phase resolved images of a ˜6 GHz nanoscale spin wave generated by a spin torque oscillator, as well as the uniform ferromagnetic precession with ˜0.1° amplitude at ˜9 GHz in a micrometer-sized cobalt strip.

  15. Fast two-dimensional grid and transmission X-ray microscopy scanning methods for visualizing and characterizing protein crystals

    PubMed Central

    Wojdyla, Justyna Aleksandra; Panepucci, Ezequiel; Martiel, Isabelle; Ebner, Simon; Huang, Chia-Ying; Caffrey, Martin; Bunk, Oliver; Wang, Meitian

    2016-01-01

    A fast continuous grid scan protocol has been incorporated into the Swiss Light Source (SLS) data acquisition and analysis software suite on the macromolecular crystallography (MX) beamlines. Its combination with fast readout single-photon counting hybrid pixel array detectors (PILATUS and EIGER) allows for diffraction-based identification of crystal diffraction hotspots and the location and centering of membrane protein microcrystals in the lipid cubic phase (LCP) in in meso in situ serial crystallography plates and silicon nitride supports. Diffraction-based continuous grid scans with both still and oscillation images are supported. Examples that include a grid scan of a large (50 nl) LCP bolus and analysis of the resulting diffraction images are presented. Scanning transmission X-ray microscopy (STXM) complements and benefits from fast grid scanning. STXM has been demonstrated at the SLS beamline X06SA for near-zero-dose detection of protein crystals mounted on different types of sample supports at room and cryogenic temperatures. Flash-cooled crystals in nylon loops were successfully identified in differential and integrated phase images. Crystals of just 10 µm thickness were visible in integrated phase images using data collected with the EIGER detector. STXM offers a truly low-dose method for locating crystals on solid supports prior to diffraction data collection at both synchrotron microfocusing and free-electron laser X-ray facilities. PMID:27275141

  16. Microwave soft x-ray microscopy for nanoscale magnetization dynamics in the 5–10 GHz frequency range

    SciTech Connect

    Bonetti, Stefano; Kukreja, Roopali; Chen, Zhao; Spoddig, Detlef; Ollefs, Katharina; Schöppner, Christian; Meckenstock, Ralf; Ney, Andreas; Pinto, Jude; Houanche, Richard; Frisch, Josef; Stöhr, Joachim; Dürr, Hermann A.; Ohldag, Hendrik

    2015-09-10

    In this study, we present a scanning transmission x-ray microscopy setup combined with a novel microwave synchronization scheme in order to study high frequency magnetization dynamics at synchrotron light sources. The sensitivity necessary to detect small changes of the magnetization on short time scales and nanometer spatial dimensions is achieved by combination of the developed excitation mechanism with a single photon counting electronics that is locked to the synchrotron operation frequency. The required mechanical stability is achieved by a compact design of the microscope. Our instrument is capable of creating direct images of dynamical phenomena in the 5-10 GHz range, with 35 nm resolution. When used together with circularly polarized x-rays, the above capabilities can be combined to study magnetic phenomena at microwave frequencies, such as ferromagnetic resonance (FMR) and spin waves. We demonstrate the capabilities of our technique by presenting phase resolved images of a –6 GHz nanoscale spin wave generated by a spin torque oscillator, as well as the uniform ferromagnetic precession with ~0.1° amplitude at –9 GHz in a micrometer-sized cobalt strip.

  17. Microwave soft x-ray microscopy for nanoscale magnetization dynamics in the 5–10 GHz frequency range

    SciTech Connect

    Bonetti, Stefano Chen, Zhao; Kukreja, Roopali; Spoddig, Detlef; Schöppner, Christian; Meckenstock, Ralf; Ollefs, Katharina; Ney, Andreas; Pinto, Jude; Houanche, Richard; Frisch, Josef; Stöhr, Joachim; Dürr, Hermann A.; Ohldag, Hendrik

    2015-09-15

    We present a scanning transmission x-ray microscopy setup combined with a novel microwave synchronization scheme for studying high frequency magnetization dynamics at synchrotron light sources. The sensitivity necessary to detect small changes in the magnetization on short time scales and nanometer spatial dimensions is achieved by combining the excitation mechanism with single photon counting electronics that is locked to the synchrotron operation frequency. Our instrument is capable of creating direct images of dynamical phenomena in the 5-10 GHz range, with high spatial resolution. When used together with circularly polarized x-rays, the above capabilities can be combined to study magnetic phenomena at microwave frequencies, such as ferromagnetic resonance (FMR) and spin waves. We demonstrate the capabilities of our technique by presenting phase resolved images of a ∼6 GHz nanoscale spin wave generated by a spin torque oscillator, as well as the uniform ferromagnetic precession with ∼0.1° amplitude at ∼9 GHz in a micrometer-sized cobalt strip.

  18. 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.

  19. 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

  20. Status of the Short-Pulse X-ray Project at the Advanced Photon Source

    SciTech Connect

    Nassiri, A; Berenc, T G; Borland, M; Brajuskovic, B; Bromberek, D J; Carwardine, J; Decker, G; Emery, L; Fuerst, J D; Grelick, A E; Horan, D; Kaluzny, J; Lenkszus, F; Lill, R M; Liu, J; Ma, H; Sajaev, V; Smith, T L; Stillwell, B K; Waldschmidt, G J; Wu, G; Yang, B X; Yang, Y; Zholents, A; Byrd, J M; Doolittle, L R; Huang, G; Cheng, G; Ciovati, G; Dhakal, P; Eremeev, G V; Feingold, J J; Geng, R L; Henry, J; Kneisel, P; Macha, K; Mammosser, J D; Matalevich, J; Palczewski, A D; Rimmer, R A; Wang, H; Wilson, K M; Wiseman, M; Li, Z; Xiao, L

    2012-07-01

    The Advanced Photon Source Upgrade (APS-U) Project at Argonne will include generation of short-pulse x-rays based on Zholents deflecting cavity scheme. We have chosen superconducting (SC) cavities in order to have a continuous train of crabbed bunches and flexibility of operating modes. In collaboration with Jefferson Laboratory, we are prototyping and testing a number of single-cell deflecting cavities and associated auxiliary systems with promising initial results. In collaboration with Lawrence Berkeley National Laboratory, we are working to develop state-of-the-art timing, synchronization, and differential rf phase stability systems that are required for SPX. Collaboration with Advanced Computations Department at Stanford Linear Accelerator Center is looking into simulations of complex, multi-cavity geometries with lower- and higher-order modes waveguide dampers using ACE3P. This contribution provides the current R&D status of the SPX project.

  1. Exploiting the Photoelectric effect for X-ray Polarimetry using Time Projection Chamber

    NASA Technical Reports Server (NTRS)

    Jahoda, Keith; Black, Kevin; Deines-Jones, Philip; Hill, Joanne; Swank, Jean

    2008-01-01

    The promise of photoelectric X-ray polarimetry has now been realized in laboratory demonstrations and may soon be used for astrophysical observations. Photoelectric polarimetry in gas filled proportional counters achieves high sensitivity through a combination of broad band width and good modulation. The band can be tuned by careful choice of gas composition and pressure. The measurements rely on imaging the tracks of photoelectrons. The initial direction of each track carries information about the electric field of the X-ray photon, and an ensemble of such measurements thus measures the net polarization of the source. A novel readout geometry using time projection chambers (TPC) allows deep (i.e. high efficiency) detectors, albeit without the ability to image the sky. Polarimeters which exploit the TPC geometry can be optimized for use behind telescopes, to study faint persistent sources, or as wide field of view instruments, designed to study bright transient events such as gamma-ray bursts or solar flares. We present the conceptual design of both types of TPC polarimeter. Recent laboratory results demonstrate that these polarimeters can achieve substantial gains in the polarization sensitivity achievable in experiments of modest size.

  2. Aluminum-phosphate binder formation in zeolites as probed with X-ray absorption microscopy.

    PubMed

    van der Bij, Hendrik E; Cicmil, Dimitrije; Wang, Jian; Meirer, Florian; de Groot, Frank M F; Weckhuysen, Bert M

    2014-12-24

    In this work, three industrially relevant zeolites with framework topologies of MOR, FAU and FER have been explored on their ability to form an AlPO4 phase by reaction of a phosphate precursor with expelled framework aluminum. A detailed study was performed on zeolite H-mordenite, using in situ STXM and soft X-ray absorption tomography, complemented with (27)Al and (31)P magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy, XRD, FT-IR spectroscopy, and N2 physisorption. Extraframework aluminum was extracted from steam-dealuminated H-mordenite and shown to dominantly consist of amorphous AlO(OH). It was found that phosphoric acid readily reacts with the AlO(OH) phase in dealuminated H-mordenite and forms an extraframework amorphous AlPO4 phase. It was found that while AlPO4 crystallizes outside of the zeolitic channel system forming AlPO4 islands, AlPO4 that remains inside tends to stay more amorphous. In the case of ultrastable zeolite Y the FAU framework collapsed during phosphatation, due to extraction of framework aluminum from the lattice. However, using milder phosphatation conditions an extraframework AlPO4 α-cristobalite/tridymite phase could also be produced within the FAU framework. Finally, in steamed zeolite ferrierite with FER topology the extraframework aluminum species were trapped and therefore not accessible for phosphoric acid; hence, no AlPO4 phase could be formed within the structure. Therefore, the parameters to be taken into account in AlPO4 synthesis are the framework Si/Al ratio, stability of framework aluminum, pore dimensionality and accessibility of extraframework aluminum species.

  3. Synchrotron-based transmission x-ray microscopy for improved extraction in shale during hydraulic fracturing

    NASA Astrophysics Data System (ADS)

    Kiss, Andrew M.; Jew, Adam D.; Joe-Wong, Claresta; Maher, Kate M.; Liu, Yijin; Brown, Gordon E.; Bargar, John

    2015-09-01

    Engineering topics which span a range of length and time scales present a unique challenge to researchers. Hydraulic fracturing (fracking) of oil shales is one of these challenges and provides an opportunity to use multiple research tools to thoroughly investigate a topic. Currently, the extraction efficiency from the shale is low but can be improved by carefully studying the processes at the micro- and nano-scale. Fracking fluid induces chemical changes in the shale which can have significant effects on the microstructure morphology, permeability, and chemical composition. These phenomena occur at different length and time scales which require different instrumentation to properly study. Using synchrotron-based techniques such as fluorescence tomography provide high sensitivity elemental mapping and an in situ micro-tomography system records morphological changes with time. In addition, the transmission X-ray microscope (TXM) at the Stanford Synchrotron Radiation Lightsource (SSRL) beamline 6-2 is utilized to collect a nano-scale three-dimensional representation of the sample morphology with elemental and chemical sensitivity. We present the study of a simplified model system, in which pyrite and quartz particles are mixed and exposed to oxidizing solution, to establish the basic understanding of the more complex geology-relevant oxidation reaction. The spatial distribution of the production of the oxidation reaction, ferrihydrite, is retrieved via full-field XANES tomography showing the reaction pathway. Further correlation between the high resolution TXM data and the high sensitivity micro-probe data provides insight into potential morphology changes which can decrease permeability and limit hydrocarbon recovery.

  4. Aluminum-phosphate binder formation in zeolites as probed with X-ray absorption microscopy.

    PubMed

    van der Bij, Hendrik E; Cicmil, Dimitrije; Wang, Jian; Meirer, Florian; de Groot, Frank M F; Weckhuysen, Bert M

    2014-12-24

    In this work, three industrially relevant zeolites with framework topologies of MOR, FAU and FER have been explored on their ability to form an AlPO4 phase by reaction of a phosphate precursor with expelled framework aluminum. A detailed study was performed on zeolite H-mordenite, using in situ STXM and soft X-ray absorption tomography, complemented with (27)Al and (31)P magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy, XRD, FT-IR spectroscopy, and N2 physisorption. Extraframework aluminum was extracted from steam-dealuminated H-mordenite and shown to dominantly consist of amorphous AlO(OH). It was found that phosphoric acid readily reacts with the AlO(OH) phase in dealuminated H-mordenite and forms an extraframework amorphous AlPO4 phase. It was found that while AlPO4 crystallizes outside of the zeolitic channel system forming AlPO4 islands, AlPO4 that remains inside tends to stay more amorphous. In the case of ultrastable zeolite Y the FAU framework collapsed during phosphatation, due to extraction of framework aluminum from the lattice. However, using milder phosphatation conditions an extraframework AlPO4 α-cristobalite/tridymite phase could also be produced within the FAU framework. Finally, in steamed zeolite ferrierite with FER topology the extraframework aluminum species were trapped and therefore not accessible for phosphoric acid; hence, no AlPO4 phase could be formed within the structure. Therefore, the parameters to be taken into account in AlPO4 synthesis are the framework Si/Al ratio, stability of framework aluminum, pore dimensionality and accessibility of extraframework aluminum species. PMID:25415849

  5. Center for X-Ray Optics, 1992

    SciTech Connect

    Not Available

    1993-08-01

    This report discusses the following topics: Center for X-Ray Optics; Soft X-Ray Imaging wit Zone Plate Lenses; Biological X-Ray microscopy; Extreme Ultraviolet Lithography for Nanoelectronic Pattern Transfer; Multilayer Reflective Optics; EUV/Soft X-ray Reflectometer; Photoemission Microscopy with Reflective Optics; Spectroscopy with Soft X-Rays; Hard X-Ray Microprobe; Coronary Angiography; and Atomic Scattering Factors.

  6. A median-Gaussian filtering framework for Moiré pattern noise removal from X-ray microscopy image.

    PubMed

    Wei, Zhouping; Wang, Jian; Nichol, Helen; Wiebe, Sheldon; Chapman, Dean

    2012-02-01

    Moiré pattern noise in Scanning Transmission X-ray Microscopy (STXM) imaging introduces significant errors in qualitative and quantitative image analysis. Due to the complex origin of the noise, it is difficult to avoid Moiré pattern noise during the image data acquisition stage. In this paper, we introduce a post-processing method for filtering Moiré pattern noise from STXM images. This method includes a semi-automatic detection of the spectral peaks in the Fourier amplitude spectrum by using a local median filter, and elimination of the spectral noise peaks using a Gaussian notch filter. The proposed median-Gaussian filtering framework shows good results for STXM images with the size of power of two, if such parameters as threshold, sizes of the median and Gaussian filters, and size of the low frequency window, have been properly selected.

  7. Repeated crack healing in MAX-phase ceramics revealed by 4D in situ synchrotron X-ray tomographic microscopy

    PubMed Central

    Sloof, Willem G.; Pei, Ruizhi; McDonald, Samuel A.; Fife, Julie L.; Shen, Lu; Boatemaa, Linda; Farle, Ann-Sophie; Yan, Kun; Zhang, Xun; van der Zwaag, Sybrand; Lee, Peter D.; Withers, Philip J.

