Coherent soft X-ray diffraction imaging of coliphage PR772 at the Linac coherent light source

PubMed Central

Reddy, Hemanth K.N.; Yoon, Chun Hong; Aquila, Andrew; Awel, Salah; Ayyer, Kartik; Barty, Anton; Berntsen, Peter; Bielecki, Johan; Bobkov, Sergey; Bucher, Maximilian; Carini, Gabriella A.; Carron, Sebastian; Chapman, Henry; Daurer, Benedikt; DeMirci, Hasan; Ekeberg, Tomas; Fromme, Petra; Hajdu, Janos; Hanke, Max Felix; Hart, Philip; Hogue, Brenda G.; Hosseinizadeh, Ahmad; Kim, Yoonhee; Kirian, Richard A.; Kurta, Ruslan P.; Larsson, Daniel S.D.; Duane Loh, N.; Maia, Filipe R.N.C.; Mancuso, Adrian P.; Mühlig, Kerstin; Munke, Anna; Nam, Daewoong; Nettelblad, Carl; Ourmazd, Abbas; Rose, Max; Schwander, Peter; Seibert, Marvin; Sellberg, Jonas A.; Song, Changyong; Spence, John C.H.; Svenda, Martin; Van der Schot, Gijs; Vartanyants, Ivan A.; Williams, Garth J.; Xavier, P. Lourdu

2017-01-01

Single-particle diffraction from X-ray Free Electron Lasers offers the potential for molecular structure determination without the need for crystallization. In an effort to further develop the technique, we present a dataset of coherent soft X-ray diffraction images of Coliphage PR772 virus, collected at the Atomic Molecular Optics (AMO) beamline with pnCCD detectors in the LAMP instrument at the Linac Coherent Light Source. The diameter of PR772 ranges from 65–70 nm, which is considerably smaller than the previously reported ~600 nm diameter Mimivirus. This reflects continued progress in XFEL-based single-particle imaging towards the single molecular imaging regime. The data set contains significantly more single particle hits than collected in previous experiments, enabling the development of improved statistical analysis, reconstruction algorithms, and quantitative metrics to determine resolution and self-consistency. PMID:28654088

Coherent soft X-ray diffraction imaging of coliphage PR772 at the Linac coherent light source

DOE PAGES

Reddy, Hemanth K. N.; Yoon, Chun Hong; Aquila, Andrew; ...

2017-06-27

Single-particle diffraction from X-ray Free Electron Lasers offers the potential for molecular structure determination without the need for crystallization. In an effort to further develop the technique, we present a dataset of coherent soft X-ray diffraction images of Coliphage PR772 virus, collected at the Atomic Molecular Optics (AMO) beamline with pnCCD detectors in the LAMP instrument at the Linac Coherent Light Source. The diameter of PR772 ranges from 65–70 nm, which is considerably smaller than the previously reported ~600 nm diameter Mimivirus. This reflects continued progress in XFEL-based single-particle imaging towards the single molecular imaging regime. As a result, themore » data set contains significantly more single particle hits than collected in previous experiments, enabling the development of improved statistical analysis, reconstruction algorithms, and quantitative metrics to determine resolution and self-consistency.« less

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

Coherent soft X-ray diffraction imaging of coliphage PR772 at the Linac coherent light source.

PubMed

Reddy, Hemanth K N; Yoon, Chun Hong; Aquila, Andrew; Awel, Salah; Ayyer, Kartik; Barty, Anton; Berntsen, Peter; Bielecki, Johan; Bobkov, Sergey; Bucher, Maximilian; Carini, Gabriella A; Carron, Sebastian; Chapman, Henry; Daurer, Benedikt; DeMirci, Hasan; Ekeberg, Tomas; Fromme, Petra; Hajdu, Janos; Hanke, Max Felix; Hart, Philip; Hogue, Brenda G; Hosseinizadeh, Ahmad; Kim, Yoonhee; Kirian, Richard A; Kurta, Ruslan P; Larsson, Daniel S D; Duane Loh, N; Maia, Filipe R N C; Mancuso, Adrian P; Mühlig, Kerstin; Munke, Anna; Nam, Daewoong; Nettelblad, Carl; Ourmazd, Abbas; Rose, Max; Schwander, Peter; Seibert, Marvin; Sellberg, Jonas A; Song, Changyong; Spence, John C H; Svenda, Martin; Van der Schot, Gijs; Vartanyants, Ivan A; Williams, Garth J; Xavier, P Lourdu

2017-06-27

Single-particle diffraction from X-ray Free Electron Lasers offers the potential for molecular structure determination without the need for crystallization. In an effort to further develop the technique, we present a dataset of coherent soft X-ray diffraction images of Coliphage PR772 virus, collected at the Atomic Molecular Optics (AMO) beamline with pnCCD detectors in the LAMP instrument at the Linac Coherent Light Source. The diameter of PR772 ranges from 65-70 nm, which is considerably smaller than the previously reported ~600 nm diameter Mimivirus. This reflects continued progress in XFEL-based single-particle imaging towards the single molecular imaging regime. The data set contains significantly more single particle hits than collected in previous experiments, enabling the development of improved statistical analysis, reconstruction algorithms, and quantitative metrics to determine resolution and self-consistency.

Lensless Tomographic Imaging of Near Surface Structures of Frozen Hydrated Malaria-Infected Human Erythrocytes by Coherent X-Ray Diffraction Microscopy.

PubMed

Frank, Viktoria; Chushkin, Yuriy; Fröhlich, Benjamin; Abuillan, Wasim; Rieger, Harden; Becker, Alexandra S; Yamamoto, Akihisa; Rossetti, Fernanda F; Kaufmann, Stefan; Lanzer, Michael; Zontone, Federico; Tanaka, Motomu

2017-10-26

Lensless, coherent X-ray diffraction microscopy has been drawing considerable attentions for tomographic imaging of whole human cells. In this study, we performed cryogenic coherent X-ray diffraction imaging of human erythrocytes with and without malaria infection. To shed light on structural features near the surface, "ghost cells" were prepared by the removal of cytoplasm. From two-dimensional images, we found that the surface of erythrocytes after 32 h of infection became much rougher compared to that of healthy, uninfected erythrocytes. The Gaussian roughness of an infected erythrocyte surface (69 nm) is about two times larger than that of an uninfected one (31 nm), reflecting the formation of protein knobs on infected erythrocyte surfaces. Three-dimensional tomography further enables to obtain images of the whole cells with no remarkable radiation damage, whose accuracy was estimated using phase retrieval transfer functions to be as good as 64 nm for uninfected and 80 nm for infected erythrocytes, respectively. Future improvements in phase retrieval algorithm, increase in degree of coherence, and higher flux in combination with complementary X-ray fluorescence are necessary to gain both structural and chemical details of mesoscopic architectures, such as cytoskeletons, membraneous structures, and protein complexes, in frozen hydrated human cells, especially under diseased states.

Catharanthus roseus: a natural source for the synthesis of silver nanoparticles

PubMed Central

Mukunthan, KS; Elumalai, EK; Patel, Trupti N; Murty, V Ramachandra

2011-01-01

Objective To develop a simple rapid procedure for bioreduction of silver nanoparticles (AgNPs) using aqueous leaves extracts of Catharanthus roseus (C. roseus). Methods Characterization were determined by using UV-Vis spectrophotometry, scanning electron microscopy (SEM), energy dispersive X-ray and X-ray diffraction. Results SEM showed the formation of silver nanoparticles with an average size of 67 nm to 48 nm. X-ray diffraction analysis showed that the particles were crystalline in nature with face centered cubic geometry. Conclusions C. roseus demonstrates strong potential for synthesis of silver nanoparticles by rapid reduction of silver ions (Ag+ to Ag0). This study provides evidence for developing large scale commercial production of value-added products for biomedical/nanotechnology-based industries. PMID:23569773

Three-dimensional structure determination protocol for noncrystalline biomolecules using x-ray free-electron laser diffraction imaging.

PubMed

Oroguchi, Tomotaka; Nakasako, Masayoshi

2013-02-01

Coherent and intense x-ray pulses generated by x-ray free-electron laser (XFEL) sources are paving the way for structural determination of noncrystalline biomolecules. However, due to the small scattering cross section of electrons for x rays, the available incident x-ray intensity of XFEL sources, which is currently in the range of 10(12)-10(13) photons/μm(2)/pulse, is lower than that necessary to perform single-molecule diffraction experiments for noncrystalline biomolecules even with the molecular masses of megadalton and submicrometer dimensions. Here, we propose an experimental protocol and analysis method for visualizing the structure of those biomolecules by the combined application of coherent x-ray diffraction imaging and three-dimensional reconstruction methods. To compensate the small scattering cross section of biomolecules, in our protocol, a thin vitreous ice plate containing several hundred biomolecules/μm(2) is used as sample, a setup similar to that utilized by single-molecule cryoelectron microscopy. The scattering cross section of such an ice plate is far larger than that of a single particle. The images of biomolecules contained within irradiated areas are then retrieved from each diffraction pattern, and finally provide the three-dimensional electron density model. A realistic atomic simulation using large-scale computations proposed that the three-dimensional structure determination of the 50S ribosomal subunit embedded in a vitreous ice plate is possible at a resolution of 0.8 nm when an x-ray beam of 10(16) photons/500×500 nm(2)/pulse is available.