    2016-01-01

    MAX phase materials are emerging as attractive engineering materials in applications where the material is exposed to severe thermal and mechanical conditions in an oxidative environment. The Ti2AlC MAX phase possesses attractive thermomechanical properties even beyond a temperature of 1000 K. An attractive feature of this material is its capacity for the autonomous healing of cracks when operating at high temperatures. Coupling a specialized thermomechanical setup to a synchrotron X-ray tomographic microscopy endstation at the TOMCAT beamline, we captured the temporal evolution of local crack opening and healing during multiple cracking and autonomous repair cycles at a temperature of 1500 K. For the first time, the rate and position dependence of crack repair in pristine Ti2AlC material and in previously healed cracks has been quantified. Our results demonstrate that healed cracks can have sufficient mechanical integrity to make subsequent cracks form elsewhere upon reloading after healing. PMID:26972608

  8. Mapping the subcellular localization of Fe3O4@TiO2 nanoparticles by X-ray Fluorescence Microscopy

    NASA Astrophysics Data System (ADS)

    Yuan, Y.; Chen, S.; Gleber, S. C.; Lai, B.; Brister, K.; Flachenecker, C.; Wanzer, B.; Paunesku, T.; Vogt, S.; Woloschak, G. E.

    2013-10-01

    The targeted delivery of Fe3O4@TiO2 nanoparticles to cancer cells is an important step in their development as nanomedicines. We have synthesized nanoparticles that can bind the Epidermal Growth Factor Receptor, a cell surface protein that is overexpressed in many epithelial type cancers. In order to study the subcellular distribution of these nanoparticles, we have utilized the sub-micron resolution of X-ray Fluorescence Microscopy to map the location of Fe3O4@TiO2 NPs and other trace metal elements within HeLa cervical cancer cells. Here we demonstrate how the higher resolution of the newly installed Bionanoprobe at the Advanced Photon Source at Argonne National Laboratory can greatly improve our ability to distinguish intracellular nanoparticles and their spatial relationship with subcellular compartments.

  9. Visualizing Cell Architecture and Molecular Location Using Soft X-Ray Tomography and Correlated Cryo-Light Microscopy

    PubMed Central

    McDermott, Gerry; Le Gros, Mark A.; Larabell, Carolyn A.

    2012-01-01

    Living cells are structured to create a range of microenvironments that support specific chemical reactions and processes. Understanding how cells function therefore requires detailed knowledge of both the subcellular architecture and the location of specific molecules within this framework. Here we review the development of two correlated cellular imaging techniques that fulfill this need. Cells are first imaged using cryogenic fluorescence microscopy to determine the location of molecules of interest that have been labeled with fluorescent tags. The same specimen is then imaged using soft X-ray tomography to generate a high-contrast, 3D reconstruction of the cells. Data from the two modalities are then combined to produce a composite, information-rich view of the cell. This correlated imaging approach can be applied across the spectrum of problems encountered in cell biology, from basic research to biotechnological and biomedical applications such as the optimization of biofuels and the development of new pharmaceuticals. PMID:22242730

  10. Study of air-induced paper discolorations by infrared spectroscopy, X-ray fluorescence, and scanning electron microscopy.

    PubMed

    Ferreira, Adriana; Figueira, Francisca; Pessanha, Sofia; Nielsen, Ingelise; Carvalho, Maria Luisa

    2010-02-01

    Air-induced paper discoloration is described as being different from other discoloration morphologies. It seems to be the result of prolonged exposure to air in a humid and polluted environment without appropriate protecting coverage. In this work, three folios from the same eighteenth century book, presenting three degrees of discoloration and opacity and subjected to different environmental conditions, were examined and compared. Samples were analyzed and compared by three different instrumental techniques, mid-infrared spectroscopy, X-ray fluorescence (XRF), and scanning electron microscopy (SEM). Chemical and physical changes were confirmed from the data collected by these techniques. The absence of the secondary amide band characteristic of proteins in the infrared spectra of the two discolored folios, accompanied by the appearance and increase of white mineral-like deposits visible in the SEM micrographs, support the idea that oxidation reactions occurred and that these two folios were subjected to more severe degradation hazard. PMID:20149275

  11. Imaging the heterogeneity of mineral surface reactivity using Ag(I) and synchrotron X-ray microscopy

    SciTech Connect

    Amonette, James E.; Heald, Steve M.; Russell, Colleen K.

    2003-10-01

    Microscopic-scale imaging of reduced zones on the surfaces of minerals can be achieved by reaction with dilute Ag(I) solutions and subsequent analysis using synchrotron X-ray microscopy (XRM) above the Ag K-edge (25.5 keV). The principal reductant is Fe(II), but other reductants such as sulfide may contribute. Reduced zones may exist instrinsically, as in the structure of biotite and augite, or may be generated by reaction with chemical agents such as dithionite or treatment with sulfate-reducing bacteria (SRB). We demonstrate the method on flakes of specular hematite and biotite, as well as on thin sections of different rocks (arfvedsonitic granite, oolitic hematite, diabase, and quartz conglomerate) treated with SRB, and discuss possible artifacts that can occur. To our knowledge, this is the only microscopic technique that can image Fe(II) zones on the surface of an Fe-bearing mineral with monolayer sensitivity.

  12. Quantifying phosphoric acid in high-temperature polymer electrolyte fuel cell components by X-ray tomographic microscopy.

    PubMed

    Eberhardt, S H; Marone, F; Stampanoni, M; Büchi, F N; Schmidt, T J

    2014-11-01

    Synchrotron-based X-ray tomographic microscopy is investigated for imaging the local distribution and concentration of phosphoric acid in high-temperature polymer electrolyte fuel cells. Phosphoric acid fills the pores of the macro- and microporous fuel cell components. Its concentration in the fuel cell varies over a wide range (40-100 wt% H3PO4). This renders the quantification and concentration determination challenging. The problem is solved by using propagation-based phase contrast imaging and a referencing method. Fuel cell components with known acid concentrations were used to correlate greyscale values and acid concentrations. Thus calibration curves were established for the gas diffusion layer, catalyst layer and membrane in a non-operating fuel cell. The non-destructive imaging methodology was verified by comparing image-based values for acid content and concentration in the gas diffusion layer with those from chemical analysis.

  13. Characterization of SiC fibers by soft x-ray photoelectron and photoabsorption spectroscopies and scanning Auger microscopy

    SciTech Connect

    Ma, Qing; McDowell, M.W.; Rosenberg, R.A.

    1996-08-01

    Synchrotron radiation soft x-ray photoelectron and photoabsorption spectroscopy was used to characterize commercially obtained SiC fibers produced by CVD on a W core and followed by a C passivating layer. Depth profiling of the fiber through the C/SiC interface was done by making Si 2p and C 1s core level PES and PAS, as well as scanning Auger microscopy, measurements following Ar{sup +} sputtering. No significant changes in either photoemission or absorption or Auger line shapes were observed versus depth, indicating no significant interfacial reaction. The line shapes of the carbonaceous coatings are predominantely graphite-like and those of the CVD SiC coatings are microcrystalline, with disorder present to some extent in both cases.

  14. Repeated crack healing in MAX-phase ceramics revealed by 4D in situ synchrotron X-ray tomographic microscopy.

    PubMed

    Sloof, Willem G; Pei, Ruizhi; McDonald, Samuel A; Fife, Julie L; Shen, Lu; Boatemaa, Linda; Farle, Ann-Sophie; Yan, Kun; Zhang, Xun; van der Zwaag, Sybrand; Lee, Peter D; Withers, Philip J

    2016-01-01

    MAX phase materials are emerging as attractive engineering materials in applications where the material is exposed to severe thermal and mechanical conditions in an oxidative environment. The Ti2AlC MAX phase possesses attractive thermomechanical properties even beyond a temperature of 1000 K. An attractive feature of this material is its capacity for the autonomous healing of cracks when operating at high temperatures. Coupling a specialized thermomechanical setup to a synchrotron X-ray tomographic microscopy endstation at the TOMCAT beamline, we captured the temporal evolution of local crack opening and healing during multiple cracking and autonomous repair cycles at a temperature of 1500 K. For the first time, the rate and position dependence of crack repair in pristine Ti2AlC material and in previously healed cracks has been quantified. Our results demonstrate that healed cracks can have sufficient mechanical integrity to make subsequent cracks form elsewhere upon reloading after healing. PMID:26972608

  15. 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.

  16. Mapping the subcellular localization of Fe3O4@TiO2 nanoparticles by X-ray Fluorescence Microscopy

    PubMed Central

    Yuan, Y; Chen, S; Gleber, SC; Lai, B; Brister, K; Flachenecker, C; Wanzer, B; Paunesku, T; Vogt, S; Woloschak, GE

    2013-01-01

    The targeted delivery of Fe3O4@TiO2 nanoparticles to cancer cells is an important step in their development as nanomedicines. We have synthesized nanoparticles that can bind the Epidermal Growth Factor Receptor, a cell surface protein that is overexpressed in many epithelial type cancers. In order to study the subcellular distribution of these nanoparticles, we have utilized the sub-micron resolution of X-ray Fluorescence Microscopy to map the locationof Fe3O4@TiO2 NPs and other trace metal elements within HeLa cervical cancer cells. Here we demonstrate how the higher resolution of the newly installed Bionanoprobe at the Advanced Photon Source at Argonne National Laboratory can greatly improve our ability to distinguish intracellular nanoparticles and their spatial relationship with subcellular compartments. PMID:26413134

  17. High-energy x-ray and transmission electron microscopy study of structural transformations in Ti-V

    NASA Astrophysics Data System (ADS)

    Ramsteiner, I. B.; Schöps, A.; Phillipp, F.; Kelsch, M.; Reichert, H.; Dosch, H.; Honkimäki, V.

    2006-01-01

    The binary system Ti-V is a paradigm for the technically important class of Ti β alloys. In the past, it received attention as a candidate for transient ordering. We elucidate the nature of structural transformations by combining transmission electron microscopy (TEM) and a high-energy x-ray diffraction technique. The latter allows to study precipitation processes time resolved and in situ, while TEM is a powerful tool to identify individual phases. In addition to α -Ti precipitation we observe the formation of TiC from minor carbon impurities. Additional diffraction peaks accompanying the α -Ti precipitation and hinting at the existence of a B2-type superstructure are shown to originate from the precipitates. No transient ordering was found.

  18. Repeatability and reproducibility of intracellular molar concentration assessed by synchrotron-based x-ray fluorescence microscopy

    NASA Astrophysics Data System (ADS)

    Merolle, L.; Malucelli, E.; Fratini, M.; Gianoncelli, A.; Notargiacomo, A.; Cappadone, C.; Farruggia, G.; Sargenti, A.; Procopio, A.; Lombardo, M.; Lagomarsino, S.; Iotti, S.

    2016-01-01

    Elemental analysis of biological sample can give information about content and distribution of elements essential for human life or trace elements whose absence is the cause of abnormal biological function or development. However, biological systems contain an ensemble of cells with heterogeneous chemistry and elemental content; therefore, accurate characterization of samples with high cellular heterogeneity may only be achieved by analyzing single cells. Powerful methods in molecular biology are abundant, among them X-Ray microscopy based on synchrotron light source has gaining increasing attention thanks to its extremely sensitivity. However, reproducibility and repeatability of these measurements is one of the major obstacles in achieving a statistical significance in single cells population analysis. In this study, we compared the elemental content of human colon adenocarcinoma cells obtained by three distinct accesses to synchrotron radiation light.

  19. Visualizing Cell Architecture and Molecular Location Using Soft X-Ray Tomography and Correlated Cryo-Light Microscopy

    NASA Astrophysics Data System (ADS)

    McDermott, Gerry; Le Gros, Mark A.; Larabell, Carolyn A.

    2012-05-01

    Living cells are structured to create a range of microenvironments that support specific chemical reactions and processes. Understanding how cells function therefore requires detailed knowledge of both the subcellular architecture and the location of specific molecules within this framework. Here we review the development of two correlated cellular imaging techniques that fulfill this need. Cells are first imaged using cryogenic fluorescence microscopy to determine the location of molecules of interest that have been labeled with fluorescent tags. The same specimen is then imaged using soft X-ray tomography to generate a high-contrast, 3D reconstruction of the cells. Data from the two modalities are then combined to produce a composite, information-rich view of the cell. This correlated imaging approach can be applied across the spectrum of problems encountered in cell biology, from basic research to biotechnological and biomedical applications such as the optimization of biofuels and the development of new pharmaceuticals.

  20. 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. PMID:23027799

  1. Characterisation of mineralisation of bone and cartilage: X-ray diffraction and Ca and Sr K α X-ray fluorescence microscopy

    NASA Astrophysics Data System (ADS)

    Bradley, D. A.; Muthuvelu, P.; Ellis, R. E.; Green, E. M.; Attenburrow, D.; Barrett, R.; Arkill, K.; Colridge, D. B.; Winlove, C. P.

    2007-10-01

    Bone is a dynamic structure, constantly remodelling in response to changing mechanical and environmental factors. This is particularly evident in the mineral component encrusting the collagenous framework. The mineral is principally in the form of calcium apatite, but calcium can exchange with strontium, both during the cellular processes of mineralisation and resorption and by passive exchange with the deposited crystals. Mineralisation is generally characterized by densitometry, but because of the differences in absorption cross sections of calcium and strontium it can be misleading in studies of composition. In this work we have used X-ray diffraction to identify calcium and strontium apatite and X-ray fluorescence to quantify strontium and calcium distribution. With the beam characteristics available from synchrotron radiation, this has enabled us to obtain microscopic resolution on thin sections of bone and cartilage from the equine metacarpophalangeal joint. Two issues have been investigated; the first is the distribution of mineral in the bone-cartilage interface and within individual trabeculae. In trabecular bone the ratio of strontium to calcium concentration was typically 0.0035 ± 0.0020, and higher by a factor of ∼3 at the periphery than in the centre of a trabeculum (possibly reflecting the more rapid turnover of mineral in the surface layer). In the dense subchondral bone the ratio was similar, approximately doubling in the calcified cartilage. The second objective was to explore the changes in mineralisation associated with development of osteoarthrosis. We analysed lesions showing cartilage thinning and changes in the trabecular organization and density of the underlying bone. At the centre of the lesion the ratio of strontium to calcium was much lower than that in normal tissue, although the calcified cartilage still showed a higher ratio than the underlying bone. In the superficially normal tissue around the lesion the calcified cartilage

  2. Wide-Band KB Optics for Spectro-Microscopy Imaging Applications in the 6-13 keV X-ray Energy Range

    SciTech Connect

    Ziegler, E.; De Panfilis, S.; Peverini, L.; Vaerenbergh, P. van; Rocca, F.

    2007-01-19

    We present a Kirkpatrick-Baez optics (KB) system specially optimized to operate in the 6-13 keV X-ray range, where valuable characteristic lines are present. The mirrors are coated with aperiodic laterally graded (Ru/B4C)35 multilayers to define a 15% energy bandpass and to gain flux as compared to total reflection mirrors. For any X-ray energy selected the shape of each mirror can be optimized with a dynamical bending system so as to concentrate the X-ray beam into a micrometer-size spot. Once the KB mirrors are aligned at the X-ray energy corresponding to the barycenter of the XAS spectrum to be performed they remain in a steady state during the micro-XAS scans to minimize beam displacements. Results regarding the performance of the wideband KB optics and of the spectro-microscopy setup are presented, including beam stability issues.

  3. The Swift Supergiant Fast X-Ray Transients Project:. [A Review, New Results and Future Perspectives

    NASA Technical Reports Server (NTRS)

    Romano, P.; Mangano, V.; Ducci, L.; Esposito, P.; Vercellone, S.; Bocchino, F.; Burrows, D. N.; Kennea, J. A.; Krimm, H. A.; Gehrels, N.; Farinelli, R.; Ceccobello, C.

    2013-01-01

    We present a review of the Supergiant Fast X-ray Transients (SFXT) Project, a systematic investigation of the properties of SFXTs with a strategy that combines Swift monitoring programs with outburst follow-up observations. This strategy has quickly tripled the available sets of broad-band data of SFXT outbursts, and gathered a wealth of out-of-outburst data, which have led us to a broad-band spectral characterization, an assessment of the fraction of the time these sources spend in each phase, and their duty cycle of inactivity. We present some new observational results obtained through our outburst follow-ups, as fitting examples of the exceptional capabilities of Swift in catching bright flares and monitor them panchromatically.

  4. 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).

  5. A method for volumetric imaging in radiotherapy using single x-ray projection

    SciTech Connect

    Xu, Yuan; Yan, Hao; Ouyang, Luo; Wang, Jing; Jiang, Steve B. E-mail: steve.jiang@utsouthwestern.edu Jia, Xun E-mail: steve.jiang@utsouthwestern.edu; Zhou, Linghong; Cervino, Laura

    2015-05-15

    Purpose: It is an intriguing problem to generate an instantaneous volumetric image based on the corresponding x-ray projection. The purpose of this study is to develop a new method to achieve this goal via a sparse learning approach. Methods: To extract motion information hidden in projection images, the authors partitioned a projection image into small rectangular patches. The authors utilized a sparse learning method to automatically select patches that have a high correlation with principal component analysis (PCA) coefficients of a lung motion model. A model that maps the patch intensity to the PCA coefficients was built along with the patch selection process. Based on this model, a measured projection can be used to predict the PCA coefficients, which are then further used to generate a motion vector field and hence a volumetric image. The authors have also proposed an intensity baseline correction method based on the partitioned projection, in which the first and the second moments of pixel intensities at a patch in a simulated projection image are matched with those in a measured one via a linear transformation. The proposed method has been validated in both simulated data and real phantom data. Results: The algorithm is able to identify patches that contain relevant motion information such as the diaphragm region. It is found that an intensity baseline correction step is important to remove the systematic error in the motion prediction. For the simulation case, the sparse learning model reduced the prediction error for the first PCA coefficient to 5%, compared to the 10% error when sparse learning was not used, and the 95th percentile error for the predicted motion vector was reduced from 2.40 to 0.92 mm. In the phantom case with a regular tumor motion, the predicted tumor trajectory was successfully reconstructed with a 0.82 mm error for tumor center localization compared to a 1.66 mm error without using the sparse learning method. When the tumor motion

  6. A method for volumetric imaging in radiotherapy using single x-ray projection

    PubMed Central

    Xu, Yuan; Yan, Hao; Ouyang, Luo; Wang, Jing; Zhou, Linghong; Cervino, Laura; Jiang, Steve B.; Jia, Xun

    2015-01-01

    Purpose: It is an intriguing problem to generate an instantaneous volumetric image based on the corresponding x-ray projection. The purpose of this study is to develop a new method to achieve this goal via a sparse learning approach. Methods: To extract motion information hidden in projection images, the authors partitioned a projection image into small rectangular patches. The authors utilized a sparse learning method to automatically select patches that have a high correlation with principal component analysis (PCA) coefficients of a lung motion model. A model that maps the patch intensity to the PCA coefficients was built along with the patch selection process. Based on this model, a measured projection can be used to predict the PCA coefficients, which are then further used to generate a motion vector field and hence a volumetric image. The authors have also proposed an intensity baseline correction method based on the partitioned projection, in which the first and the second moments of pixel intensities at a patch in a simulated projection image are matched with those in a measured one via a linear transformation. The proposed method has been validated in both simulated data and real phantom data. Results: The algorithm is able to identify patches that contain relevant motion information such as the diaphragm region. It is found that an intensity baseline correction step is important to remove the systematic error in the motion prediction. For the simulation case, the sparse learning model reduced the prediction error for the first PCA coefficient to 5%, compared to the 10% error when sparse learning was not used, and the 95th percentile error for the predicted motion vector was reduced from 2.40 to 0.92 mm. In the phantom case with a regular tumor motion, the predicted tumor trajectory was successfully reconstructed with a 0.82 mm error for tumor center localization compared to a 1.66 mm error without using the sparse learning method. When the tumor motion

  7. In situ characterization of aluminum-containing mineral-microorganism aqueous suspensions using scanning transmission X-ray microscopy.

    PubMed

    Yoon, Tae Hyun; Johnson, Stephen B; Benzerara, Karim; Doyle, Colin S; Tyliszczak, Tolek; Shuh, David K; Brown, Gordon E

    2004-11-23

    In situ characterization of colloidal particles under hydrous conditions is one of the key requirements for understanding their state of aggregation and impact on the transport of pollutants in aqueous environments. Scanning transmission X-ray microscopy (STXM) is one of the few techniques that can satisfy this need by providing element- and chemical-state-specific 2-D maps at a spatial resolution better than 50 nm using soft X-rays from synchrotron radiation wiggler or undulator sources tuned to the absorption edges of different elements. X-ray absorption near-edge structure (XANES) spectra can also be collected simultaneously at a similar spatial resolution and can provide phase identification in many cases. In this study, we report STXM images and XANES spectroscopy measurements at or above the Al K-edge (E = 1559.6 eV) of various Al-containing minerals and synthetic oxides [alpha-Al2O3 (corundum), gamma-Al2O3, gamma-AlOOH (boehmite), alpha-Al(OH)3 (bayerite), KAl2(AlSi3O10)(OH)2 (muscovite), (Al,Mg)8(Si4O10)4(OH)8.nH2O (montmorillonite), and Mg6Al2(OH)16CO3.4H2O (hydrotalcite)] and demonstrate the capability of this spectromicroscopic tool to identify different Al-containing mineral colloids in multiphase mixtures in aqueous solution. We also demonstrate that STXM imaging at or above the C K-edge (E = 284.2 eV) and Al K-edge can provide unique information on the interactions between bacteria and Al-containing nanoparticles in aqueous suspensions. STXM images of a mixture of Caulobacter crescentus and montmorillonite and corundum particles just above the C and Al K-edges show that the mineral particles and bacteria are closely associated in aggregates, which is likely due to the binding of bacteria to clay and corundum particles by extracellular polysaccharides.

  8. Ordering in bio-inorganic hybrid nanomaterials probed by in situ scanning transmission X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Lee, Jonathan R. I.; Bagge-Hansen, Michael; Tunuguntla, Ramya; Kim, Kyunghoon; Bangar, Mangesh; Willey, Trevor M.; Tran, Ich C.; Kilcoyne, David A.; Noy, Aleksandr; van Buuren, Tony

    2015-05-01

    Phospholipid bilayer coated Si nanowires are one-dimensional (1D) composites that provide versatile bio-nanoelectronic functionality via incorporation of a wide variety of biomolecules into the phospholipid matrix. The physiochemical behaviour of the phospholipid bilayer is strongly dependent on its structure and, as a consequence, substantial modelling and experimental efforts have been directed at the structural characterization of supported bilayers and unsupported phospholipid vesicles; nonetheless, the experimental studies conducted to date have exclusively involved volume-averaged techniques, which do not allow for the assignment of spatially resolved structural variations that could critically impact the performance of the 1D phospholipid-Si NW composites. In this manuscript, we use scanning transmission X-ray microscopy (STXM) to probe bond orientation and bilayer thickness as a function of position with a spatial resolution of ~30 nm for Δ9-cis 1,2-dioleoyl-sn-glycero-3-phosphocholine layers prepared Si NWs. When coupled with small angle X-ray scattering measurements, the STXM data reveal structural motifs of the Si NWs that give rise to multi-bilayer formation and enable assignment of the orientation of specific bonds known to affect the order and rigidity of phospholipid bilayers.Phospholipid bilayer coated Si nanowires are one-dimensional (1D) composites that provide versatile bio-nanoelectronic functionality via incorporation of a wide variety of biomolecules into the phospholipid matrix. The physiochemical behaviour of the phospholipid bilayer is strongly dependent on its structure and, as a consequence, substantial modelling and experimental efforts have been directed at the structural characterization of supported bilayers and unsupported phospholipid vesicles; nonetheless, the experimental studies conducted to date have exclusively involved volume-averaged techniques, which do not allow for the assignment of spatially resolved structural

  9. 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.

  10. X-ray laser

    DOEpatents

    Nilsen, Joseph

    1991-01-01

    An X-ray laser (10) that lases between the K edges of carbon and oxygen, i.e. between 44 and 23 Angstroms, is provided. The laser comprises a silicon (12) and dysprosium (14) foil combination (16) that is driven by two beams (18, 20) of intense line focused (22, 24) optical laser radiation. Ground state nickel-like dysprosium ions (34) are resonantly photo-pumped to their upper X-ray laser state by line emission from hydrogen-like silicon ions (32). The novel X-ray laser should prove especially useful for the microscopy of biological specimens.

  11. X-rays of inner worlds: the mid-twentieth-century American projective test movement.

    PubMed

    Lemov, Rebecca

    2011-01-01

    This essay begins to tell the neglected history of the projective test movement in the U.S. behavioral sciences from approximately 1941 to 1968. This cross-disciplinary enterprise attempted to use projective techniques as "X-ray" machines to see into the psyches of subjects tested around the world. The aim was to gather subjective materials en masse, pursuing data on a scope, scale, and manner rarely hazarded before in any science. In particular, the targeted data included the traces of the inner life and elusive aspects of subjective experience including dreams, life stories, and myriad test results from a battery of tests. This essay explores how the movement and the experimental data bank that resulted were unlikely yet telling sites for the practice and pursuit of the Cold War human sciences. To look closely at the encounters that resulted is to show how the most out-of-the-way places and seemingly insignificant moments played a role in heady scientific ambitions and global geopolitical projects. At times, the projective test movement became a mirror of Cold War rationality itself, as tests were employed at the very limits of their possible extension. The essay argues for an off-kilter centrality in the movement itself, shedding light on the would-be unified social sciences after World War II and the "subjective turn" they took. PMID:21732375

  12. Imaging of the intracellular topography of copper with a fluorescent sensor and by synchrotron x-ray fluorescence microscopy

    PubMed Central

    Yang, Liuchun; McRae, Reagan; Henary, Maged M.; Patel, Raxit; Lai, Barry; Vogt, Stefan; Fahrni, Christoph J.

    2005-01-01

    Copper is an essential micronutrient that plays a central role for a broad range of biological processes. Although there is compelling evidence that the intracellular milieu does not contain any free copper ions, the rapid kinetics of copper uptake and release suggests the presence of a labile intracellular copper pool. To elucidate the subcellular localization of this pool, we have synthesized and characterized a membrane-permeable, copper-selective fluorescent sensor (CTAP-1). Upon addition of Cu(I), the sensor exhibits a 4.6-fold emission enhancement and reaches a quantum yield of 14%. The sensor exhibits excellent selectivity toward Cu(I), and its emission response is not compromised by the presence of millimolar concentrations of Ca(II) or Mg(II) ions. Variable temperature dynamic NMR studies revealed a rapid Cu(I) self-exchange equilibrium with a low activation barrier of ΔG‡ = 44 kJ·mol–1 and kobs ∼ 105 s–1 at room temperature. Mouse fibroblast cells (3T3) incubated with the sensor produced a copper-dependent perinuclear staining pattern, which colocalizes with the subcellular locations of mitochondria and the Golgi apparatus. To evaluate and confirm the sensor's copper-selectivity, we determined the subcellular topography of copper by synchrotron-based x-ray fluorescence microscopy. Furthermore, microprobe x-ray absorption measurements at various subcellular locations showed a near-edge feature that is characteristic for low-coordinate monovalent copper but does not resemble the published spectra for metallothionein or glutathione. The presented data provide a coherent picture with strong evidence for a kinetically labile copper pool, which is predominantly localized in the mitochondria and the Golgi apparatus. PMID:16061820

  13. Quantified, whole section trace element mapping of carbonaceous chondrites by Synchrotron X-ray Fluorescence Microscopy: 1. CV meteorites

    NASA Astrophysics Data System (ADS)

    Dyl, Kathryn A.; Cleverley, James S.; Bland, Phil A.; Ryan, Chris G.; Fisher, Louise A.; Hough, Robert M.

    2014-06-01

    We present the application of a new synchrotron-based technique for rapid mapping of trace element distributions across large areas of the CV3 meteorites Allende and Vigarano. This technique utilizes the Australian Synchrotron X-ray Fluorescence Microscopy (XFM) beam line with its custom designed and built X-ray detector array called Maia. XFM with Maia allows data to be collected using a 2 μm spot size at very low dwell times (∼0.1-0.5 ms), resulting in maps of entire thin sections in ∼5 h. Maia is an energy dispersive detector system with a large collection solid-angle, which allows full spectral acquisition and high sensitivity. Hence, there is no need to constrain the elements of interest a priori. We collected whole section maps (∼2 cm × 1 cm) from 3 thick sections of Allende and a single map (2 cm × 1.5 cm) from a thick section of Vigarano. Our experimental conditions provide data for elements with 20 ⩽ Z ⩽ 40 (K-shell, Ca through Zr) and the L-emissions of Os, Ir, Pt, Au, and Pb. We illustrate the unique capabilities of this technique by presenting observations across myriad length scales, from the centimeter-scale down to the detection of sub-micrometer particles within these objects. Our initial results show the potential of this technique to help decipher spatial and textural variations in trace element chemistry between CAIs, chondrules, matrix, and other chondritic components. We also illustrate how these datasets can be applied to understanding both nebular and parent-body processes within meteorites.

  14. Imaging of the intracellular topography of copper with a fluorescent sensor and by synchrotron x-ray fluorescence microscopy.

    PubMed

    Yang, Liuchun; McRae, Reagan; Henary, Maged M; Patel, Raxit; Lai, Barry; Vogt, Stefan; Fahrni, Christoph J

    2005-08-01

    Copper is an essential micronutrient that plays a central role for a broad range of biological processes. Although there is compelling evidence that the intracellular milieu does not contain any free copper ions, the rapid kinetics of copper uptake and release suggests the presence of a labile intracellular copper pool. To elucidate the subcellular localization of this pool, we have synthesized and characterized a membrane-permeable, copper-selective fluorescent sensor (CTAP-1). Upon addition of Cu(I), the sensor exhibits a 4.6-fold emission enhancement and reaches a quantum yield of 14%. The sensor exhibits excellent selectivity toward Cu(I), and its emission response is not compromised by the presence of millimolar concentrations of Ca(II) or Mg(II) ions. Variable temperature dynamic NMR studies revealed a rapid Cu(I) self-exchange equilibrium with a low activation barrier of deltaG++ = 44 kJ.mol(-1) and k(obs) approximately 10(5) s(-1) at room temperature. Mouse fibroblast cells (3T3) incubated with the sensor produced a copper-dependent perinuclear staining pattern, which colocalizes with the subcellular locations of mitochondria and the Golgi apparatus. To evaluate and confirm the sensor's copper-selectivity, we determined the subcellular topography of copper by synchrotron-based x-ray fluorescence microscopy. Furthermore, microprobe x-ray absorption measurements at various subcellular locations showed a near-edge feature that is characteristic for low-coordinate monovalent copper but does not resemble the published spectra for metallothionein or glutathione. The presented data provide a coherent picture with strong evidence for a kinetically labile copper pool, which is predominantly localized in the mitochondria and the Golgi apparatus.