High-energy cryo x-ray nano-imaging at the ID16A beamline of ESRF

NASA Astrophysics Data System (ADS)

da Silva, Julio C.; Pacureanu, Alexandra; Yang, Yang; Fus, Florin; Hubert, Maxime; Bloch, Leonid; Salome, Murielle; Bohic, Sylvain; Cloetens, Peter

2017-09-01

The ID16A beamline at ESRF offers unique capabilities for X-ray nano-imaging, and currently produces the worlds brightest high energy diffraction-limited nanofocus. Such a nanoprobe was designed for quantitative characterization of the morphology and the elemental composition of specimens at both room and cryogenic temperatures. Billions of photons per second can be delivered in a diffraction-limited focus spot size down to 13 nm. Coherent X-ray imaging techniques, as magnified holographic-tomography and ptychographic-tomography, are implemented as well as X-ray fluorescence nanoscopy. We will show the latest developments in coherent and spectroscopic X-ray nanoimaging implemented at the ID16A beamline

Soft x-ray reduction camera for submicron lithography

DOEpatents

Hawryluk, Andrew M.; Seppala, Lynn G.

1991-01-01

Soft x-ray projection lithography can be performed using x-ray optical components and spherical imaging lenses (mirrors), which form an x-ray reduction camera. The x-ray reduction is capable of projecting a 5x demagnified image of a mask onto a resist coated wafer using 4.5 nm radiation. The diffraction limited resolution of this design is about 135 nm with a depth of field of about 2.8 microns and a field of view of 0.2 cm.sup.2. X-ray reflecting masks (patterned x-ray multilayer mirrors) which are fabricated on thick substrates and can be made relatively distortion free are used, with a laser produced plasma for the source. Higher resolution and/or larger areas are possible by varying the optic figures of the components and source characteristics.

HYBRID Simulations of Diffraction-Limited Focusing with Kirkpatrick-Baez Mirrors for a Next-Generation In Situ Hard X-ray Nanoprobe

NASA Astrophysics Data System (ADS)

Maser, Jörg; Shi, Xianbo; Reininger, Ruben; Lai, Barry; Vogt, Stefan

2016-12-01

Next-generation hard X-ray nanoprobe beamlines such as the In Situ Nanoprobe (ISN) beamline being planned at the Advanced Photon Source aim at providing very high spatial resolution while also enabling very high focused flux, to study complex materials and devices using fast, multidimensional imaging across many length scales. The ISN will use diffractive optics to focus X-rays with a bandpass of Δ E/ E = 10-4 into a focal spot of 20 nm or below. Reflective optics in Kirkpatrick-Baez geometry will be used to focus X-rays with a bandpass as large as Δ E/ E = 10-2 into a focal spot of 50 nm. Diffraction-limited focusing with reflective optics is achieved by spatial filtering and use of a very long, vertically focusing mirror. To quantify the performance of the ISN beamline, we have simulated the propagation of both partially and fully coherent wavefronts from the undulator source, through the ISN beamline and into the mirror-based focal spot. Simulations were carried out using the recently developed software " HYBRID."

Optical properties of cerium oxide (CeO2) nanoparticles synthesized by hydroxide mediated method

NASA Astrophysics Data System (ADS)

Ali, Mawlood Maajal; Mahdi, Hadeel Salih; Parveen, Azra; Azam, Ameer

2018-05-01

The nanoparticles of cerium oxide have been successfully synthesized by hydroxide mediated method, using cerium nitrate and sodium hydroxide as precursors. The microstructural properties were analyzed by X-ray diffraction technique (XRD). The X-ray diffraction results show that the cerium oxide nanoparticles were in cubic structure. The optical absorption spectra of cerium oxide were recorded by UV-VIS spectrophotometer in the range of 320 to 600 nm and photoluminescence spectra in the range of 400-540 nm and have been presented. The energy band gap was determined by Tauc relationship. The crystallite size was determined from Debye-Scherer equation and came out to be 6.4 nm.

Soft x-ray reduction camera for submicron lithography

DOEpatents

Hawryluk, A.M.; Seppala, L.G.

1991-03-26

Soft x-ray projection lithography can be performed using x-ray optical components and spherical imaging lenses (mirrors), which form an x-ray reduction camera. The x-ray reduction is capable of projecting a 5x demagnified image of a mask onto a resist coated wafer using 4.5 nm radiation. The diffraction limited resolution of this design is about 135 nm with a depth of field of about 2.8 microns and a field of view of 0.2 cm[sup 2]. X-ray reflecting masks (patterned x-ray multilayer mirrors) which are fabricated on thick substrates and can be made relatively distortion free are used, with a laser produced plasma for the source. Higher resolution and/or larger areas are possible by varying the optic figures of the components and source characteristics. 9 figures.

Coherent diffraction imaging analysis of shape-controlled nanoparticles with focused hard X-ray free-electron laser pulses.

PubMed

Takahashi, Yukio; Suzuki, Akihiro; Zettsu, Nobuyuki; Oroguchi, Tomotaka; Takayama, Yuki; Sekiguchi, Yuki; Kobayashi, Amane; Yamamoto, Masaki; Nakasako, Masayoshi

2013-01-01

We report the first demonstration of the coherent diffraction imaging analysis of nanoparticles using focused hard X-ray free-electron laser pulses, allowing us to analyze the size distribution of particles as well as the electron density projection of individual particles. We measured 1000 single-shot coherent X-ray diffraction patterns of shape-controlled Ag nanocubes and Au/Ag nanoboxes and estimated the edge length from the speckle size of the coherent diffraction patterns. We then reconstructed the two-dimensional electron density projection with sub-10 nm resolution from selected coherent diffraction patterns. This method enables the simultaneous analysis of the size distribution of synthesized nanoparticles and the structures of particles at nanoscale resolution to address correlations between individual structures of components and the statistical properties in heterogeneous systems such as nanoparticles and cells.

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

PubMed

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

2009-09-01

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

Growth of high quality and large-sized Rb 0.3MoO 3 single crystals by molten salt electrolysis method

NASA Astrophysics Data System (ADS)

Wang, Junfeng; Xiong, Rui; Yi, Fan; Yin, Di; Ke, Manzhu; Li, Changzhen; Liu, Zhengyou; Shi, Jing

2005-05-01

High quality and large-sized Rb 0.3MoO 3 single crystals were synthesized by molten salt electrolysis method. X-ray diffraction (XRD) patterns and rocking curves, as well as the white beam Laue diffraction of X-ray images show the crystals grown by this method have high quality. The lattice constants evaluated from XRD patterns are a0=1.87 nm, b0=0.75 nm, c0=1.00 nm, β=118.83∘. The in situ selected area electron diffraction (SAED) patterns along the [101¯], [11¯1¯] and [103¯] zone axes at room temperature indicate that the Rb 0.3MoO 3 crystal possess perfect C-centered symmetry. Temperature dependence of the resistivity shows this compound undergoes a metal to semiconductor transition at 183 K.

Hard X-ray multilayer zone plate with 25-nm outermost zone width

NASA Astrophysics Data System (ADS)

Takano, H.; Sumida, K.; Hirotomo, H.; Koyama, T.; Ichimaru, S.; Ohchi, T.; Takenaka, H.; Kagoshima, Y.

2017-06-01

We have improved the performance of a previously reported multilayer zone plate by reducing its outermost zone width, using the same multilayer materials (MoSi2 and Si) and fabrication technique. The focusing performance was evaluated at the BL24XU of SPring-8 using 20-keV X-rays. The line spread function (LSF) in the focal plane was measured using a dark-field knife-edge scan method, and the point spread function was obtained from the LSF through a tomographic reconstruction principle. The spatial resolution was estimated to be 30 nm, which is in relatively good agreement with the calculated diffraction-limited value of 25 nm, while the measured diffraction efficiency of the +1st order was 24%.

An instrument for 3D x-ray nano-imaging

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

Holler, M.; Raabe, J.; Diaz, A.

We present an instrument dedicated to 3D scanning x-ray microscopy, allowing a sample to be precisely scanned through a beam while the angle of x-ray incidence can be changed. The position of the sample is controlled with respect to the beam-defining optics by laser interferometry. The instrument achieves a position stability better than 10 nm standard deviation. The instrument performance is assessed using scanning x-ray diffraction microscopy and we demonstrate a resolution of 18 nm in 2D imaging of a lithographic test pattern while the beam was defined by a pinhole of 3 {mu}m in diameter. In 3D on amore » test object of copper interconnects of a microprocessor, a resolution of 53 nm is achieved.« less

HYBRID simulations of diffraction-limited focusing with Kirkpatrick-Baez mirrors for a next-generation In Situ hard X-ray nanoprobe

DOE PAGES

Maser, Jorg; Shi, Xianbo; Reininger, Ruben; ...

2016-02-22

Next-generation hard X-ray nanoprobe beamlines such as the In Situ Nanoprobe (ISN) beamline being planned at the Advanced Photon Source aim at providing very high spatial resolution while also enabling very high focused flux, to study complex materials and devices using fast, multidimensional imaging across many length scales. The ISN will use diffractive optics to focus X-rays with a bandpass of ΔE/E = 10 –4 into a focal spot of 20 nm or below. Reflective optics in Kirkpatrick-Baez geometry will be used to focus X-rays with a bandpass as large as ΔE/E = 10 –2 into a focal spot ofmore » 50 nm. Diffraction-limited focusing with reflective optics is achieved by spatial filtering and use of a very long, vertically focusing mirror. Furthermore, to quantify the performance of the ISN beamline, we have simulated the propagation of both partially and fully coherent wavefronts from the undulator source, through the ISN beamline and into the mirror-based focal spot. Simulations were carried out using the recently developed software “HYBRID.”« less

Crystalline Stratification in Semiconducting Polymer Thin Film Quantified by Grazing Incidence X-ray Scattering

NASA Astrophysics Data System (ADS)

Gann, Eliot; Caironi, Mario; Noh, Yong-Young; Kim, Yun-Hi; McNeill, Christopher R.

The depth dependence of crystalline structure within thin films is critical for many technological applications, but has been impossible to measure directly using common techniques. In this work, by monitoring diffraction peak intensity and location and utilizing the highly angle-dependent waveguiding effects of X-rays near grazing incidence we quantitatively measure the thickness, roughness and orientation of stratified crystalline layers within thin films of a high-performance semiconducting polymer. In particular, this diffractive X-ray waveguiding reveals a self-organized 5-nm-thick crystalline surface layer with crystalline orientation orthogonal to the underlying 65-nm-thick layer. While demonstrated for an organic semiconductor film, this approach is applicable to any thin film material system where stratified crystalline structure and orientation can influence important interfacial processes such as charge injection and field-effect transport.

Low-dose, high-resolution and high-efficiency ptychography at STXM beamline of SSRF

NASA Astrophysics Data System (ADS)

Xu, Zijian; Wang, Chunpeng; Liu, Haigang; Tao, Xulei; Tai, Renzhong

2017-06-01

Ptychography is a diffraction-based X-ray microscopy method that can image extended samples quantitatively while remove the resolution limit imposed by image-forming optical elements. As a natural extension of scanning transmission X-ray microscopy (STXM) imaging method, we developed soft X-ray ptychographic coherent diffraction imaging (PCDI) method at the STXM endstation of BL08U beamline of Shanghai Synchrotron Radiation Facility. Compared to the traditional STXM imaging, the new PCDI method has resulted in significantly lower dose, higher resolution and higher efficiency imaging in our platform. In the demonstration experiments shown here, a spatial resolution of sub-10 nm was obtained for a gold nanowires sample, which is much better than the limit resolution 30 nm of the STXM method, while the radiation dose is only 1/12 of STXM.

Imaging fully hydrated whole cells by coherent x-ray diffraction microscopy.

PubMed

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Naitow, Hisashi; Kunishima, Naoki; Yoshida, Takashi; Ishikawa, Tetsuya; Song, Changyong

2013-03-01

Nanoscale imaging of biological specimens in their native condition is of long-standing interest, in particular with direct, high resolution views of internal structures of intact specimens, though as yet progress has been limited. Here we introduce wet coherent x-ray diffraction microscopy capable of imaging fully hydrated and unstained biological specimens. Whole cell morphologies and internal structures better than 25 nm can be clearly visualized without contrast degradation.

Hydrothermal synthesis infrared to visible upconversion luminescence of SrMoO4: Er3+/Yb3+ phosphor

NASA Astrophysics Data System (ADS)

Sinha, Shriya; Kumar, Kaushal

2018-04-01

The upconversion emission properties in Er3+/Yb3+ doped SrMoO4 phosphor synthesized via hydrothermal method is investigated upon 980 nm laser light excitation. The crystal structure and morphology of the synthesized phosphor are characterized by X-ray diffraction and field emission scanning electron microscopy. The X-ray diffraction pattern suggests that SrMoO4 phosphor has tetragonal phase structure. The phosphor emits strong green (525 and 552 nm) and red (665 nm) UC emissions along with weak blue (410 and 488 nm) and near infrared (798 nm) emission bands. The color emitted from the phosphor is shifted from yellow to green region with increasing the power density from 15 to 65 W/cm2. The result indicates that the present material is suitable for making infrared to visible up-converts and display devices.

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

DOE PAGES

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

2017-10-05

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

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

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

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

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

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

Munke, Anna; Andreasson, Jakob; Aquila, Andrew

Single particle diffractive imaging data from Rice Dwarf Virus (RDV) were recorded using the Coherent X-ray Imaging (CXI) instrument at the Linac Coherent Light Source (LCLS). RDV was chosen as it is a well-characterized model system, useful for proof-of-principle experiments, system optimization and algorithm development. RDV, an icosahedral virus of about 70 nm in diameter, was aerosolized and injected into the approximately 0.1 μm diameter focused hard X-ray beam at the CXI instrument of LCLS. Diffraction patterns from RDV with signal to 5.9 Ångström were recorded. Here, the diffraction data are available through the Coherent X-ray Imaging Data Bank (CXIDB)more » as a resource for algorithm development, the contents of which are described here.« less

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Preparation and X-Ray diffraction studies of curium hydrides

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

Gibson, J.K.; Maire, R.G.

Curium hydrides were prepared by reaction of curium-248 metal with hydrogen and characterized by X-ray powder diffraction. Several of the syntheses resulted in a hexagonal compound with average lattice parameters of a/sub 0/ = 0.3769(8) nm and c/sub 0/ = 0.6732(12) nm. These products are considere to be CmH/sub 3//sup -//sub 8/ by analogy with the behavior of lanthanide-hydrogen and lighter actinide-hydrogen systems. Face-centered cubic products with an average lattice parameter of a/sub 0/ = 0.5322(4) nm were obtained from other curium hydride preparations. This parameter is slightly smaller than that reported previously for cubic curium dihydride, CmH /SUB 2-x/more » (B.M. Bansal and D. Damien. Inorg. Nucl. Chem. Lett. 6 603, 1970). The present results established a continuation of typical heavy trivalent lanthanidelike behavior of the transuranium actinide-hydrogen systems through curium.« less

Preparation and X-ray diffraction studies of curium hydrides

NASA Astrophysics Data System (ADS)

Gibson, J. K.; Haire, R. G.

1985-10-01

Curium hydrides were prepared by reaction of curium-248 metal with hydrogen and characterized by X-ray powder diffraction. Several of the syntheses resulted in a hexagonal compound with average lattice parameters of a0 = 0.3769(8) nm and c0 = 0.6732(12) nm. These products are considered to be CmH 3-δ by analogy with the behavior of lanthanide-hydrogen and lighter actinide-hydrogen systems. Face-centered cubic products with an average lattice parameter of a0 = 0.5322(4) nm were obtained from other curium hydride preparations. This parameter is slightly smaller than that reported previously for cubic curium dihydride, CmH 2+ x (B. M. Bansal and D. Damien, Inorg. Nucl. Chem. Lett., 6, 603, 1970). The present results established a continuation of typical heavy trivalent lanthanide-like behavior of the transuranium actinide-hydrogen systems through curium.

High-dynamic-range coherent diffractive imaging: ptychography using the mixed-mode pixel array detector

PubMed Central

Giewekemeyer, Klaus; Philipp, Hugh T.; Wilke, Robin N.; Aquila, Andrew; Osterhoff, Markus; Tate, Mark W.; Shanks, Katherine S.; Zozulya, Alexey V.; Salditt, Tim; Gruner, Sol M.; Mancuso, Adrian P.