  15. Oxygenated interface on biomass burn tar balls determined by single particle scanning transmission X-ray microscopy.

    PubMed

    Tivanski, Alexei V; Hopkins, Rebecca J; Tyliszczak, Tolek; Gilles, Mary K

    2007-06-28

    Carbonaceous particles originating from biomass burning can account for a large fraction of organic aerosols in a local environment. Presently, their composition, physical and chemical properties, as well as their environmental effects are largely unknown. Tar balls, a distinct type of highly spherical carbonaceous biomass burn particles, have been observed in a number of field campaigns. The Yosemite Aerosol Characterization Study that took place in summer 2002 occurred during an active fire season in the western United States; tar balls collected during this field campaign are described in this article. Scanning transmission X-ray microscopy and near-edge X-ray absorption fine structure spectroscopy are used to determine the shape, structure, and size-dependent chemical composition of approximately 150 individual spherical particles ranging in size from 0.15 to 1.2 mum. The elemental composition of tar balls is approximately 55% atomic carbon and approximately 45% atomic oxygen. Oxygen is present primarily as carboxylic carbonyls and oxygen-substituted alkyl (O-alkyl-C) functional groups, followed by moderate amounts of ketonic carbonyls. The observed chemical composition, density, and carbon functional groups are distinctly different from soot or black carbon and more closely resemble high molecular weight polymeric humic-like substances, which could account for their reported optical properties. A detailed examination of the carboxylic carbonyl and O-alkyl-C functional groups as a function of particle size reveals a thin oxygenated interface layer. The high oxygen content, as well as the presence of water-soluble carboxylic carbonyl groups, could account for the reported hygroscopic properties of tar balls. The presence of the oxygenated layer is attributed to atmospheric processing of biomass burn particles.

  16. Tracking Changes in Absorptivity, Stiffness, and Organic Chemical Composition in Laboratory Generated HULIS SOA using Atomic Force Microscopy and X-ray Microscopy

    NASA Astrophysics Data System (ADS)

    Hawkins, L. N.; Lemire, A.; Kong, W.

    2014-12-01

    Light absorbing organic compounds are among the many products of aqueous phase secondary organic aerosol formation. Once formed, these compounds can alter the optical and material properties of SOA in ways that impact their ability to scatter and absorb solar radiation, deliquesce and evaporate quickly during cloud cycling, and react with gas phase species such as oxidants. To quantify these effects, we have characterized the changes in UV-visible absorption, stiffness, and particle shape that occur when aqueous SOA is exposed to repeated wet-dry cycles and photooxidation. Material properties were measured with Atomic Force Microscopy of atomized laboratory generated SOA; this material was created by combining glyoxal, methylglyoxal, or glycolaldehyde with ammonium sulfate, glycine, or methylamine in solution and either spray drying or evaporating the bulk solution. In addition to optical and material properties, changes in organic functional groups were tracked using scanning transmission x-ray microscopy (STXM) of the near carbon edge x-ray absorption fine structure (NEXAFS). Photooxidation experiments of the same aqueous SOA revealed concomitant changes in the organic functional groups and light absorption spectra, along with measurable changes in particle stiffness.

  17. In Depth Analyses of LEDs by a Combination of X-ray Computed Tomography (CT) and Light Microscopy (LM) Correlated with Scanning Electron Microscopy (SEM).

    PubMed

    Meyer, Jörg; Thomas, Christian; Tappe, Frank; Ogbazghi, Tekie

    2016-01-01

    In failure analysis, device characterization and reverse engineering of light emitting diodes (LEDs), and similar electronic components of micro-characterization, plays an important role. Commonly, different techniques like X-ray computed tomography (CT), light microscopy (LM) and scanning electron microscopy (SEM) are used separately. Similarly, the results have to be treated for each technique independently. Here a comprehensive study is shown which demonstrates the potentials leveraged by linking CT, LM and SEM. In depth characterization is performed on a white emitting LED, which can be operated throughout all characterization steps. Major advantages are: planned preparation of defined cross sections, correlation of optical properties to structural and compositional information, as well as reliable identification of different functional regions. This results from the breadth of information available from identical regions of interest (ROIs): polarization contrast, bright and dark-field LM images, as well as optical images of the LED cross section in operation. This is supplemented by SEM imaging techniques and micro-analysis using energy dispersive X-ray spectroscopy. PMID:27341190

  18. In Depth Analyses of LEDs by a Combination of X-ray Computed Tomography (CT) and Light Microscopy (LM) Correlated with Scanning Electron Microscopy (SEM).

    PubMed

    Meyer, Jörg; Thomas, Christian; Tappe, Frank; Ogbazghi, Tekie

    2016-06-16

    In failure analysis, device characterization and reverse engineering of light emitting diodes (LEDs), and similar electronic components of micro-characterization, plays an important role. Commonly, different techniques like X-ray computed tomography (CT), light microscopy (LM) and scanning electron microscopy (SEM) are used separately. Similarly, the results have to be treated for each technique independently. Here a comprehensive study is shown which demonstrates the potentials leveraged by linking CT, LM and SEM. In depth characterization is performed on a white emitting LED, which can be operated throughout all characterization steps. Major advantages are: planned preparation of defined cross sections, correlation of optical properties to structural and compositional information, as well as reliable identification of different functional regions. This results from the breadth of information available from identical regions of interest (ROIs): polarization contrast, bright and dark-field LM images, as well as optical images of the LED cross section in operation. This is supplemented by SEM imaging techniques and micro-analysis using energy dispersive X-ray spectroscopy.

  19. The TESIS Project: Are Type 2 QSO Hidden in X-Ray Emitting EROs?

    NASA Astrophysics Data System (ADS)

    Severgnini, P.; Della Ceca, R.; Braito, V.; Saracco, P.; Longhetti, M.; Bender, R.; Drory, N.; Feulner, G.; Hopp, U.; Mannucci, F.; Maraston, C.

    X-ray selected EROs are, on average, the hardest X-ray sources in medium and deep X-ray fields. This coupled with their extremely red colors (R-K > 5) suggest that they represent one of the most promising population where looking for high-luminosity (LX > 1044 erg s-1) and X-ray obscured (NH > 1022 cm-2) type2 AGNs, the so called QSO2 (e.g., [5]; [4]; Mignoli et al. submitted to A&A). These latter are predicted in large density by the synthesis model of the Cosmic X-ray background [9] even if only few observational evidences have been found so far (e.g., [1] and references therein; Caccianiga et al. A&A accepted).

  20. Raman microscopy and x-ray fluorescence analysis of pigments on medieval and Renaissance Italian manuscript cuttings

    PubMed Central

    Burgio, Lucia; Clark, Robin J. H.; Hark, Richard R.

    2010-01-01

    Italian medieval and Renaissance manuscript cuttings and miniatures from the Victoria and Albert Museum were analyzed by Raman microscopy to compile a database of pigments used in different periods and different Italian regions. The palette identified in most manuscripts and cuttings was found to include lead white, gypsum, azurite, lazurite, indigo, malachite, vermilion, red lead, lead tin yellow (I), goethite, carbon, and iron gall ink. A few of the miniatures, such as the historiated capital “M” painted by Gerolamo da Cremona and the Petrarca manuscript by Bartolomeo Sanvito, are of exceptional quality and were analyzed extensively; some contained unusual materials. The widespread usage of iron oxides such as goethite and hematite as minor components of mixtures with azurite is particularly notable. The use of a needle-shaped form of iron gall ink as a pigment rather than a writing material was established by both Raman microscopy and x-ray fluorescence spectroscopy for the Madonna and Child by Franco de’ Russi. PMID:20304797

  1. 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.

  2. 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. PMID:27212049

  3. 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.

  4. Coagulation of Na-montmorillonite by inorganic cations at neutral pH. A combined transmission X-ray microscopy, small angle and wide angle X-ray scattering study.

    PubMed

    Michot, Laurent J; Bihannic, Isabelle; Thomas, Fabien; Lartiges, Bruno S; Waldvogel, Yves; Caillet, Céline; Thieme, Juergen; Funari, Sérgio S; Levitz, Pierre

    2013-03-12

    The coagulation of sodium montmorillonite by inorganic salts (NaNO3, Ca(NO3)2 and La(NO3)3) was studied by combining classical turbidity measurements with wide-angle-X-ray scattering (WAXS), small-angle-X-ray scattering (SAXS), and transmission X-ray microscopy (TXM). Using size-selected samples, such a combination, associated with an original quantitative treatment of TXM images, provides a true multiscale investigation of the formed structures in a spatial range extending from a few ångstroms to a few micrometers. We then show that, at neutral pH and starting with fully Na-exchanged samples, coagulation proceeds via the formation of stacks of particles with a slight mismatch between layers. These stacks arrange themselves into larger porous anisotropic particles, the porosity of which depends on the valence of the cation used for coagulation experiments. Face-face coagulation is clearly dominant under those conditions, and no evidence for significant face-edge coagulation was found. These structures appear to arrange as larger clusters, the organization of which should control the mechanical properties of the flocs. PMID:23421550

  5. Photoionization-pumped, Ne II, x-ray laser studies project. Final report

    SciTech Connect

    Richardson, M.C.; Hagelstein, P.L.; Eckart, M.J.; Forsyth, J.M.; Gerrassimenko, M.; Soures, J.M.

    1984-01-01

    The energetics of this pumping scheme are shown. Short-pulse (50 to 100 ps) laser irradiation of an appropriate x-ray flashlamp medium generates broad-band emission in the range of 300 to 800 eV which preferentially photoionizes Ne to the /sup 2/S state of Ne II creating an inversion at approximately 27 eV. Although this approach does not depend on precise spectral overlap between the x-ray pump radiation and the medium to be pumped, it does require that the x-ray medium remain un-ionized prior to photoionization by the soft x-ray emission. Well-controlled focus conditions are required to ensure that the x-ray medium is not subjected to electron or x-ray preheat prior to irradiation by the soft x-ray source. The magnitude of the population inversion is predicted to be critically dependent upon rapid photoionization of the two states; therefore, ultra-short pulse irradiation of the laser flashlamps is required.

  6. The EXTraS project: Exploring the X-ray Transient and variable Sky

    NASA Astrophysics Data System (ADS)

    De Luca, A.; Tiengo, A.; D'Agostino, D.; Watson, M.; Haberl, F.; Wilms, J.

    2016-06-01

    The EXTraS project is extracting the hitherto unexplored temporal domain information buried in the serendipitous data collected by XMM-Newton/EPIC since its launch. This includes a search for fast transients, missed by standard image analysis, as well as a search and characterization of variability (both periodic and aperiodic) in hundreds of thousands of sources, spanning more than nine orders of magnitude in time scale and six orders of magnitude in flux. Phenomenological classification of variable sources will also be performed. All our results, together with new analysis tools, will be made available to the community in an easy-to-use form at the end of 2016, with prospects of extending the analysis to future data. EXTraS products will have a very broad range of applications, from the search for rare events to population studies, with a large impact in almost all fields of astrophysics. This will boost the scientific exploitation of XMM data and make EPIC the reference for time-domain astronomy in the soft X-rays. The EXTraS project (2014-2016), funded within the EU/FP7 framework, is carried out by a collaboration including INAF (Italy), IUSS (Italy), CNR/IMATI (Italy), University of Leicester (UK), MPE (Germany) and ECAP (Germany).

  7. 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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  8. An Inquiry-Based Project Focused on the X-Ray Powder Diffraction Analysis of Common Household Solids

    ERIC Educational Resources Information Center

    Hulien, Molly L.; Lekse, Jonathan W.; Rosmus, Kimberly A.; Devlin, Kasey P.; Glenn, Jennifer R.; Wisneski, Stephen D.; Wildfong, Peter; Lake, Charles H.; MacNeil, Joseph H.; Aitken, Jennifer A.

    2015-01-01

    While X-ray powder diffraction (XRPD) is a fundamental analytical technique used by solid-state laboratories across a breadth of disciplines, it is still underrepresented in most undergraduate curricula. In this work, we incorporate XRPD analysis into an inquiry-based project that requires students to identify the crystalline component(s) of…

  9. The Effect of Electrode Coupling on Single Molecule Device Characteristics: An X-Ray Spectroscopy and Scanning Probe Microscopy Study

    NASA Astrophysics Data System (ADS)

    Batra, Arunabh

    This thesis studies electronic properties of molecular devices in the limiting cases of strong and weak electrode-molecule coupling. In these two limits, we use the complementary techniques of X-Ray spectroscopy and Scanning Tunneling Microscopy (STM) to understand the mechanisms for electrode-molecule bond formation, the energy level realignment due to metal-molecule bonds, the effect of coupling strength on single-molecule conductance in low-bias measurements, and the effect of coupling on transport under high-bias. We also introduce molecular designs with inherent asymmetries, and develop an analytical method to determine the effect of these features on high-bias conductance. This understanding of the role of electrode-molecule coupling in high-bias regimes enables us to develop a series of functional electronic devices whose properties can be predictably tuned through chemical design. First, we explore the weak electrode-molecule coupling regime by studing the interaction of two types of paracyclophane derivates that are coupled 'through-space' to underlying gold substrates. The two paracyclophane derivatives differ in the strength of their intramolecular through-space coupling. X-Ray photoemission spectroscopy (XPS) and Near-Edge X-ray Absorbance Fine Structure (NEXAFS) spectroscopy allows us to determine the orientation of both molecules; Resonant Photoemission Spectroscopy (RPES) then allows us to measure charge transfer time from molecule to metal for both molecules. This study provides a quantititative measure of charge transfer time as a function of through-space coupling strength. Next we use this understanding in STM based single-molecule current-voltage measurements of a series of molecules that couple through-space to one electrode, and through-bond to the other. We find that in the high-bias regime, these molecules respond differently depending on the direction of the applied field. This asymmetric response to electric field direction results in

  10. The making of the Chandra X-Ray Observatory: The project scientist’s perspective

    PubMed Central

    Weisskopf, Martin C.

    2010-01-01

    The history of the development of the Chandra X-Ray Observatory is reviewed from a personal perspective. This review is necessarily biased and limited by space because it attempts to cover a time span approaching five decades. PMID:20194740

  11. Scanning transmission X-ray microscopy of nano structured thin film catalysts for proton-exchange-membrane fuel cells

    NASA Astrophysics Data System (ADS)

    Lee, Vincent; Berejnov, Viatcheslav; West, Marcia; Kundu, Sumit; Susac, Darija; Stumper, Jürgen; Atanasoski, Radoslav T.; Debe, Mark; Hitchcock, Adam P.

    2014-10-01

    Scanning transmission X-ray microscopy (STXM) has been applied to characterize nano structured thin film (NSTF) catalysts implemented as electrode materials in proton-exchange-membrane (PEM) fuel cells. STXM is used to study all chemical constituents at various stages in the fabrication process, from the perylene red (PR149) starting material, through the formation of the uncoated perylene whiskers, their coated form with Pt-based catalyst, and toward the NSTF anode fully integrated into the catalyst coated membrane (CCM). CCM samples were examined prior to operational testing and after several different accelerated testing protocols: start-up/shut-down (SU/SD), and reversal tests. It was found that, while the perylene support material is present in the pre-test samples, it was completely absent in the post-test samples. We attribute this loss of perylene material to the presence of cracks in the catalyst combined with intensive hydrogenation processes happening at the anode during operation. Despite the loss of the perylene support, the platinum shells forming the NSTF anode catalyst layer performed well during the tests.

  12. Smectite flocculation structure modified by Al13 macro-molecules--as revealed by the transmission X-ray microscopy (TXM).