2014-01-01

Coherent (X-ray) diffractive imaging (CDI) is an increasingly popular form of X-ray microscopy, mainly due to its potential to produce high-resolution images and the lack of an objective lens between the sample and its corresponding imaging detector. One challenge, however, is that very high dynamic range diffraction data must be collected to produce both quantitative and high-resolution images. In this work, hard X-ray ptychographic coherent diffractive imaging has been performed at the P10 beamline of the PETRA III synchrotron to demonstrate the potential of a very wide dynamic range imaging X-ray detector (the Mixed-Mode Pixel Array Detector, or MM-PAD). The detector is capable of single photon detection, detecting fluxes exceeding 1 × 108 8-keV photons pixel−1 s−1, and framing at 1 kHz. A ptychographic reconstruction was performed using a peak focal intensity on the order of 1 × 1010 photons µm−2 s−1 within an area of approximately 325 nm × 603 nm. This was done without need of a beam stop and with a very modest attenuation, while ‘still’ images of the empty beam far-field intensity were recorded without any attenuation. The treatment of the detector frames and CDI methodology for reconstruction of non-sensitive detector regions, partially also extending the active detector area, are described. PMID:25178008

High-dynamic-range coherent diffractive imaging: ptychography using the mixed-mode pixel array detector.

PubMed

Giewekemeyer, Klaus; Philipp, Hugh T; Wilke, Robin N; Aquila, Andrew; Osterhoff, Markus; Tate, Mark W; Shanks, Katherine S; Zozulya, Alexey V; Salditt, Tim; Gruner, Sol M; Mancuso, Adrian P

2014-09-01

Coherent (X-ray) diffractive imaging (CDI) is an increasingly popular form of X-ray microscopy, mainly due to its potential to produce high-resolution images and the lack of an objective lens between the sample and its corresponding imaging detector. One challenge, however, is that very high dynamic range diffraction data must be collected to produce both quantitative and high-resolution images. In this work, hard X-ray ptychographic coherent diffractive imaging has been performed at the P10 beamline of the PETRA III synchrotron to demonstrate the potential of a very wide dynamic range imaging X-ray detector (the Mixed-Mode Pixel Array Detector, or MM-PAD). The detector is capable of single photon detection, detecting fluxes exceeding 1 × 10(8) 8-keV photons pixel(-1) s(-1), and framing at 1 kHz. A ptychographic reconstruction was performed using a peak focal intensity on the order of 1 × 10(10) photons µm(-2) s(-1) within an area of approximately 325 nm × 603 nm. This was done without need of a beam stop and with a very modest attenuation, while `still' images of the empty beam far-field intensity were recorded without any attenuation. The treatment of the detector frames and CDI methodology for reconstruction of non-sensitive detector regions, partially also extending the active detector area, are described.

Imaging whole Escherichia coli bacteria by using single-particle x-ray diffraction

NASA Astrophysics Data System (ADS)

Miao, Jianwei; Hodgson, Keith O.; Ishikawa, Tetsuya; Larabell, Carolyn A.; Legros, Mark A.; Nishino, Yoshinori

2003-01-01

We report the first experimental recording, to our knowledge, of the diffraction pattern from intact Escherichia coli bacteria using coherent x-rays with a wavelength of 2 Å. By using the oversampling phasing method, a real space image at a resolution of 30 nm was directly reconstructed from the diffraction pattern. An R factor used for characterizing the quality of the reconstruction was in the range of 5%, which demonstrated the reliability of the reconstruction process. The distribution of proteins inside the bacteria labeled with manganese oxide has been identified and this distribution confirmed by fluorescence microscopy images. Compared with lens-based microscopy, this diffraction-based imaging approach can examine thicker samples, such as whole cultured cells, in three dimensions with resolution limited only by radiation damage. Looking forward, the successful recording and reconstruction of diffraction patterns from biological samples reported here represent an important step toward the potential of imaging single biomolecules at near-atomic resolution by combining single-particle diffraction with x-ray free electron lasers.

The structural properties of flower-like ZnO nanostructures on porous silicon

NASA Astrophysics Data System (ADS)

Eswar, Kevin Alvin; Suhaimi, Mohd Husairi Fadzillah; Guliling, Muliyadi; Mohamad, Maryam; Khusaimi, Zuraida; Rusop, M.; Abdullah, Saifollah

2018-05-01

The flower-like zinc oxide (ZnO) were successfully synthesized on porous silicon (PSi) via hydrothermal method. The characteristic of ZnO nanostructures was investigated using field emission scanning microscopy (FESEM) and X-ray diffraction (X-Ray). The FESEM images show the flower-like ZnO nanostructures composed ZnO nanoparticles. The X-ray diffraction shows that strong intensity of (100), (002) and (101) peaks. The structural analysis revealed that the peaks angles were shifted due to the stress or imperfection of the crystalline of ZnO nanostructures. The crystalline sizes in range of 42.60 to 54.09 nm were produced.

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

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

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

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

Growth and characterization of 4-chloro-3-nitrobenzophenone single crystals using vertical Bridgman technique

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

Aravinth, K., E-mail: anandcgc@gmail.com; Babu, G. Anandha, E-mail: anandcgc@gmail.com; Ramasamy, P., E-mail: anandcgc@gmail.com

2014-04-24

4-chloro-3-nitrobenzophenone (4C3N) has been grown by using vertical Bridgman technique. The grown crystal was confirmed by Powder X-ray diffraction analysis. The crystalline perfection of the grown crystal was examined by high-resolution X-ray diffraction study. The fluorescence spectra of grown 4C3N single crystals exhibit emission peak at 575 nm. The micro hardness measurements were used to analyze the mechanical property of the grown crystal.

FT-IR and Zeta potential measurements on TiO nanoparticles

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

Singh, Jaiveer; Rathore, Ravi; Kaurav, Netram, E-mail: netramkaurav@yahoo.co.uk

2016-05-23

In the present investigation, ultrafine TiO particles have been synthesized successfully by thermal decomposition method. The sample was characterized by X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. As-synthesized TiO nanoparticles have a cubic structure as characterized by power X-ray diffraction (XRD), which shows that TiO nanoparticles have narrow size distribution with particle size 11.5 nm. FTIR data shows a strong peak at 1300 cm{sup −1}, assignable to the Ti-O stretching vibrations mode.

Synthesis and photoluminescence of ultra-pure germanium nanoparticles

NASA Astrophysics Data System (ADS)

Chivas, R.; Yerci, S.; Li, R.; Dal Negro, L.; Morse, T. F.

2011-09-01

We have used aerosol deposition to synthesize defect and micro-strain free, ultra-pure germanium nanoparticles. Transmission electron microscopy images show a core-shell configuration with highly crystalline core material. Powder X-ray diffraction measurements verify the presence of highly pure, nano-scale germanium with average crystallite size of 30 nm and micro-strain of 0.058%. X-ray photoelectron spectroscopy demonstrates that GeO x ( x ⩽ 2) shells cover the surfaces of the nanoparticles. Under optical excitation, these nanoparticles exhibit two separate emission bands at room temperature: a visible emission at 500 nm with 0.5-1 ns decay times and an intense near-infrared emission at 1575 nm with up to ˜20 μs lifetime.

Experimental strategies for imaging bioparticles with femtosecond hard X-ray pulses

DOE PAGES

Daurer, Benedikt J.; Okamoto, Kenta; Bielecki, Johan; ...

2017-04-07

This study explores the capabilities of the Coherent X-ray Imaging Instrument at the Linac Coherent Light Source to image small biological samples. The weak signal from small samples puts a significant demand on the experiment. AerosolizedOmono River virusparticles of ~40 nm in diameter were injected into the submicrometre X-ray focus at a reduced pressure. Diffraction patterns were recorded on two area detectors. The statistical nature of the measurements from many individual particles provided information about the intensity profile of the X-ray beam, phase variations in the wavefront and the size distribution of the injected particles. The results point to amore » wider than expected size distribution (from ~35 to ~300 nm in diameter). This is likely to be owing to nonvolatile contaminants from larger droplets during aerosolization and droplet evaporation. The results suggest that the concentration of nonvolatile contaminants and the ratio between the volumes of the initial droplet and the sample particles is critical in such studies. The maximum beam intensity in the focus was found to be 1.9 × 10 12photons per µm 2per pulse. The full-width of the focus at half-maximum was estimated to be 500 nm (assuming 20% beamline transmission), and this width is larger than expected. Under these conditions, the diffraction signal from a sample-sized particle remained above the average background to a resolution of 4.25 nm. Finally, the results suggest that reducing the size of the initial droplets during aerosolization is necessary to bring small particles into the scope of detailed structural studies with X-ray lasers.« less

Structure and giant magnetoresistance of granular Co-Cu nanolayers prepared by cross-beam pulsed laser deposition

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

Jesche, A.; Stoecker, H.; Levin, A. A.