    PubMed

    Zbik, Marek S; Martens, Wayde N; Frost, Ray L; Song, Yen-Fang; Chen, Yi-Ming; Chen, Jian-Hua

    2010-05-01

    The aggregate structure which occurs in aqueous smectitic suspensions is responsible for poor water clarification, difficulties in sludge dewatering and the unusual rheological behaviour of smectite rich soils. These macroscopic properties are dictated by the 3D structural arrangement of smectite finest fraction within flocculated aggregates. Here, we report results from a relatively new technique, transmission X-ray microscopy (TXM), which makes it possible to investigate the internal structure and 3D tomographic reconstruction of the smectite clay aggregates modified by Al(13) Keggin macro-molecule [Al(13)(O)(4)(OH)(24)(H(2)O)(12)](7+). Three different treatment methods were shown resulted in three different micro-structural environments of the resulting flocculation. In case of smectite sample prepared in Methods 1 and 3 particles fall into the primary minimum where Van der Waals forces act between FF oriented smectite flakes and aggregates become approach irreversible flocculation. In case of sample prepared using Method 2, particles contacting by edges (EE) and edge to face (EF) orientation fell into secondary minimum and weak flocculation resulted in severe gelation and formation of the micelle-like texture in fringe superstructure, which was first time observed in smectite based gel.

  13. Real-time X-ray transmission microscopy for fundamental studies solidification: Al-Al2Au eutectic

    NASA Astrophysics Data System (ADS)

    Curreri, Peter A.; Kaukler, William F.; Sen, Subhayu

    1998-01-01

    High resolution real-time X-ray Transmission Microscopy, XTM, has been applied to obtain information fundamental to solidification of optically opaque metallic systems. We have previously reported the measurement of the solute profile in the liquid, phase growth, and detailed solid-liquid interfacial morphology of aluminum based alloys with exposure times less than 2 seconds. Recent advances in XTM furnace design have provided an increase in real-time magnification (during solidification) for the XTM from 40X to 160X. The increased magnification has enabled for the first time the XTM imaging of real-time growth of fibers and particles with diameters of 5 μm. We have previously applied this system to study the kinetics of formation and morphological evolution of secondary fibers and particles in Al-Bi monotectic alloys. In this paper we present the preliminary results of the first real-time observations of fiber morphology evolution in optically opaque bulk metal sample of Aluminum-Gold eutectic alloy. These studies show that the XTM can be applied to study the fundamentals of eutectic and monotectic solidification. We are currently attempting to apply this technology in the fundamentals of solidification in microgravity.

  14. Real-time X-ray transmission microscopy for fundamental studies solidification: Al-Al{sub 2}Au eutectic

    SciTech Connect

    Curreri, Peter A.; Kaukler, William F.; Sen, Subhayu

    1998-01-15

    High resolution real-time X-ray Transmission Microscopy, XTM, has been applied to obtain information fundamental to solidification of optically opaque metallic systems. We have previously reported the measurement of the solute profile in the liquid, phase growth, and detailed solid-liquid interfacial morphology of aluminum based alloys with exposure times less than 2 seconds. Recent advances in XTM furnace design have provided an increase in real-time magnification (during solidification) for the XTM from 40X to 160X. The increased magnification has enabled for the first time the XTM imaging of real-time growth of fibers and particles with diameters of 5 {mu}m. We have previously applied this system to study the kinetics of formation and morphological evolution of secondary fibers and particles in Al-Bi monotectic alloys. In this paper we present the preliminary results of the first real-time observations of fiber morphology evolution in optically opaque bulk metal sample of Aluminum-Gold eutectic alloy. These studies show that the XTM can be applied to study the fundamentals of eutectic and monotectic solidification. We are currently attempting to apply this technology in the fundamentals of solidification in microgravity.

  15. 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. PMID:26802337

  16. Analysis of ER-mitochondria contacts using correlative fluorescence microscopy and soft X-ray tomography of mammalian cells.

    PubMed

    Elgass, Kirstin D; Smith, Elizabeth A; LeGros, Mark A; Larabell, Carolyn A; Ryan, Michael T

    2015-08-01

    Mitochondrial fission is important for organelle transport, quality control and apoptosis. Changes to the fission process can result in a wide variety of neurological diseases. In mammals, mitochondrial fission is executed by the GTPase dynamin-related protein 1 (Drp1; encoded by DNM1L), which oligomerizes around mitochondria and constricts the organelle. The mitochondrial outer membrane proteins Mff, MiD49 (encoded by MIEF2) and MiD51 (encoded by MIEF1) are involved in mitochondrial fission by recruiting Drp1 from the cytosol to the organelle surface. In addition, endoplasmic reticulum (ER) tubules have been shown to wrap around and constrict mitochondria before a fission event. Up to now, the presence of MiD49 and MiD51 at ER-mitochondrial division foci has not been established. Here, we combine confocal live-cell imaging with correlative cryogenic fluorescence microscopy and soft x-ray tomography to link MiD49 and MiD51 to the involvement of the ER in mitochondrial fission. We gain further insight into this complex process and characterize the 3D structure of ER-mitochondria contact sites.

  17. Elemental changes in the hippocampal formation following two different formulas of ketogenic diet: an X-ray fluorescence microscopy study.

    PubMed

    Chwiej, J; Patulska, A; Skoczen, A; Janeczko, K; Ciarach, M; Simon, R; Setkowicz, Z

    2015-12-01

    The main purpose of the following study was the determination of elemental changes occurring within hippocampal formation as a result of high-fat and carbohydrate-restricted ketogenic diet (KD). To realize it, X-ray fluorescence microscopy was applied for topographic and quantitative analysis of P, S, K, Ca, Fe, Cu, Zn and Se in hippocampal formations taken from rats fed with two different KDs and naive controls. The detailed comparisons were done for sectors 1 and 3 of the Ammon's, the dentate gyrus and hilus of dentate gyrus. The results of elemental analysis showed that the KDs induced statistically significant changes in the accumulation of P, K, Ca, Zn and Se in particular areas of hippocampal formation and these alterations strongly depended on the composition of the diets. Much greater influence on the hippocampal areal densities of examined elements was found for the KD which was characterized by a lower content of carbohydrates, higher content of fats and increased proportion of unsaturated fatty acids. The levels of P, K and Zn decreased whilst those of Ca and Se increased as a result of the treatment with the KDs. PMID:26537249

  18. Smectite flocculation structure modified by Al13 macro-molecules--as revealed by the transmission X-ray microscopy (TXM).

    PubMed

    Zbik, Marek S; Martens, Wayde N; Frost, Ray L; Song, Yen-Fang; Chen, Yi-Ming; Chen, Jian-Hua

    2010-05-01

    The aggregate structure which occurs in aqueous smectitic suspensions is responsible for poor water clarification, difficulties in sludge dewatering and the unusual rheological behaviour of smectite rich soils. These macroscopic properties are dictated by the 3D structural arrangement of smectite finest fraction within flocculated aggregates. Here, we report results from a relatively new technique, transmission X-ray microscopy (TXM), which makes it possible to investigate the internal structure and 3D tomographic reconstruction of the smectite clay aggregates modified by Al(13) Keggin macro-molecule [Al(13)(O)(4)(OH)(24)(H(2)O)(12)](7+). Three different treatment methods were shown resulted in three different micro-structural environments of the resulting flocculation. In case of smectite sample prepared in Methods 1 and 3 particles fall into the primary minimum where Van der Waals forces act between FF oriented smectite flakes and aggregates become approach irreversible flocculation. In case of sample prepared using Method 2, particles contacting by edges (EE) and edge to face (EF) orientation fell into secondary minimum and weak flocculation resulted in severe gelation and formation of the micelle-like texture in fringe superstructure, which was first time observed in smectite based gel. PMID:20149386

  19. Threshold for ion movements in wood cell walls below fiber saturation observed by X-ray fluorescence microscopy (XFM)

    SciTech Connect

    Zelinka, Samuel L.; Gleber, Sophie-Charlotte; Vogt, Stefan; Rodriguez Lopez, Gabriela M.; Jakes, Joseph E.

    2015-05-01

    Diffusion of chemicals and ions through the wood cell wall plays an important role in wood damage mechanisms. In the present work, free diffusion of ions through wood secondary walls and middle lamellae has been investigated as a function of moisture content (MC) and anatomical direction. Various ions (K, Cl, Zn, Cu) were injected into selected regions of 2 mu m thick wood sections with a microinjector and then the ion distribution was mapped by means of X-ray fluorescence microscopy with submicron spatial resolution. The MC of the wood was controlled in situ by means of climatic chamber with controlled relative humidity (RH). For all ions investigated, there was a threshold RH below which the concentration profiles did not change. The threshold RH depended upon ionic species, cell wall layer, and wood anatomical orientation. Above the threshold RH, differences in mobility among ions were observed and the mobility depended upon anatomical direction and cell wall layer. These observations support a recently proposed percolation model of electrical conduction in wood. The results contribute to understanding the mechanisms of fungal decay and fastener corrosion that occur below the fiber saturation point.

  20. Faults and foibles of quantitative scanning electron microscopy/energy dispersive x-ray spectrometry (SEM/EDS)

    NASA Astrophysics Data System (ADS)

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

    2012-06-01

    Scanning electron microscopy with energy dispersive x-ray spectrometry (SEM/EDS) is a powerful and flexible elemental analysis method that can identify and quantify elements with atomic numbers > 4 (Be) present as major constituents (where the concentration C > 0.1 mass fraction, or 10 weight percent), minor (0.01<= C <= 0.1) and trace (C < 0.01, with a minimum detectable limit of ~+/- 0.0005 - 0.001 under routine measurement conditions, a level which is analyte and matrix dependent ). SEM/EDS can select specimen volumes with linear dimensions from ~ 500 nm to 5 μm depending on composition (masses ranging from ~ 10 pg to 100 pg) and can provide compositional maps that depict lateral elemental distributions. Despite the maturity of SEM/EDS, which has a history of more than 40 years, and the sophistication of modern analytical software, the method is vulnerable to serious shortcomings that can lead to incorrect elemental identifications and quantification errors that significantly exceed reasonable expectations. This paper will describe shortcomings in peak identification procedures, limitations on the accuracy of quantitative analysis due to specimen topography or failures in physical models for matrix corrections, and quantitative artifacts encountered in xray elemental mapping. Effective solutions to these problems are based on understanding the causes and then establishing appropriate measurement science protocols. NIST DTSA II and Lispix are open source analytical software available free at www.nist.gov that can aid the analyst in overcoming significant limitations to SEM/EDS.

  1. Mechanical design and performance evaluation for plane grating monochromator in a soft X-ray microscopy beamline at SSRF.

    PubMed

    Gong, Xuepeng; Lu, Qipeng

    2015-01-01

    A new monochromator is designed to develop a high performance soft X-ray microscopy beamline at Shanghai Synchrotron Radiation Facility (SSRF). But owing to its high resolving power and high accurate spectrum output, there exist many technical difficulties. In the paper presented, as two primary design targets for the monochromator, theoretical energy resolution and photon flux of the beamline are calculated. For wavelength scanning mechanism, primary factors affecting the rotary angle errors are presented, and the measuring results are 0.15'' and 0.17'' for plane mirror and plane grating, which means that it is possible to provide sufficient scanning precision to specific wavelength. For plane grating switching mechanism, the repeatabilities of roll, yaw and pitch angles are 0.08'', 0.12'' and 0.05'', which can guarantee the high accurate switch of the plane grating effectively. After debugging, the repeatability of light spot drift reaches to 0.7'', which further improves the performance of the monochromator. The commissioning results show that the energy resolving power is higher than 10000 at Ar L-edge, the photon flux is higher than 1 × 108 photons/sec/200 mA, and the spatial resolution is better than 30 nm, demonstrating that the monochromator performs very well and reaches theoretical predictions. PMID:26410653

  2. Local structure of titania decorated double-walled carbon nanotube characterized by scanning transmission X-ray microscopy.

    PubMed

    Zhang, Hongbo; Wang, Jian; Pan, Xiulian; Hu, Yongfeng; Bao, Xinhe

    2012-05-01

    Scanning transmission X-ray microscopy was demonstrated to deliver detailed local structure and chemical composition of a complicated system with titania nanoparticles dispersed inside and outside the double-walled carbon nanotube (DWNT) channels. Areas with inhomogeneous distribution of titania and the associated water were particularly investigated at the C K-edge, Ti L-edge, and O K-edge. The results show that titania nanoparticles located inside DWNTs are present as amorphous, while those unsuccessfully introduced into the channels behave more like bulk materials in forms of anatase and rutile. Strong interaction was detected between the confined titania and DWNTs, as evidenced by up to 0.6 eV energy shift at the Ti L-edge. Strong hydration was observed for the as-prepared samples. Functionalization due to reduction and oxidation between titania and carbon layer is observed upon heat-treatment. This detailed structural information of specific areas cannot be provided by other techniques such as HRTEM, XRD, and XANES.

  3. Spatial Distributions of Discharged Products of Lithium-Oxygen Batteries Revealed by Synchrotron X-ray Transmission Microscopy.

    PubMed

    Olivares-Marín, Mara; Sorrentino, Andrea; Lee, Rung-Chuan; Pereiro, Eva; Wu, Nae-Lih; Tonti, Dino

    2015-10-14

    The discharge products of ether-based Li-O2 cells were grown directly on common carbon-coated TEM grids and observed by oxidation-state-sensitive full field transmission soft X-ray microscopy (TXM). The acquired data have permitted to quantify and localize with spatial resolution the distribution of the oxygen discharge products in these samples (i.e., lithium superoxide, peroxide, and carbonates) and appreciate several compositional, structural, and morphological aspects. Most of the peroxide particles had a toroidal shape, often with a central hole usually open on only one side, and which included significant amounts of superoxide-like phases (LiO2/Li2O2 ratio between 0.2 and 0.5). Smaller particles had smaller or no superoxide content, from which we infer that abundance of soluble LiO2 may have a role in toroid formation. Significant amount of carbonates were found irregularly distributed on the electrode surface, occasionally appearing as small particles and aggregates, and mostly coating lithium peroxide particles. This suggests the formation of a barrier that, similar to the solid electrolyte interface (SEI) critical in Li-ion batteries, requires an appropriate management for a reversible operation.

  4. Triosmium clusters on a support: determination of structure by X-ray absorption spectroscopy and high-resolution microscopy.

    PubMed

    Mehraeen, Shareghe; Kulkarni, Apoorva; Chi, Miaofang; Reed, Bryan W; Okamoto, Norihiko L; Browning, Nigel D; Gates, Bruce C

    2011-01-17

    The structures of small, robust metal clusters on a solid support were determined by a combination of spectroscopic and microscopic methods: extended X-ray absorption fine structure (EXAFS) spectroscopy, scanning transmission electron microscopy (STEM), and aberration-corrected STEM. The samples were synthesized from [Os(3) (CO)(12) ] on MgO powder to provide supported clusters intended to be triosmium. The results demonstrate that the supported clusters are robust in the absence of oxidants. Conventional high-angle annular dark-field (HAADF) STEM images demonstrate a high degree of uniformity of the clusters, with root-mean-square (rms) radii of 2.03±0.06 Å. The EXAFS OsOs coordination number of 2.1±0.4 confirms the presence of triosmium clusters on average and correspondingly determines an average rms cluster radius of 2.02±0.04 Å. The high-resolution STEM images show the individual Os atoms in the clusters, confirming the triangular structures of their frames and determining OsOs distances of 2.80±0.14 Å, matching the EXAFS value of 2.89±0.06 Å. IR and EXAFS spectra demonstrate the presence of CO ligands on the clusters. This set of techniques is recommended as optimal for detailed and reliable structural characterization of supported clusters. PMID:21226118

  5. Triosmium Clusters on a Support: Determination of Structure by X-Ray Absorption Spectroscopy and High-Resolution Microscopy

    SciTech Connect

    Shareghe, Mehraeen; Chi, Miaofang; Browning, Nigel D.