2010-01-15

A series of Co{sub x}Cu{sub 100-x} (x=0, 40-75, 100) layers with thicknesses between 13 and 55 nm were prepared on silicon substrates using cross-beam pulsed laser deposition. Wide-angle x-ray diffraction (WAXRD), transmission electron microscopy (TEM), and electrical transport measurements revealed a structure consisting of decomposed cobalt and copper grains with grain sizes of about 10 nm. The influence of cobalt content and layer thickness on the grain size is discussed. Electron diffraction indicates the presence of an intermetallic Co-Cu phase of Cu{sub 3}Au structure type. Thermal treatment at temperatures between 525 and 750 K results in the progressive decomposition ofmore » Co and Cu, with an increase of the grain sizes up to about 100 nm. This is tunable by controlling the temperature and duration of the anneal, and is directly observable in WAXRD patterns and TEM images. A careful analysis of grain size and the coherence length of the radiation used allows for an accurate interpretation of the x-ray diffraction patterns, by taking into account coherent and noncoherent scattering. The alloy films show a giant magnetoresistance of 1%-2.3% with the maximum obtained after annealing at around 725 K.« less

Biological imaging by soft X-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Shapiro, David

We have developed a microscope for soft x-ray diffraction imaging of dry or frozen hydrated biological specimens. This lensless imaging system does not suffer from the resolution or specimen thickness limitations that other short wavelength microscopes experience. The microscope, currently situated at beamline 9.0.1 of the Advanced Light Source, can collect diffraction data to 12 nm resolution with 750 eV photons and 17 nm resolution with 520 eV photons. The specimen can be rotated with a precision goniometer through an angle of 160 degrees allowing for the collection of nearly complete three-dimensional diffraction data. The microscope is fully computer controlled through a graphical user interface and a scripting language automates the collection of both two-dimensional and three-dimensional data. Diffraction data from a freeze-dried dwarf yeast cell, Saccharomyces cerevisiae carrying the CLN3-1 mutation, was collected to 12 run resolution from 8 specimen orientations spanning a total rotation of 8 degrees. The diffraction data was phased using the difference map algorithm and the reconstructions provide real space images of the cell to 30 nm resolution from each of the orientations. The agreement of the different reconstructions provides confidence in the recovered, and previously unknown, structure and indicates the three dimensionality of the cell. This work represents the first imaging of the natural complex refractive contrast from a whole unstained cell by the diffraction microscopy method and has achieved a resolution superior to lens based x-ray tomographic reconstructions of similar specimens. Studies of the effects of exposure to large radiation doses were also carried out. It was determined that the freeze-dried cell suffers from an initial collapse, which is followed by a uniform, but slow, shrinkage. This structural damage to the cell is not accompanied by a diminished ability to see small features in the specimen. Preliminary measurements on frozen-hydrated yeast indicate that the frozen specimens do not exhibit these changes even with doses as high as 5 x 109 Gray.

Fabrication of Three-Dimensional Nanostructures for Thermal Study

DTIC Science & Technology

2013-01-01

Cu2O Inverse Opal …………………………………24 3.4 X - ray Analysis of the Structure …………………………………………………….26 3.5 Discussion and Future Direction...2.3 Characterization of Silicon Inverse Opal The 80 nm and 40 nm silicon inverse opal material properties were characterized by x - ray diffraction... x - ray beam of 1 ° relative to the surface of the sample was used due to the low amounts silicon present in the thin porous structure to enhance the

Green synthesis, characterization and some physico-chemical studies on a novel intermolecular compound; 4-nitro-o-phenylenediamine-N, N-dimethylaminobenzaldehyde system

NASA Astrophysics Data System (ADS)

Rai, U. S.; Singh, Manjeet; Rai, R. N.

2017-09-01

An inter-molecular compound (IMC) L1 was synthesized by taking 1:1 molar ratio of p-nitro-o-phenylenediamine (NOPDA) and N, N-dimethylaminobenzaldehyde (DMAB) via thermally initiated solid state reaction. It was characterized by X-ray diffraction, spectral and optical studies. The single crystal of the (L1) was grown from saturated solution of ethanol using slow evaporation technique at 29 °C. From the single crystal X-ray diffraction analysis, it can be inferred that it crystallizes in triclinic unit cell with P-1 space group (CCDC No 1422765). Absorption spectrum of IMC (L1) shows a band at 318 nm attributed to the intra-molecular charge-transfer (ICT) excited state absorption and the other band at 376 nm is due to n→π* transition. The IMC (L1) shows a strong fluorescence at 418 nm with a Stokes shift (≈100 nm) and quantum efficiency (0.22) upon excitation in methyl alcohol at 318 nm.

Development of variable-magnification X-ray Bragg optics.

PubMed

Hirano, Keiichi; Yamashita, Yoshiki; Takahashi, Yumiko; Sugiyama, Hiroshi

2015-07-01

A novel X-ray Bragg optics is proposed for variable-magnification of an X-ray beam. This X-ray Bragg optics is composed of two magnifiers in a crossed arrangement, and the magnification factor, M, is controlled through the azimuth angle of each magnifier. The basic properties of the X-ray optics such as the magnification factor, image transformation matrix and intrinsic acceptance angle are described based on the dynamical theory of X-ray diffraction. The feasibility of the variable-magnification X-ray Bragg optics was verified at the vertical-wiggler beamline BL-14B of the Photon Factory. For X-ray Bragg magnifiers, Si(220) crystals with an asymmetric angle of 14° were used. The magnification factor was calculated to be tunable between 0.1 and 10.0 at a wavelength of 0.112 nm. At various magnification factors (M ≥ 1.0), X-ray images of a nylon mesh were observed with an air-cooled X-ray CCD camera. Image deformation caused by the optics could be corrected by using a 2 × 2 transformation matrix and bilinear interpolation method. Not only absorption-contrast but also edge-contrast due to Fresnel diffraction was observed in the magnified images.

Crystalline silicon growth in nickel/a-silicon bilayer

NASA Astrophysics Data System (ADS)

Mohiddon, Md Ahamad; Naidu, K. Lakshun; Dalba, G.; Rocca, F.; Krishna, M. Ghanashyam

2013-02-01

The effect of substrate temperature on amorphous Silicon crystallization, mediated by metal impurity is reported. Bilayers of Ni(200nm)/Si(400nm) are deposited on fused silica substrate by electron beam evaporator at 200 and 500 °C. Raman mapping shows that, 2 to 5 micron size crystalline silicon clusters are distributed over the entire surface of the sample. X-ray diffraction and X-ray absorption spectroscopy studies demonstrate silicon crystallizes over the metal silicide seeds and grow with the annealing temperature.

Near-surface density profiling of Fe ion irradiated Si (100) using extremely asymmetric x-ray diffraction by variation of the wavelength

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

Khanbabaee, B., E-mail: khanbabaee@physik.uni-siegen.de; Pietsch, U.; Facsko, S.

2014-10-20

In this work, we report on correlations between surface density variations and ion parameters during ion beam-induced surface patterning process. The near-surface density variations of irradiated Si(100) surfaces were investigated after off-normal irradiation with 5 keV Fe ions at different fluences. In order to reduce the x-ray probing depth to a thickness below 5 nm, the extremely asymmetrical x-ray diffraction by variation of wavelength was applied, exploiting x-ray refraction at the air-sample interface. Depth profiling was achieved by measuring x-ray rocking curves as function of varying wavelengths providing incidence angles down to 0°. The density variation was extracted from the deviationsmore » from kinematical Bragg angle at grazing incidence angles due to refraction of the x-ray beam at the air-sample interface. The simulations based on the dynamical theory of x-ray diffraction revealed that while a net near-surface density decreases with increasing ion fluence which is accompanied by surface patterning, there is a certain threshold of ion fluence to surface density modulation. Our finding suggests that the surface density variation can be relevant with the mechanism of pattern formation.« less

Optics for coherent X-ray applications.

PubMed

Yabashi, Makina; Tono, Kensuke; Mimura, Hidekazu; Matsuyama, Satoshi; Yamauchi, Kazuto; Tanaka, Takashi; Tanaka, Hitoshi; Tamasaku, Kenji; Ohashi, Haruhiko; Goto, Shunji; Ishikawa, Tetsuya

2014-09-01

Developments of X-ray optics for full utilization of diffraction-limited storage rings (DLSRs) are presented. The expected performance of DLSRs is introduced using the design parameters of SPring-8 II. To develop optical elements applicable to manipulation of coherent X-rays, advanced technologies on precise processing and metrology were invented. With propagation-based coherent X-rays at the 1 km beamline of SPring-8, a beryllium window fabricated with the physical-vapour-deposition method was found to have ideal speckle-free properties. The elastic emission machining method was utilized for developing reflective mirrors without distortion of the wavefronts. The method was further applied to production of diffraction-limited focusing mirrors generating the smallest spot size in the sub-10 nm regime. To enable production of ultra-intense nanobeams at DLSRs, a low-vibration cooling system for a high-heat-load monochromator and advanced diagnostic systems to characterize X-ray beam properties precisely were developed. Finally, new experimental schemes for combinative nano-analysis and spectroscopy realised with novel X-ray optics are discussed.

Structural and spectral properties of MgZnO2:Sm3+ phosphor

NASA Astrophysics Data System (ADS)

Rajput, Preasha; Sharma, Pallavi; Biswas, Pankaj; Kamni

2018-05-01

The samarium doped MgZnO2 phosphor was synthesized by the low-cost combustion method. The powder X-ray diffraction (XRD) analysis confirmed the crystallinity and phase purity of the phosphor. The lattice parameters were determined by indexing the diffraction peaks. The photoluminescence (PL) study revealed that the phosphor exhibited a broad excitation band in the UV region ranging between 200 to 350 nm. The 601 nm emission was ascribed to 4G5/2 to 6H7/2 transitions of the Sm3+ ion. The optical bandgap of MgZnO2:Sm3+ was obtained to be 3.56 eV. The phosphor can be projected as a useful material in X- and gamma-ray scintillators.

In situ X-ray-based imaging of nano materials

DOE PAGES

Weker, Johanna Nelson; Huang, Xiaojing; Toney, Michael F.

2016-02-13

We study functional nanomaterials that are heterogeneous and understanding their behavior during synthesis and operation requires high resolution diagnostic imaging tools that can be used in situ. Over the past decade, huge progress has been made in the development of X-ray based imaging, including full field and scanning microscopy and their analogs in coherent diffractive imaging. Currently, spatial resolution of about 10 nm and time resolution of sub-seconds are achievable. For catalysis, X-ray imaging allows tracking of particle chemistry under reaction conditions. In energy storage, in situ X-ray imaging of electrode particles is providing important insight into degradation processes. Recently,more » both spatial and temporal resolutions are improving to a few nm and milliseconds and these developments will open up unprecedented opportunities.« less

Symposium U: Thermoelectric Power Generation. Held in Boston, Massachusetts on November 26-29, 2007

DTIC Science & Technology

2008-04-01

including X - ray /electron diffraction, TGA analysis, Raman / Fourier Transform Infrared Spectroscopy, electron microscopy, Rutherford back-scattering and...Energy dispersive X - ray analysis were performed on the treated sample. The results revealed that a surface layer (from 10 nm to up to micron in...nanoparticles into a matrix of bulk Bi2Te 3 material via a hot pressing process. These nanocomposites have been examined by SEM and X - ray powder

Soft X-ray holographic grating beam splitter including a double frequency grating for interferometer pre-alignment.

PubMed

Liu, Ying; Tan, Xin; Liu, Zhengkun; Xu, Xiangdong; Hong, Yilin; Fu, Shaojun

2008-09-15

Grating beam splitters have been fabricated for soft X-ray Mach- Zehnder interferometer using holographic interference lithography. The grating beam splitter consists of two gratings, one works at X-ray laser wavelength of 13.9 nm with the spatial frequency of 1000 lines/mm as the operation grating, the other works at visible wavelength of 632.8 nm for pre-aligning the X-ray interferometer with the spatial frequency of 22 lines/mm as the pre-alignment grating. The two gratings lie vertically on the same substrate. The main feature of the beam splitter is the use of low-spatial- frequency beat grating of a holographic double frequency grating as the pre-alignment grating of the X-ray interferometer. The grating line parallelism between the two gratings can be judged by observing the diffraction patterns of the pre-alignment grating directly.

A scheme for lensless X-ray microscopy combining coherent diffraction imaging and differential corner holography.

PubMed

Capotondi, F; Pedersoli, E; Kiskinova, M; Martin, A V; Barthelmess, M; Chapman, H N

2012-10-22

We successfully use the corners of a common silicon nitride supporting window in lensless X-ray microscopy as extended references in differential holography to obtain a real space hologram of the illuminated object. Moreover, we combine this method with the iterative phasing techniques of coherent diffraction imaging to enhance the spatial resolution on the reconstructed object, and overcome the problem of missing areas in the collected data due to the presence of a beam stop, achieving a resolution close to 85 nm.

Femtosecond X-ray protein nanocrystallography.

PubMed

Chapman, Henry N; Fromme, Petra; Barty, Anton; White, Thomas A; Kirian, Richard A; Aquila, Andrew; Hunter, Mark S; Schulz, Joachim; DePonte, Daniel P; Weierstall, Uwe; Doak, R Bruce; Maia, Filipe R N C; Martin, Andrew V; Schlichting, Ilme; Lomb, Lukas; Coppola, Nicola; Shoeman, Robert L; Epp, Sascha W; Hartmann, Robert; Rolles, Daniel; Rudenko, Artem; Foucar, Lutz; Kimmel, Nils; Weidenspointner, Georg; Holl, Peter; Liang, Mengning; Barthelmess, Miriam; Caleman, Carl; Boutet, Sébastien; Bogan, Michael J; Krzywinski, Jacek; Bostedt, Christoph; Bajt, Saša; Gumprecht, Lars; Rudek, Benedikt; Erk, Benjamin; Schmidt, Carlo; Hömke, André; Reich, Christian; Pietschner, Daniel; Strüder, Lothar; Hauser, Günter; Gorke, Hubert; Ullrich, Joachim; Herrmann, Sven; Schaller, Gerhard; Schopper, Florian; Soltau, Heike; Kühnel, Kai-Uwe; Messerschmidt, Marc; Bozek, John D; Hau-Riege, Stefan P; Frank, Matthias; Hampton, Christina Y; Sierra, Raymond G; Starodub, Dmitri; Williams, Garth J; Hajdu, Janos; Timneanu, Nicusor; Seibert, M Marvin; Andreasson, Jakob; Rocker, Andrea; Jönsson, Olof; Svenda, Martin; Stern, Stephan; Nass, Karol; Andritschke, Robert; Schröter, Claus-Dieter; Krasniqi, Faton; Bott, Mario; Schmidt, Kevin E; Wang, Xiaoyu; Grotjohann, Ingo; Holton, James M; Barends, Thomas R M; Neutze, Richard; Marchesini, Stefano; Fromme, Raimund; Schorb, Sebastian; Rupp, Daniela; Adolph, Marcus; Gorkhover, Tais; Andersson, Inger; Hirsemann, Helmut; Potdevin, Guillaume; Graafsma, Heinz; Nilsson, Björn; Spence, John C H

2011-02-03

X-ray crystallography provides the vast majority of macromolecular structures, but the success of the method relies on growing crystals of sufficient size. In conventional measurements, the necessary increase in X-ray dose to record data from crystals that are too small leads to extensive damage before a diffraction signal can be recorded. It is particularly challenging to obtain large, well-diffracting crystals of membrane proteins, for which fewer than 300 unique structures have been determined despite their importance in all living cells. Here we present a method for structure determination where single-crystal X-ray diffraction 'snapshots' are collected from a fully hydrated stream of nanocrystals using femtosecond pulses from a hard-X-ray free-electron laser, the Linac Coherent Light Source. We prove this concept with nanocrystals of photosystem I, one of the largest membrane protein complexes. More than 3,000,000 diffraction patterns were collected in this study, and a three-dimensional data set was assembled from individual photosystem I nanocrystals (∼200 nm to 2 μm in size). We mitigate the problem of radiation damage in crystallography by using pulses briefer than the timescale of most damage processes. This offers a new approach to structure determination of macromolecules that do not yield crystals of sufficient size for studies using conventional radiation sources or are particularly sensitive to radiation damage.

Nanoepitaxy of GaAs on a Si(001) substrate using a round-hole nanopatterned SiO2 mask.

PubMed

Hsu, Chao-Wei; Chen, Yung-Feng; Su, Yan-Kuin

2012-12-14

GaAs is grown by metal-organic vapor-phase epitaxy on a 55 nm round-hole patterned Si substrate with SiO(2) as a mask. The threading dislocations, which are stacked on the lowest energy facet plane, move along the SiO(2) walls, reducing the number of dislocations. The etching pit density of GaAs on the 55 nm round-hole patterned Si substrate is about 3.3 × 10(5) cm(-2). Compared with the full width at half maximum measurement from x-ray diffraction and photoluminescence spectra of GaAs on a planar Si(001) substrate, those of GaAs on the 55 nm round-hole patterned Si substrate are reduced by 39.6 and 31.4%, respectively. The improvement in material quality is verified by transmission electron microscopy, field-emission scanning electron microscopy, Hall measurements, Raman spectroscopy, photoluminescence, and x-ray diffraction studies.

Experimental strategies for imaging bioparticles with femtosecond hard X-ray pulses

PubMed Central

Okamoto, Kenta; Bielecki, Johan; Maia, Filipe R. N. C.; Mühlig, Kerstin; Seibert, M. Marvin; Hantke, Max F.; Benner, W. Henry; Svenda, Martin; Ekeberg, Tomas; Loh, N. Duane; Pietrini, Alberto; Zani, Alessandro; Rath, Asawari D.; Westphal, Daniel; Kirian, Richard A.; Awel, Salah; Wiedorn, Max O.; van der Schot, Gijs; Carlsson, Gunilla H.; Hasse, Dirk; Sellberg, Jonas A.; Barty, Anton; Andreasson, Jakob; Boutet, Sébastien; Williams, Garth; Koglin, Jason; Hajdu, Janos; Larsson, Daniel S. D.