    2011-01-01

    The structures of small, robust metal clusters on a solid support were determined by a combination of spectroscopic and microscopic methods: extended X-ray absorption fine structure (EXAFS) spectroscopy, scanning transmission electron microscopy (STEM), and aberration-corrected STEM. The samples were synthesized from [Os{sub 3}(CO){sub 12}] on MgO powder to provide supported clusters intended to be triosmium. The results demonstrate that the supported clusters are robust in the absence of oxidants. Conventional high-angle annular dark-field (HAADF) STEM images demonstrate a high degree of uniformity of the clusters, with root-mean-square (rms) radii of 2.03 {+-} 0.06 {angstrom}. The EXAFS OsOs coordination number of 2.1 {+-} 0.4 confirms the presence of triosmium clusters on average and correspondingly determines an average rms cluster radius of 2.02 {+-} 0.04 {angstrom}. The high-resolution STEM images show the individual Os atoms in the clusters, confirming the triangular structures of their frames and determining OsOs distances of 2.80 {+-} 0.14 {angstrom}, matching the EXAFS value of 2.89 {+-} 0.06 {angstrom}. IR and EXAFS spectra demonstrate the presence of CO ligands on the clusters. This set of techniques is recommended as optimal for detailed and reliable structural characterization of supported clusters.

  6. Charge state mapping of mixed valent iron and manganese mineral particles using Scanning Transmission X-ray Microscopy (STXM)

    NASA Astrophysics Data System (ADS)

    Pecher, K.; Kneedler, E.; Rothe, J.; Meigs, G.; Warwick, T.; Nealson, K.; Tonner, B.

    2000-05-01

    The interfaces between solid mineral particles and water play a crucial role in partitioning and chemical transformation of many inorganic as well as organic pollutants in environmental systems. Among environmentally significant minerals, mixed-valent oxides and hydroxides of iron (e.g. magnetite, green rusts) and manganese (hausmanite, birnessite) have been recognized as particularly strong sorbents for metal ions. In addition, minerals containing Fe(II) have recently been proven to be powerful reductants for a wide range of pollutants. Chemical properties of these minerals strongly depend on the distribution and availability of reactive sites and little is known quantitatively about the nature of these sites. We have investigated the bulk distribution of charge states of manganese (Mn (II, III, IV)) and iron (Fe(II, III)) in single particles of natural manganese nodules and synthetic green rusts using Scanning Transmission X-ray SpectroMicroscopy (STXM). Pixel resolved spectra (XANES) extracted from stacks of images taken at different wave lengths across the metal absorption edge were fitted to total electron yield (TEY) spectra of single valent reference compounds. Two dimensional maps of bulk charge state distributions clearly reveal domains of different oxidation states within single particles of Mn-nodules and green rust precipitates. Changes of oxidation states of iron were followed as a result of reductive transformation of an environmental contaminant (CCl4) using green rust as the only reductant.

  7. Internal soft-tissue anatomy of Cambrian 'Orsten' arthropods as revealed by synchrotron X-ray tomographic microscopy.

    PubMed

    Eriksson, Mats E; Terfelt, Fredrik; Elofsson, Rolf; Marone, Federica

    2012-01-01

    The world-famous 'Orsten' Konservat-Lagerstätte has yielded detailed information about Cambrian arthropods and their morphology. Internal organs or soft tissues have, however, rarely been reported, an obvious palaeobiological drawback. In this study, we employed synchrotron radiation X-ray tomographic microscopy (SRXTM) to study microscopic 'Orsten' arthropods from the Cambrian of Sweden: Skara minuta and two phosphatocopine species, Hesslandona sp. and Hesslandona trituberculata. This exceptionally high-resolution technique reveals internal organs or soft tissues that allow detailed comparison with equivalent structures in extant crustaceans and functional inferences to be made. The S. minuta specimen shows the digestive system and muscles that extend to the extremities. The slanting anterior portion of the head and anterior position of the mouth with a straight oesophagus suggest a primarily brushing and scraping way of feeding. The prominent head appendage muscles indicate muscle strength and good capacity for food manipulation. In the phosphatocopines the bulbous labrum is one of the most prominent morphological structures of the body. All specimens analysed reveal pairs of muscle bundles within the labrum. Based on comparisons with extant crustacean relatives, these muscles would fulfil the function of moving the labrum up and down in order to open the buccal cavity. The results of this pilot study demonstrate that there is still much to be learned about the 'Orsten' taxa.

  8. 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

    2009-04-01

    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.

  9. Interrogation of EGFR-Targeted Uptake of TiO2 Nanoconjugates by X-ray Fluorescence Microscopy

    NASA Astrophysics Data System (ADS)

    Yuan, Y.; Paunesku, T.; Arora, H.; Ward, J.; Vogt, S.; Woloschak, G.

    2011-09-01

    We are developing TiO2 nanoconjugates that can be used as therapeutic and diagnostic agents. Nanoscale TiO2 can be surface conjugated with various molecules and has the unique ability to induce the production of reactive oxygen species after radiation activation. One way to improve the potential clinical usefulness of TiO2 nanoparticles is to control their delivery to malignant cells by targeting them to cancer-cell-specific antigens. Epidermal growth factor receptor (EGFR) is one potential target that is enriched in epithelial cancers and is rapidly internalized after ligand binding. Hence, we have synthesized TiO2 nanoparticles and functionalized them with a short EGFR-binding peptide to create EGFR-targeted NCs. X-ray fluorescence microscopy was used to image nanoconjugates within EGFR-positive HeLa cells. Further labeling of fixed cells with antibodies against EGFR and Protein A nanogold showed that TiO2 nanoconjugates can colocalize with receptors at the cell's plasma membrane. Interestingly, with increased incubation times, EGFR-targeted nanoconjugates could also be found colocalized with EGFR within the cell nucleus. This suggests that EGFR-targeted nanoconjugates can bind the receptor at the cell membrane, which leads to the internalization of NC-receptor complexes and the subsequent transport of nanoconjugates into the nucleus.

  10. 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.

  11. Microscopy and X-ray spectroscopy analyses for assessment of gilding and silvering techniques of Portuguese illuminated manuscripts.

    PubMed

    Le Gac, Agnès; Nogueira, Isabel D; Guerra, Mauro; Frade, José Carlos; Longelin, Stéphane; Manso, Marta; Pessanha, Sofia; Seruya, Ana Isabel M; Carvalho, Maria Luisa

    2015-02-01

    The objects of this study are various local charters (cartas de foral, in Portuguese) granted by Dom Manuel I, King of Portugal (1495-1521), which substituted for medieval ones and were intended to achieve an administrative unification. These are luxuriously illuminated manuscripts, and our study aims at obtaining a better understanding of the gilding and silvering techniques applied to the parchments, in which the forais were written, between 1500 and 1520. The combined use of microscopy and X-ray spectroscopy analyses allowed us to identify the vestigial materials used for making the parchments, including products such as salt (NaCl), lime (CaO), pumice stone (SiO2+Al2O3), and chalk (CaCO3). Chalk was employed as a whitening agent to give the parchment its final color and opacity. Shell-gold and shell-silver mixed in with animal glue or gum binding media were directly applied on type 1 and 3 forais, while very thin gold leaves (<1 µm) were applied over lead-based tempera grounds (50-180 µm thick) in type 2 forais. Silver was always employed in its finest form without a further protective layer (thus its recursive state of corrosion), while gold was used in various alloy grades.

  12. Evolution and Function of Dinosaur Teeth at Ultramicrostructural Level Revealed Using Synchrotron Transmission X-ray Microscopy

    PubMed Central

    Wang, Chun-Chieh; Song, Yen-Fang; Song, Sheng-Rong; Ji, Qiang; Chiang, Cheng-Cheng; Meng, Qingjin; Li, Haibing; Hsiao, Kiko; Lu, Yi-Chia; Shew, Bor-Yuan; Huang, Timothy; Reisz, Robert R.

    2015-01-01

    The relationship between tooth form and dietary preference is a crucial issue in vertebrate evolution. However, the mechanical properties of a tooth are influenced not only by its shape but also by its internal structure. Here, we use synchrotron transmission X-ray microscopy to examine the internal microstructures of multiple dinosaur teeth within a phylogenetic framework. We found that the internal microstructures of saurischian teeth are very different from advanced ornithischian teeth, reflecting differences in dental developmental strategies. The three-tissue composition (enamel–mantle dentin–bulk dentin) near the dentinoenamel junction (DEJ) in saurischian teeth represents the primitive condition of dinosaur teeth. Mantle dentin, greatly reduced or absent from DEJ in derived ornithischian teeth, is a key difference between Saurischia and Ornithischia. This may be related to the derived herbivorous feeding behavior of ornithischians, but interestingly, it is still retained in the herbivorous saurischian sauropods. The protective functions of mantle dentin with porous microstructures between enamel and bulk dentin inside typical saurischian teeth are also discussed using finite-element analysis method. Evolution of the dental modifications in ornithischian dinosaurs, with the absence of mantle dentin, may be related to changes in enamel characteristics with enamel spindles extending through the DEJ. PMID:26512629

  13. Humidity-controlled preparation of frozen-hydrated biological samples for cryogenic coherent x-ray diffraction microscopy.

    PubMed

    Takayama, Yuki; Nakasako, Masayoshi

    2012-05-01

    Coherent x-ray diffraction microscopy (CXDM) has the potential to visualize the structures of micro- to sub-micrometer-sized biological particles, such as cells and organelles, at high resolution. Toward advancing structural studies on the functional states of such particles, here, we developed a system for the preparation of frozen-hydrated biological samples for cryogenic CXDM experiments. The system, which comprised a moist air generator, microscope, micro-injector mounted on a micromanipulator, custom-made sample preparation chamber, and flash-cooling device, allowed for the manipulation of sample particles in the relative humidity range of 20%-94%rh at 293 K to maintain their hydrated and functional states. Here, we report the details of the system and the operation procedure, including its application to the preparation of a frozen-hydrated chloroplast sample. Sample quality was evaluated through a cryogenic CXDM experiment conducted at BL29XUL of SPring-8. Taking the performance of the system and the quality of the sample, the system was suitable to prepare frozen-hydrated biological samples for cryogenic CXDM experiments.

  14. Humidity-controlled preparation of frozen-hydrated biological samples for cryogenic coherent x-ray diffraction microscopy

    SciTech Connect

    Takayama, Yuki; Nakasako, Masayoshi

    2012-05-15

    Coherent x-ray diffraction microscopy (CXDM) has the potential to visualize the structures of micro- to sub-micrometer-sized biological particles, such as cells and organelles, at high resolution. Toward advancing structural studies on the functional states of such particles, here, we developed a system for the preparation of frozen-hydrated biological samples for cryogenic CXDM experiments. The system, which comprised a moist air generator, microscope, micro-injector mounted on a micromanipulator, custom-made sample preparation chamber, and flash-cooling device, allowed for the manipulation of sample particles in the relative humidity range of 20%-94%rh at 293 K to maintain their hydrated and functional states. Here, we report the details of the system and the operation procedure, including its application to the preparation of a frozen-hydrated chloroplast sample. Sample quality was evaluated through a cryogenic CXDM experiment conducted at BL29XUL of SPring-8. Taking the performance of the system and the quality of the sample, the system was suitable to prepare frozen-hydrated biological samples for cryogenic CXDM experiments.

  15. Evolution and Function of Dinosaur Teeth at Ultramicrostructural Level Revealed Using Synchrotron Transmission X-ray Microscopy.

    PubMed

    Wang, Chun-Chieh; Song, Yen-Fang; Song, Sheng-Rong; Ji, Qiang; Chiang, Cheng-Cheng; Meng, Qingjin; Li, Haibing; Hsiao, Kiko; Lu, Yi-Chia; Shew, Bor-Yuan; Huang, Timothy; Reisz, Robert R

    2015-10-29

    The relationship between tooth form and dietary preference is a crucial issue in vertebrate evolution. However, the mechanical properties of a tooth are influenced not only by its shape but also by its internal structure. Here, we use synchrotron transmission X-ray microscopy to examine the internal microstructures of multiple dinosaur teeth within a phylogenetic framework. We found that the internal microstructures of saurischian teeth are very different from advanced ornithischian teeth, reflecting differences in dental developmental strategies. The three-tissue composition (enamel-mantle dentin-bulk dentin) near the dentinoenamel junction (DEJ) in saurischian teeth represents the primitive condition of dinosaur teeth. Mantle dentin, greatly reduced or absent from DEJ in derived ornithischian teeth, is a key difference between Saurischia and Ornithischia. This may be related to the derived herbivorous feeding behavior of ornithischians, but interestingly, it is still retained in the herbivorous saurischian sauropods. The protective functions of mantle dentin with porous microstructures between enamel and bulk dentin inside typical saurischian teeth are also discussed using finite-element analysis method. Evolution of the dental modifications in ornithischian dinosaurs, with the absence of mantle dentin, may be related to changes in enamel characteristics with enamel spindles extending through the DEJ.

  16. Microscopy and X-ray spectroscopy analyses for assessment of gilding and silvering techniques of Portuguese illuminated manuscripts.

    PubMed

    Le Gac, Agnès; Nogueira, Isabel D; Guerra, Mauro; Frade, José Carlos; Longelin, Stéphane; Manso, Marta; Pessanha, Sofia; Seruya, Ana Isabel M; Carvalho, Maria Luisa

    2015-02-01

    The objects of this study are various local charters (cartas de foral, in Portuguese) granted by Dom Manuel I, King of Portugal (1495-1521), which substituted for medieval ones and were intended to achieve an administrative unification. These are luxuriously illuminated manuscripts, and our study aims at obtaining a better understanding of the gilding and silvering techniques applied to the parchments, in which the forais were written, between 1500 and 1520. The combined use of microscopy and X-ray spectroscopy analyses allowed us to identify the vestigial materials used for making the parchments, including products such as salt (NaCl), lime (CaO), pumice stone (SiO2+Al2O3), and chalk (CaCO3). Chalk was employed as a whitening agent to give the parchment its final color and opacity. Shell-gold and shell-silver mixed in with animal glue or gum binding media were directly applied on type 1 and 3 forais, while very thin gold leaves (<1 µm) were applied over lead-based tempera grounds (50-180 µm thick) in type 2 forais. Silver was always employed in its finest form without a further protective layer (thus its recursive state of corrosion), while gold was used in various alloy grades. PMID:25591998

  17. Spatial Distributions of Discharged Products of Lithium-Oxygen Batteries Revealed by Synchrotron X-ray Transmission Microscopy.