2017-01-01

This study explores the capabilities of the Coherent X-ray Imaging Instrument at the Linac Coherent Light Source to image small biological samples. The weak signal from small samples puts a significant demand on the experiment. Aerosolized Omono River virus particles of ∼40 nm in diameter were injected into the submicrometre X-ray focus at a reduced pressure. Diffraction patterns were recorded on two area detectors. The statistical nature of the measurements from many individual particles provided information about the intensity profile of the X-ray beam, phase variations in the wavefront and the size distribution of the injected particles. The results point to a wider than expected size distribution (from ∼35 to ∼300 nm in diameter). This is likely to be owing to nonvolatile contaminants from larger droplets during aerosolization and droplet evaporation. The results suggest that the concentration of nonvolatile contaminants and the ratio between the volumes of the initial droplet and the sample particles is critical in such studies. The maximum beam intensity in the focus was found to be 1.9 × 1012 photons per µm2 per pulse. The full-width of the focus at half-maximum was estimated to be 500 nm (assuming 20% beamline transmission), and this width is larger than expected. Under these conditions, the diffraction signal from a sample-sized particle remained above the average background to a resolution of 4.25 nm. The results suggest that reducing the size of the initial droplets during aerosolization is necessary to bring small particles into the scope of detailed structural studies with X-ray lasers. PMID:28512572

Zeta-potential and particle size studies of silver sulphide nanoparticles

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

Sharma, Vikash, E-mail: vikash@csr.res.in; Tarachand,; Ganesan, V.

Silver sulfide (Ag{sub 2}S) nanoparticles (NPs) were prepared successfully for the first time using diethylene glycol (DEG) as a surfactant. X-ray diffraction (XRD) data revealed single phase nature of the compound and energy-dispersive X-ray (EDX) confirmed its nominal composition. Their sizes were 43 nm from XRD, 50 nm from atomic force microscopy (AFM) and 19 nm & 213 nm from dynamic light scattering (DLS); their differences have been discussed. Autotitration study of zeta potential of these NPs in deionized water by DLS at different pH values confirmed an isoelectric point at pH = 5.14 and their very unstable nature in deionized water.

Direct micromachining of quartz glass plates using pulsed laser plasma soft x-rays

NASA Astrophysics Data System (ADS)

Makimura, Tetsuya; Miyamoto, Hisao; Kenmotsu, Youichi; Murakami, Kouichi; Niino, Hiroyuki

2005-03-01

We have investigated direct micromachining of quartz glass, using pulsed laser plasma soft x-rays (LPSXs) having a potential capability of nanomachining because the diffraction limit is ˜10nm. The LPSX's were generated by irradiation of a Ta target with 532nm laser light from a conventional Q switched Nd :YAG laser at 700mJ/pulse. In order to achieve a sufficient power density of LPSX's beyond the ablation threshold, we developed an ellipsoidal mirror to obtain efficient focusing of LPSXs at around 10nm. It was found that quartz glass plates are smoothly ablated at 45nm/shot using the focused and pulsed LPSX's.

Investigation of the nanoscale two-component ZnS-ZnO heterostructures by means of HR-TEM and X-ray based analysis

NASA Astrophysics Data System (ADS)

Pankin, I. A.; Polozhentsev, O. E.; Soldatov, M. A.; Bugaev, A. L.; Tsaturyan, A.; Lomachenko, K. A.; Guda, A. A.; Budnyk, A. P.; Lamberti, C.; Soldatov, A. V.

2018-06-01

This article is devoted to the spectroscopic characterization of ZnS-ZnO nanoscale heterostructures synthesized by the microwave-assisted solvothermal method. The synthesized samples were investigated by means of X-ray powder diffraction (XRPD), high energy resolution fluorescence detected X-ray absorption near-edge-structure (HERFD-XANES) spectroscopy, valence-to-core X-ray emission spectroscopy (VtC-XES) and high resolution transmission electron microscopy (HR-TEM) as well as energy dispersive X-ray spectroscopy (EDX). The average crystallite size estimated by the broadening of XRPD peaks increases from 2.7 nm to 3.7 nm in the temperature range from 100 °C to 150 °C. HR-TEM images show that nanoparticles are arranged in aggregates with the 60-200 nm size. Theoretical estimation shows that the systems synthesized at higher temperatures more prone to the agglomeration. The full profile Reitveld analysis of XRPD data reveals the formation of hexagonal zinc sulfide structure, whereas electron diffraction data reveal also the formation of cubic zinc sulfide and claim the polymorphous character of the system. High energy resolution Zn K-edge XANES data unambiguously demonstrate the presence of a certain amount of the zinc oxide which is likely to have an amorphous structure and could not be detected by XRPD. Qualitative analysis of XANES data allows deriving ZnS/ZnO ratio as a function of synthesis temperature. EDX analysis depicts homogeneous distribution of ZnS and amorphous ZnO phases across the conglomerates. A complementary element-selective valence to core X-ray emission spectroscopy evidences formation of two-component system and confirms estimations of ZnS/ZnO fractions obtained by linear combination fit of XANES data.

Magnetic field effects on ultrafast lattice compression dynamics of Si(111) crystal when excited by linearly-polarized femtosecond laser pulses

NASA Astrophysics Data System (ADS)

Hatanaka, Koji; Odaka, Hideho; Ono, Kimitoshi; Fukumura, Hiroshi

2007-03-01

Time-resolved X-ray diffraction measurements of Si (111) single crystal are performed when excited by linearly-polarized femtosecond laser pulses (780 nm, 260 fs, negatively-chirped, 1 kHz) under a magnetic field (0.47 T). Laser fluence on the sample surface is 40 mJ/cm^2, which is enough lower than the ablation threshold at 200 mJ/cm^2. Probing X-ray pulses of iron characteristic X-ray lines at 0.193604 and 0.193998 nm are generated by focusing femtosecond laser pulses onto audio-cassette tapes in air. Linearly-polarized femtosecond laser pulse irradiation onto Si(111) crystal surface induces transient lattice compression in the picosecond time range, which is confirmed by transient angle shift of X-ray diffraction to higher angles. Little difference of compression dynamics is observed when the laser polarization is changed from p to s-pol. without a magnetic field. On the other hand, under a magnetic field, the lattice compression dynamics changes when the laser is p-polarized which is vertical to the magnetic field vector. These results may be assigned to photo-carrier formation and energy-band distortion.

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

Benkert, A.; Schumacher, C.; Brunner, K.

The authors demonstrate in situ high-resolution x-ray diffraction applied during heteroepitaxy on (001)GaAs for instant layer characterization. The current thickness, composition, strain, and relaxation dynamics of pseudomorphic layers are precisely determined from q{sub z} scans at the (113) reflection measured at a molecular beam epitaxy chamber with a conventional x-ray tube in static geometry. A simple fitting routine enables real-time in situ x-ray diffraction analysis of layers as thin as 20 nm. Critical thicknesses for dislocation formation and plastic relaxation of ZnCdSe layers versus Cd content are determined. The strong influence of substrate temperature on heteroepitaxial nucleation process, deposition rate,more » composition, and strain relaxation dynamics of ZnCdSe on GaAs is also studied.« less

Surfactant-assisted morphological studies of α-Al2O3 nanoparticles

NASA Astrophysics Data System (ADS)

Shah, Janki; Ranjan, Mukesh; Gupta, Sanjeev K.; Sonvane, Yogesh

2018-05-01

The present study deals with the synthesis and characterization of aluminum oxide (Al2O3) nanopowders, it is very useful material as dielectric, ceramic and catalyst. The high-quality nanopowders were obtained by adding surfactants urea and sodium acetate. Further, all characterizations are done for with (urea and sodium acetate) and without surfactant. X-ray diffraction was used to characterize phase formation and the crystallite size of powder while, FTIR gives information about the particle composition and surface intermediates. X-ray diffraction spectra revealed the synthesized nanoparticles phase transformation were γ-Al2O3 to α-Al2O3 phase. Furthermore, the addition of urea and sodium acetate significantly reduced the crystalline size of α-Al2O3 nanoparticles from 43.94 nm to 35.12 nm respectively.

Nanobelt formation of magnesium hydroxide sulfate hydrate via a soft chemistry process.

PubMed

Zhou, Zhengzhi; Sun, Qunhui; Hu, Zeshan; Deng, Yulin

2006-07-13

The nanobelt formation of magnesium hydroxide sulfate hydrate (MHSH) via a soft chemistry approach using carbonate salt and magnesium sulfate as reactants was successfully demonstrated. X-ray diffraction (XRD), energy dispersion X-ray spectra (EDS), selected area electron diffraction (SAED), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) analysis revealed that the MHSH nanobelts possessed a thin belt structure (approximately 50 nm in thickness) and a rectangular cross profile (approximately 200 nm in width). The MHSH nanobelts suffered decomposition under electron beam irradiation during TEM observation and formed MgO with the pristine nanobelt morphology preserved. The formation process of the MHSH nanobelts was studied by tracking the morphology of the MHSH nanobelts during the reaction. A possible chemical reaction mechanism is proposed.