    PubMed

    Olivares-Marín, Mara; Sorrentino, Andrea; Lee, Rung-Chuan; Pereiro, Eva; Wu, Nae-Lih; Tonti, Dino

    2015-10-14

    The discharge products of ether-based Li-O2 cells were grown directly on common carbon-coated TEM grids and observed by oxidation-state-sensitive full field transmission soft X-ray microscopy (TXM). The acquired data have permitted to quantify and localize with spatial resolution the distribution of the oxygen discharge products in these samples (i.e., lithium superoxide, peroxide, and carbonates) and appreciate several compositional, structural, and morphological aspects. Most of the peroxide particles had a toroidal shape, often with a central hole usually open on only one side, and which included significant amounts of superoxide-like phases (LiO2/Li2O2 ratio between 0.2 and 0.5). Smaller particles had smaller or no superoxide content, from which we infer that abundance of soluble LiO2 may have a role in toroid formation. Significant amount of carbonates were found irregularly distributed on the electrode surface, occasionally appearing as small particles and aggregates, and mostly coating lithium peroxide particles. This suggests the formation of a barrier that, similar to the solid electrolyte interface (SEI) critical in Li-ion batteries, requires an appropriate management for a reversible operation. PMID:26339872

  18. Mechanical design and performance evaluation for plane grating monochromator in a soft X-ray microscopy beamline at SSRF.

    PubMed

    Gong, Xuepeng; Lu, Qipeng

    2015-01-01

    A new monochromator is designed to develop a high performance soft X-ray microscopy beamline at Shanghai Synchrotron Radiation Facility (SSRF). But owing to its high resolving power and high accurate spectrum output, there exist many technical difficulties. In the paper presented, as two primary design targets for the monochromator, theoretical energy resolution and photon flux of the beamline are calculated. For wavelength scanning mechanism, primary factors affecting the rotary angle errors are presented, and the measuring results are 0.15'' and 0.17'' for plane mirror and plane grating, which means that it is possible to provide sufficient scanning precision to specific wavelength. For plane grating switching mechanism, the repeatabilities of roll, yaw and pitch angles are 0.08'', 0.12'' and 0.05'', which can guarantee the high accurate switch of the plane grating effectively. After debugging, the repeatability of light spot drift reaches to 0.7'', which further improves the performance of the monochromator. The commissioning results show that the energy resolving power is higher than 10000 at Ar L-edge, the photon flux is higher than 1 × 108 photons/sec/200 mA, and the spatial resolution is better than 30 nm, demonstrating that the monochromator performs very well and reaches theoretical predictions.

  19. Analysis of ER–mitochondria contacts using correlative fluorescence microscopy and soft X-ray tomography of mammalian cells

    PubMed Central

    Elgass, Kirstin D.; Smith, Elizabeth A.; LeGros, Mark A.; Larabell, Carolyn A.; Ryan, Michael T.

    2015-01-01

    ABSTRACT Mitochondrial fission is important for organelle transport, quality control and apoptosis. Changes to the fission process can result in a wide variety of neurological diseases. In mammals, mitochondrial fission is executed by the GTPase dynamin-related protein 1 (Drp1; encoded by DNM1L), which oligomerizes around mitochondria and constricts the organelle. The mitochondrial outer membrane proteins Mff, MiD49 (encoded by MIEF2) and MiD51 (encoded by MIEF1) are involved in mitochondrial fission by recruiting Drp1 from the cytosol to the organelle surface. In addition, endoplasmic reticulum (ER) tubules have been shown to wrap around and constrict mitochondria before a fission event. Up to now, the presence of MiD49 and MiD51 at ER–mitochondrial division foci has not been established. Here, we combine confocal live-cell imaging with correlative cryogenic fluorescence microscopy and soft x-ray tomography to link MiD49 and MiD51 to the involvement of the ER in mitochondrial fission. We gain further insight into this complex process and characterize the 3D structure of ER–mitochondria contact sites. PMID:26101352

  20. Non-invasive airway health measurement using synchrotron x-ray microscopy of high refractive index glass microbeads

    NASA Astrophysics Data System (ADS)

    Donnelley, Martin; Morgan, Kaye; Farrow, Nigel; Siu, Karen; Parsons, David

    2016-01-01

    Cystic fibrosis (CF) is caused by a gene defect that compromises the ability of the mucociliary transit (MCT) system to clear the airways of debris and pathogens. To directly characterise airway health and the effects of treatments we have developed a synchrotron X-ray microscopy method that non-invasively measures the local rate and patterns of MCT behaviour. Although the nasal airways of CF mice exhibit the CF pathophysiology, there is evidence that nasal MCT is not altered in CF mice1. The aim of this experiment was to determine if our non-invasive local airway health assessment method could identify differences in nasal MCT rate between normal and CF mice, information that is potentially lost in bulk MCT measurements. Experiments were performed on the BL20XU beamline at the SPring-8 Synchrotron in Japan. Mice were anaesthetized, a small quantity of micron-sized marker particles were delivered to the nose, and images of the nasal airways were acquired for 15 minutes. The nasal airways were treated with hypertonic saline or mannitol to increase surface hydration and MCT. Custom software was used to locate and track particles and calculate individual and bulk MCT rates. No statistically significant differences in MCT rate were found between normal and CF mouse nasal airways or between treatments. However, we hope that the improved sensitivity provided by this technique will accelerate the ability to identify useful CF lung disease-modifying interventions in small animal models, and enhance the development and efficacy of proposed new therapies.

  1. Lifetime Estimation of a Time Projection Chamber X-ray Polarimeter

    NASA Technical Reports Server (NTRS)

    Hill, Joanne E.; Black, J. Kevin; Brieda, Lubos; Dickens, Patsy L.; deGarcia, Kristina Montt; Hawk, Douglas L.; Hayato, Asami; Jahoda, Keith; Mohammed, Jelila

    2013-01-01

    The Gravity and Extreme Magnetism Small Explorer (GEMS) X-ray polarimeter Instrument (XPI) was designed to measure the polarization of 23 sources over the course of its 9 month mission. The XPI design consists of two telescopes each with a polarimeter assembly at the focus of a grazing incidence mirror. To make sensitive polarization measurements the GEMS Polarimeter Assembly (PA) employed a gas detection system based on a Time Projection Chamber (TPC) technique. Gas detectors are inherently at risk of degraded performance arising from contamination from outgassing of internal detector components or due to loss of gas. This paper describes the design and the materials used to build a prototype of the flight polarimeter with the required GEMS lifetime. We report the results from outgassing measurements of the polarimeter subassemblies and assemblies, enclosure seal tests, life tests, and performance tests that demonstrate that the GEMS lifetime is achievable. Finally we report performance measurements and the lifetime enhancement from the use of a getter.

  2. Scanning electron microscopy, X-ray diffraction and thermal analysis study of the TiH{sub 2} foaming agent

    SciTech Connect

    Mandrino, Djordje; Paulin, Irena; Skapin, Sreco D.

    2012-10-15

    The decomposition of commercially available TiH{sub 2} was investigated while performing different thermal treatments. TiH{sub 2} powder, which is widely used as a foaming agent, was heat treated at 450 Degree-Sign C for various times, from 15 min to 120 min. Scanning electron microscopy (SEM) images of the surfaces at different magnifications were obtained and interpreted. A Bragg-Brentano X-ray diffractometer was used to measure the X-ray diffraction (XRD) spectra on all five samples. A close examination of the diffraction spectra showed that for an as-received sample and samples undergoing the longest thermal treatment (1 and 2 h) these spectra can be explained as deriving from cubic TiH{sub 1.924}, while for the other two samples they can be explained as deriving from tetragonal TiH{sub 1.924}. A constant-unit-cell-volume phase transition between the cubic and tetragonal phases in TiH{sub 2-y}-type compounds had been described in the literature. The unit-cell parameters obtained from measured spectra confirm that within the measurement uncertainty the unit-cell volume is indeed constant in all five samples. Thermo-gravimetry (TG) and differential thermal analysis (DTA) measurements were performed on all the samples, showing that the intensity of the dehydrogenation depends on the previous treatment of the TiH{sub 2}. After the thermal analysis XRD of the samples was performed again and the material was found to exhibit a Ti-like unit cell, but slightly enlarged due to the unreleased hydrogen. - Highlights: Black-Right-Pointing-Pointer TiH{sub 2} samples were cubic or tetragonal TiH{sub 1.924} Black-Right-Pointing-Pointer Onset of the hydrogen release temperature increases with the pre-treatment time. Black-Right-Pointing-Pointer Thermal dehydrogenation for the as-prepared TiH{sub 2} is a three-step process. Black-Right-Pointing-Pointer After thermal analysis 2 residual hydrogen TiH{sub x} phases, close to {alpha}Ti, appeared.

  3. Application of Scanning-Imaging X-Ray Microscopy to Fluid Inclusion Candidates in Carbonates of Carbonaceous Chondrites

    NASA Technical Reports Server (NTRS)

    Tsuchiyama, Akira; Nakano, Tsukasa; Miyake, Akira; Akihisa, Takeuchi; Uesugi, Kentaro; Suzuki, Yoshio; Kitayama, Akira; Matsuno, Junya; Zolensky, Michael E.

    2016-01-01

    In order to search for such fluid inclusions in carbonaceous chondrites, a nondestructive technique using x-ray micro-absorption tomography combined with FIB sampling was developed and applied to a carbonaceous chondrite. They found fluid inclusion candidates in calcite grains, which were formed by aqueous alteration. However, they could not determine whether they are really aqueous fluids or merely voids. Phase and absorption contrast images can be simultaneously obtained in 3D by using scanning-imaging x-ray microscopy (SIXM). In refractive index, n=1-sigma+i(beta), in the real part, 1-sigma is the refractive index with decrement, sigma, which is nearly proportional to the density, and the imaginary part, beta, is the extinction coefficient, which is related to the liner attenuation coefficient, mu. Many phases, including water and organic materials as well as minerals, can be identified by SIXM, and this technique has potential availability for Hayabusa-2 sample analysis too. In this study, we examined quantitative performance of d and m values and the spatial resolution in SIXM by using standard materials, and applied this technique to carbonaceous chondrite samples. We used POM ([CH2O]n), silicon, quartz, forsterite, corundum, magnetite and nickel as standard materials for examining the sigma and mu values. A fluid inclusion in terrestrial quartz and bi-valve shell (Atrina vexillum), which are composed of calcite and organic layers with different thickness, were also used for examining the spatial resolution. The Ivuna (CI) and Sutter's Mill (CM) meteorites were used as carbonaceous chondrite samples. Rod- or cube-shaped samples 20-30 micron in size were extracted by using FIB from cross-sectional surfaces of the standard materials or polished thin sections of the chondrites, which was previously observed with SEM. Then, the sample was attached to a thin W-needle and imaged by SIXM system at beamline BL47XU, SPring-8, Japan. The slice thickness was 109.3 nm

  4. Transmission photoemission electron microscopy for lateral mapping of the X-ray absorption structure of a metalloprotein in a liquid cell.

    PubMed

    Panzer, D; Beck, C; Maul, J; Möller, M; Decker, H; Schönhense, G

    2008-11-01

    We use photoemission electron microscopy in an X-ray transmission mode for full-field imaging of the X-ray absorption structure of copper in the respiratory metalloprotein hemocyanin KLH1. It contains 160 oxygen binding sites. Each site reversibly binds one molecule oxygen between two copper atoms. In our setup, hemocyanin is dissolved in aqueous solution and enclosed in an ultra-high vacuum compatible liquid sample cell with silicon nitride membranes. The local X-ray absorption structure of the liquid sample is converted into photoelectrons at the microscope side of the cell acting as a photocathode. In this way, different copper valencies are laterally distinguished under in vivo-like conditions, attributed to Cu(I) in the deoxy-state and Cu(II) in the oxy-state.

  5. Achromatic and high-resolution full-field X-ray microscopy based on total-reflection mirrors.

    PubMed

    Matsuyama, Satoshi; Emi, Yoji; Kino, Hidetoshi; Kohmura, Yoshiki; Yabashi, Makina; Ishikawa, Tetsuya; Yamauchi, Kazuto

    2015-04-20

    We developed an achromatic and high-resolution full-field X-ray microscope based on advanced Kirkpatrick-Baez mirror optics that comprises two pairs of elliptical mirrors and hyperbolic mirrors utilizing the total reflection of X-rays. Performance tests to investigate the spatial resolution and chromatic aberration were performed at SPring-8. The microscope clearly resolved the pattern with ~100-nm feature size. Imaging the pattern by changing the X-ray energy revealed achromatism in the wide energy range of 8-11 keV.

  6. Error analysis of the x-ray projection geometry of camera-augmented mobile C-arm

    NASA Astrophysics Data System (ADS)

    Chen, Xin; Wang, Lejing; Fallavollita, Pascal; Navab, Nassir

    2012-02-01

    The Camera-Augmented Mobile C-arm (CamC) augments X-ray by optical camera images and is used as an advanced visualization and guidance tool in trauma and orthopedic surgery. However, in its current form the calibration is suboptimal. We investigated and compared calibration and distortion correction between: (i) the existing CamC calibration framework (ii) Zhang's calibration for video images, and (iii) the traditional C-arm fluoroscopy calibration technique. Accuracy of the distortion correction for each of the three methods is compared by analyzing the error based on a synthetic model and the linearity and cross-ratio properties. Also, the accuracy of calibrated X-ray projection geometry is evaluated by performing C-arm pose estimation using a planar pattern with known geometry. The RMS errors based on a synthetic model and pose estimation shows that the traditional C-arm method (μ=0.39 pixels) outperforms both Zhang (μ=0.68 pixels) and original CamC (μ=1.07 pixels) methods. The relative pose estimation comparison shows that the translation error of the traditional method (μ=0.25mm) outperforms Zhang (μ=0.41mm) and CamC (μ=1.13mm) method. In conclusion, we demonstrated that the traditional X-ray calibration procedure outperforms the existing CamC solution and Zhang's method for the calibration of C-arm X-ray projection geometry.

  7. Comparison of different numerical treatments for x-ray phase tomography of soft tissue from differential phase projections

    NASA Astrophysics Data System (ADS)

    Pelliccia, Daniele; Vaz, Raquel; Svalbe, Imants; Morgan, Kaye S.; Marathe, Shashidhara; Xiao, Xianghui; Assoufid, Lahsen; Anderson, Rebecca A.; Topczewski, Jacek; Bryson-Richardson, Robert J.

    2015-04-01

    X-ray imaging of soft tissue is made difficult by their low absorbance. The use of x-ray phase imaging and tomography can significantly enhance the detection of these tissues and several approaches have been proposed to this end. Methods such as analyzer-based imaging or grating interferometry produce differential phase projections that can be used to reconstruct the 3D distribution of the sample refractive index. We report on the quantitative comparison of three different methods to obtain x-ray phase tomography with filtered back-projection from differential phase projections in the presence of noise. The three procedures represent different numerical approaches to solve the same mathematical problem, namely phase retrieval and filtered back-projection. It is found that obtaining individual phase projections and subsequently applying a conventional filtered back-projection algorithm produces the best results for noisy experimental data, when compared with other procedures based on the Hilbert transform. The algorithms are tested on simulated phantom data with added noise and the predictions are confirmed by experimental data acquired using a grating interferometer. The experiment is performed on unstained adult zebrafish, an important model organism for biomedical studies. The method optimization described here allows resolution of weak soft tissue features, such as muscle fibers.

  8. Monitoring X-Ray Emission from X-Ray Bursters

    NASA Technical Reports Server (NTRS)

    Halpern, Jules P.; Kaaret, Philip

    1999-01-01

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

  9. Visualization of the effects of electron microscopy fixatives on the structure of hydrated epidermal hairs of tomato (lycopersicum peruvianum) as revealed by soft x-ray contact microscopy

    NASA Astrophysics Data System (ADS)

    Stead, Anthony D.; Cotton, Robin A.; Page, Anton M.; Dooley, Mike D.; Ford, Thomas W.

    1993-01-01

    In order to examine the ultrastructure of biological specimens by electron microscopy it is necessary to stabilize the highly labile cellular contents before embedding and sectioning the specimens. This is commonly achieved by treating the tissues with various chemical fixatives. The assessment of the efficacy of these fixative is usually based upon the appearance of the specimen under the microscope although this is somewhat intuitive as the ultrastructure of the living cell cannot be studied. Previous studies, in which the structure of epidermal hairs has been followed under the light microscope as the commonly used fixatives are perfused into the tissue, have shown that the cellular contents are drastically rearranged by these fixatives. This paper describes the effects of some of the commonly used fixatives on cell ultrastructure using firstly electron microscopy and secondly soft x-ray contact microscopy. The latter technique allows not only direct comparisons of the effects of the fixatives but also allows living, hydrated specimens to be imaged so that the true ultrastructural effects of the fixatives can be seen and compared to the ultrastructure of the living material.

  10. Carbon corrosion of proton exchange membrane fuel cell catalyst layers studied by scanning transmission X-ray microscopy

    NASA Astrophysics Data System (ADS)

    Hitchcock, Adam P.; Berejnov, Viatcheslav; Lee, Vincent; West, Marcia; Colbow, Vesna; Dutta, Monica; Wessel, Silvia

    2014-11-01

    Scanning Transmission X-ray Microscopy (STXM) at the C 1s, F 1s and S 2p edges has been used to investigate degradation of proton exchange membrane fuel cell (PEM-FC) membrane electrode assemblies (MEA) subjected to accelerated testing protocols. Quantitative chemical maps of the catalyst, carbon support and ionomer in the cathode layer are reported for beginning-of-test (BOT), and end-of-test (EOT) samples for two types of carbon support, low surface area carbon (LSAC) and medium surface area carbon (MSAC), that were exposed to accelerated stress testing with upper potentials (UPL) of 1.0, 1.2, and 1.3 V. The results are compared in order to characterize catalyst layer degradation in terms of the amounts and spatial distributions of these species. Pt agglomeration, Pt migration and corrosion of the carbon support are all visualized, and contribute to differing degrees in these samples. It is found that there is formation of a distinct Pt-in-membrane (PTIM) band for all EOT samples. The cathode thickness shrinks due to loss of the carbon support for all MSAC samples that were exposed to the different upper potentials, but only for the most aggressive testing protocol for the LSAC support. The amount of ionomer per unit volume significantly increases indicating it is being concentrated in the cathode as the carbon corrosion takes place. S 2p spectra and mapping of the cathode catalyst layer indicates there are still sulfonate groups present, even in the most damaged material.

  11. In situ X-ray tomographic microscopy observations of vesiculation of bubble-free and bubble-bearing magmas

    NASA Astrophysics Data System (ADS)

    Pistone, Mattia; Caricchi, Luca; Fife, Julie L.; Mader, Kevin; Ulmer, Peter

    2015-12-01

    Magma degassing is thought to play a major role in magma fractionation, transport, storage, and volcanic eruption dynamics. However, the conditions that determine when and how magma degassing operates prior to and during an eruption remain poorly constrained. We performed experiments to explore if the initial presence of gas bubbles in magma influences the capability of gas to escape from the magma. Vesiculation of natural H2O-poor (<<1 wt.%) silicic obsidian glasses was investigated by in situ, high-temperature (above the glass transition) experiments using synchrotron-based X-ray tomographic microscopy with high spatial (3 μm/pixel) and temporal resolution (1 second per 3D dataset). As a validation, a second set of experiments was performed on identical starting materials using a Karl-Fisher titration setup to quantify the amount of extracted gas that escapes via volatile diffusion and/or bubble coalescence during vesiculation. In both sets of experiments, vesiculation was triggered by heating the samples at room pressure. Our results suggest that the presence of pre-existing gas bubbles during a nucleation event significantly decreases the tendency of bubbles to coalesce and inhibits magma outgassing. In contrast, in initially bubble-free samples, the nucleation and growth of bubbles is accompanied by significant coalescence and outgassing. We infer that volatile-undersaturated (i.e. bubble-free) magmas in the reservoirs are more likely to erupt effusively, while the presence of excess gas already at depth (i.e. bubble-bearing systems) increases the likelihood of explosive eruptions.

  12. Atomic level study of water-gas shift catalysts via transmission electron microscopy and x-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Akatay, Mehmed Cem

    Water-gas shift (WGS), CO + H2O ⇆ CO2 + H2 (DeltaH° = -41 kJ mol -1), is an industrially important reaction for the production of high purity hydrogen. Commercial Cu/ZnO/Al2O3 catalysts are employed to accelerate this reaction, yet these catalysts suffer from certain drawbacks, including costly regeneration processes and sulfur poisoning. Extensive research is focused on developing new catalysts to replace the current technology. Supported noble metals stand out as promising candidates, yet comprise intricate nanostructures complicating the understanding of their working mechanism. In this study, the structure of the supported Pt catalysts is explored by transmission electron microscopy and X-ray spectroscopy. The effect of the supporting phase and the use of secondary metals on the reaction kinetics is investigated. Structural heterogeneities are quantified and correlated with the kinetic descriptors of the catalysts to develop a fundamental understanding of the catalytic mechanism. The effect of the reaction environment on catalyst structure is examined by in-situ techniques. This study benefitted greatly from the use of model catalysts that provide a convenient medium for the atomic level characterization of nanostructures. Based on these studies, Pt supported on iron oxide nano islands deposited on inert spherical alumina exhibited 48 times higher WGS turnover rate (normalized by the total Pt surface area) than Pt supported on bulk iron oxide. The rate of aqueous phase glycerol reforming reaction of Pt supported on multiwall carbon nanotubes (MWCNT) is promoted by co-impregnating with cobalt. The synthesis resulted in a variety of nanostructures among which Pt-Co bimetallic nanoparticles are found to be responsible for the observed promotion. The unprecedented WGS rate of Pt supported on Mo2C is explored by forming Mo 2C patches on top of MWCNTs and the rate promotion is found to be caused by the Pt-Mo bimetallic entities.

  13. Thin-film-based scintillators for hard x-ray microimaging detectors: the ScinTAX Project

    NASA Astrophysics Data System (ADS)

    Rack, A.; Cecilia, A.; Douissard, P.-A.; Dupré, K.; Wesemann, V.; Baumbach, T.; Couchaud, M.; Rochet, X.; Riesemeier, H.; Radtke, M.; Martin, T.

    2014-09-01

    The project ScinTAX developed novel thin scintillating films for the application in high performance X-ray imaging and subsequent introduced new X-ray detectors to the market. To achieve this aim lutetium orthosilicate (LSO) scintillators doped with different activators were grown successfully by liquid phase epitaxy. The high density of LSO (7.4 g/cm3), the effective atomic number (65.2) and the high light yield make this scintillator highly applicable for indirect X-ray detection in which the ionizing radiation is converted into visible light and then registered by a digital detector. A modular indirect detection system has been developed to fully exploit the potential of this thin film scintillator for radiographic and tomographic imaging. The system is compatible for high-resolution imaging with moderate dose as well as adaptable to intense high-dose applications where radiation hard microimaging detectors are required. This proceedings article shall review the achieved performances and technical details on this high-resolution detector system which is now available. A selected example application demonstrates the great potential of the optimized detector system for hard X-ray microimaging, i.e. either to improve image contrast due to the availability of efficient thin crystal films or to reduce the dose to the sample.

  14. Spatial frequency spectrum of the x-ray scatter distribution in CBCT projections

    SciTech Connect

    Bootsma, G. J.; Verhaegen, F.; Jaffray, D. A.

    2013-11-15

    Purpose: X-ray scatter is a source of significant image quality loss in cone-beam computed tomography (CBCT). The use of Monte Carlo (MC) simulations separating primary and scattered photons has allowed the structure and nature of the scatter distribution in CBCT to become better elucidated. This work seeks to quantify the structure and determine a suitable basis function for the scatter distribution by examining its spectral components using Fourier analysis.Methods: The scatter distribution projection data were simulated using a CBCT MC model based on the EGSnrc code. CBCT projection data, with separated primary and scatter signal, were generated for a 30.6 cm diameter water cylinder [single angle projection with varying axis-to-detector distance (ADD) and bowtie filters] and two anthropomorphic phantoms (head and pelvis, 360 projections sampled every 1°, with and without a compensator). The Fourier transform of the resulting scatter distributions was computed and analyzed both qualitatively and quantitatively. A novel metric called the scatter frequency width (SFW) is introduced to determine the scatter distribution's frequency content. The frequency content results are used to determine a set basis functions, consisting of low-frequency sine and cosine functions, to fit and denoise the scatter distribution generated from MC simulations using a reduced number of photons and projections. The signal recovery is implemented using Fourier filtering (low-pass Butterworth filter) and interpolation. Estimates of the scatter distribution are used to correct and reconstruct simulated projections.Results: The spatial and angular frequencies are contained within a maximum frequency of 0.1 cm{sup −1} and 7/(2π) rad{sup −1} for the imaging scenarios examined, with these values varying depending on the object and imaging setup (e.g., ADD and compensator). These data indicate spatial and angular sampling every 5 cm and π/7 rad (∼25°) can be used to properly capture

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

    NASA Astrophysics Data System (ADS)

    Klappenberger, Florian

    2014-02-01

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

  16. Effects of the environmental factors on the casein micelle structure studied by cryo transmission electron microscopy and small-angle x-ray scattering/ultrasmall-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Marchin, Stéphane; Putaux, Jean-Luc; Pignon, Frédéric; Léonil, Joëlle

    2007-01-01

    Casein micelles are colloidal protein-calcium-transport complexes whose structure has not been unequivocally elucidated. This study used small-angle x-ray scattering (SAXS) and ultrasmall angle x-ray scattering (USAXS) as well as cryo transmission electron microscopy (cryo-TEM) to provide fine structural details on their structure. Cryo-TEM observations of native casein micelles fractionated by differential centrifugation showed that colloidal calcium phosphate appeared as nanoclusters with a diameter of about 2.5nm. They were uniformly distributed in a homogeneous tangled web of caseins and were primarily responsible for the intensity distribution in the SAXS profiles at the highest q vectors corresponding to the internal structure of the casein micelles. A specific demineralization of casein micelles by decreasing the pH from 6.7 to 5.2 resulted in a reduced granular aspect of the micelles observed by cryo-TEM and the existence of a characteristic point of inflection in SAXS profiles. This supports the hypothesis that the smaller substructures detected by SAXS are colloidal calcium phosphate nanoclusters rather than putative submicelles.

  17. Technical Report on DOE project: X-ray physics of materials (proposal No.Z817)

    SciTech Connect

    Colella, Roberto; Durbin, Stephen

    2001-01-01

    The SRI-CAT was able to order the construction of the First Optics Enclosure, the second enclosure housing the monochromator and the first user station, and various motors, controllers, and electronics for the control of the hard x-ray beamline components.

  18. Tabletop coherent diffractive microscopy with soft x-ray illumination from high harmonic generation at 29 nm and 13.5 nm

    NASA Astrophysics Data System (ADS)

    Raymondson, Daisy Arrelle

    Soft x-ray microscopy allows imaging at higher resolution than is possible with optical wavelengths. At the same time, it allows imaging of the internal structure of thick samples that cannot be viewed with electron microscopy. Optics for the soft x-ray region of the spectrum are limited, but coherent diffractive imaging techniques use computerized image reconstruction in place of a lens to form high-resolution images with x-rays. This dissertation presents a practical soft x-ray diffractive microscope with sub-100 nm resolution using tabletop coherent soft x-rays at 13.5 nm and 29 nm [1]. This represents the first demonstration of tabletop coherent imaging with 13.5 nm from high harmonics. Images with holography and phase retrieval are shown, with near-diffraction-limited resolution down to 53 nm [2--4]. The first tabletop diffractive images of biological samples with 13.5 nm and 29 nm beams are also shown [5]. This thesis also presents work on the construction of a high-power, high-repetition-rate laser amplifier implementing carrier-envelope phase stabilization. CEP stabilization provides unprecedented levels of control over the full electric field of an ultrafast laser. The first stage of the amplifier was stabilized to 250 mrad CEP noise on 100s timescales. The route to stabilizing the full 10 kHz, 30 W amplifier is outlined. This laser will be used for future coherent diffractive imaging applications at using high harmonic generation at 13.5 nm and shorter wavelengths, and will also be used for time-resolved studies of molecular dissociation [6].

  19. Study of the crystallographic architecture of corals at the nanoscale by scanning transmission X-ray microscopy and transmission electron microscopy.

    PubMed

    Benzerara, Karim; Menguy, Nicolas; Obst, Martin; Stolarski, Jarosław; Mazur, Maciej; Tylisczak, Tolek; Brown, Gordon E; Meibom, Anders

    2011-07-01

    We have investigated the nanotexture and crystallographic orientation of aragonite in a coral skeleton using synchrotron-based scanning transmission X-ray microscopy (STXM) and transmission electron microscopy (TEM). Polarization-dependent STXM imaging at 40-nm spatial resolution was used to obtain an orientation map of the c-axis of aragonite on a focused ion beam milled ultrathin section of a Porites coral. This imaging showed that one of the basic units of coral skeletons, referred to as the center of calcification (COC), consists of a cluster of 100-nm aragonite globules crystallographically aligned over several micrometers with a fan-like distribution and with the properties of single crystals at the mesoscale. The remainder of the skeleton consists of aragonite single-crystal fibers in crystallographic continuity with the nanoglobules comprising the COC. Our observation provides information on the nm-scale processes that led to biomineral formation in this sample. Importantly, the present study illustrates how the methodology described here, which combines HRTEM and polarization-dependent synchrotron-based STXM imaging, offers an interesting new approach for investigating biomineralizing systems at the nm-scale.

  20. Study of the crystallographic architecture of corals at the nanoscale by scanning transmission X-ray microscopy and transmission electron microscopy.

    PubMed

    Benzerara, Karim; Menguy, Nicolas; Obst, Martin; Stolarski, Jarosław; Mazur, Maciej; Tylisczak, Tolek; Brown, Gordon E; Meibom, Anders

    2011-07-01

    We have investigated the nanotexture and crystallographic orientation of aragonite in a coral skeleton using synchrotron-based scanning transmission X-ray microscopy (STXM) and transmission electron microscopy (TEM). Polarization-dependent STXM imaging at 40-nm spatial resolution was used to obtain an orientation map of the c-axis of aragonite on a focused ion beam milled ultrathin section of a Porites coral. This imaging showed that one of the basic units of coral skeletons, referred to as the center of calcification (COC), consists of a cluster of 100-nm aragonite globules crystallographically aligned over several micrometers with a fan-like distribution and with the properties of single crystals at the mesoscale. The remainder of the skeleton consists of aragonite single-crystal fibers in crystallographic continuity with the nanoglobules comprising the COC. Our observation provides information on the nm-scale processes that led to biomineral formation in this sample. Importantly, the present study illustrates how the methodology described here, which combines HRTEM and polarization-dependent synchrotron-based STXM imaging, offers an interesting new approach for investigating biomineralizing systems at the nm-scale. PMID:21864767