Structural and optical properties of CuS thin films deposited by Thermal co-evaporation

NASA Astrophysics Data System (ADS)

Sahoo, A. K.; Mohanta, P.; Bhattacharyya, A. S.

2015-02-01

Copper sulfide (CuS) thin films with thickness 100, 150 and 200 nm have been deposited on glass substrates by thermal co-evaporation of Copper and Sulphur. The effect of CuS film thickness on the structural and optical properties have investigated and discussed. Structural and optical investigations of the films were carried out by X-ray diffraction, atomic force microscopy, high-resolution transmission electron microscopy and UV spectroscopy. XRD and selected area electron diffraction conforms that polycrystalline in nature with hexagonal crystal structure. AFM studies revealed a smooth surface morphology with root mean-square roughness values increases from 24 nm to 42 nm as the film thickness increase from 100 nm to 200 nm. AFM image showed that grain size increases with thickness of film increases and good agreement with the calculated from full width half maximum of the X-ray diffraction peak using Scherrer's formula and Williamson-Hall plot. The absorbance of the thin films were absorbed decreases with wavelength through UV-visible regions but showed a increasing in the near-infrared regions. The reflectance spectra also showed lower reflectance peak (25% to 32%) in visible region and high reflectance peak (49 % to 54 %) in near-infrared region. These high absorbance films made them for photo-thermal conversion of solar energy.

Measuring the X-ray Resolving Power of Bent Potassium Acid Phthalate Diffraction Crystals

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

Haugh, M. J.; Wu, M.; Jacoby, K. D.

2014-11-01

This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals thatmore » we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories (SNL) in Albuquerque, NM. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a dual goniometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.« less

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

PubMed

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

2015-06-16

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

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

PubMed Central

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

2013-01-01

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

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

PubMed

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

2013-08-01

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

X ray reflection masks: Manufacturing, characterization and first tests

NASA Astrophysics Data System (ADS)

Rahn, Stephen

1992-09-01

SXPL (Soft X-ray Projection Lithography) multilayer mirrors are characterized, laterally structured and then used as reflection masks in a projecting lithography procedure. Mo/Si-multilayer mirrors with a 2d in the region of 14 nm were characterized by Cu-k(alpha) grazing incidence as well as soft X-ray normal incidence reflectivity measurements. The multilayer mirrors were patterned by reactive ion etching with CF4 using a photoresist as etch mask, thus producing X-ray reflection masks. The masks were tested at the synchrotron radiation laboratory of the electron accelerator ELSA. A double crystal X-ray monochromator was modified so as to allow about 0.5 sq cm of the reflection mask to be illuminated by white synchrotron radiation. The reflected patterns were projected (with an energy of 100 eV) onto a resist and structure sizes down to 8 micrometers were nicely reproduced. Smaller structures were distorted by Fresnel-diffraction. The theoretically calculated diffraction images agree very well with the observed images.

Preparation and physical properties of polycrystalline (Bi1-xPbx)2Sr2Ca2Cu3Oy high T c superconductors

NASA Astrophysics Data System (ADS)

Awan, M. S.; Maqsood, M.; Mirza, S. A.; Yousaf, M.; Maqsood, A.

1995-02-01

(Bi1-xPbx:)2Sr2Ca2Cu3Oy ( x = 0.3) high critical transition temperature ( T c) superconductors are synthesized by the solid-state reaction method in polycrystalline form. X-ray diffraction (XRD) studies, direct current (dc) electrical resistivity measurements, scanning electron microscopic (SEM) studies, critical current density measurements, and zero-field alternating current (ac) susceptibility measurements are performed to investigate the physical changes, structural changes, and magnetic behavior of the superconducting samples. X-ray diffraction studies show that a high T c phase exists with orthorhombic symmetry in the specimen. According to the XRD data, the lattice parameters of the high T c phase were determined as a = 0.537(1) nm, b = 0.539(1) nm, and c = 3.70(1) nm. The compound exhibits a superconducting transition at 106 ±1 K for zero resistance. The ac susceptibility measurements in zero field confirm the dc electrical resistivity results; hence both support the XRD results. The particle size and structural changes as a function of the cold-pressing and aging effect are also reported.

Optics for coherent X-ray applications

PubMed Central

Yabashi, Makina; Tono, Kensuke; Mimura, Hidekazu; Matsuyama, Satoshi; Yamauchi, Kazuto; Tanaka, Takashi; Tanaka, Hitoshi; Tamasaku, Kenji; Ohashi, Haruhiko; Goto, Shunji; Ishikawa, Tetsuya

2014-01-01

Developments of X-ray optics for full utilization of diffraction-limited storage rings (DLSRs) are presented. The expected performance of DLSRs is introduced using the design parameters of SPring-8 II. To develop optical elements applicable to manipulation of coherent X-rays, advanced technologies on precise processing and metrology were invented. With propagation-based coherent X-rays at the 1 km beamline of SPring-8, a beryllium window fabricated with the physical-vapour-deposition method was found to have ideal speckle-free properties. The elastic emission machining method was utilized for developing reflective mirrors without distortion of the wavefronts. The method was further applied to production of diffraction-limited focusing mirrors generating the smallest spot size in the sub-10 nm regime. To enable production of ultra-intense nanobeams at DLSRs, a low-vibration cooling system for a high-heat-load monochromator and advanced diagnostic systems to characterize X-ray beam properties precisely were developed. Finally, new experimental schemes for combinative nano-analysis and spectroscopy realised with novel X-ray optics are discussed. PMID:25177986

Coherent X-ray diffraction from collagenous soft tissues

PubMed Central

Berenguer de la Cuesta, Felisa; Wenger, Marco P. E.; Bean, Richard J.; Bozec, Laurent; Horton, Michael A.; Robinson, Ian K.

2009-01-01

Coherent X-ray diffraction has been applied in the imaging of inorganic materials with great success. However, its application to biological specimens has been limited to some notable exceptions, due to the induced radiation damage and the extended nature of biological samples, the last limiting the application of most part of the phasing algorithms. X-ray ptychography, still under development, is a good candidate to overcome such difficulties and become a powerful imaging method for biology. We describe herein the feasibility of applying ptychography to the imaging of biological specimens, in particular collagen rich samples. We report here speckles in diffraction patterns from soft animal tissue, obtained with an optimized small angle X-ray setup that exploits the natural coherence of the beam. By phasing these patterns, dark field images of collagen within tendon, skin, bone, or cornea will eventually be obtained with a resolution of 60–70 nm. We present simulations of the contrast mechanism in collagen based on atomic force microscope images of the samples. Simulations confirmed the ‘speckled’ nature of the obtained diffraction patterns. Once inverted, the patterns will show the disposition and orientation of the fibers within the tissue, by enhancing the phase contrast between protein and no protein regions of the sample. Our work affords the application of the most innovative coherent X-ray diffraction tools to the study of biological specimens, and this approach will have a significant impact in biology and medicine because it overcomes many of the limits of current microscopy techniques. PMID:19706395

Coherent X-ray diffraction from collagenous soft tissues.

PubMed

Berenguer de la Cuesta, Felisa; Wenger, Marco P E; Bean, Richard J; Bozec, Laurent; Horton, Michael A; Robinson, Ian K

2009-09-08

Coherent X-ray diffraction has been applied in the imaging of inorganic materials with great success. However, its application to biological specimens has been limited to some notable exceptions, due to the induced radiation damage and the extended nature of biological samples, the last limiting the application of most part of the phasing algorithms. X-ray ptychography, still under development, is a good candidate to overcome such difficulties and become a powerful imaging method for biology. We describe herein the feasibility of applying ptychography to the imaging of biological specimens, in particular collagen rich samples. We report here speckles in diffraction patterns from soft animal tissue, obtained with an optimized small angle X-ray setup that exploits the natural coherence of the beam. By phasing these patterns, dark field images of collagen within tendon, skin, bone, or cornea will eventually be obtained with a resolution of 60-70 nm. We present simulations of the contrast mechanism in collagen based on atomic force microscope images of the samples. Simulations confirmed the 'speckled' nature of the obtained diffraction patterns. Once inverted, the patterns will show the disposition and orientation of the fibers within the tissue, by enhancing the phase contrast between protein and no protein regions of the sample. Our work affords the application of the most innovative coherent X-ray diffraction tools to the study of biological specimens, and this approach will have a significant impact in biology and medicine because it overcomes many of the limits of current microscopy techniques.

Studying Pulsed Laser Deposition conditions for Ni/C-based multi-layers

NASA Astrophysics Data System (ADS)

Bollmann, Tjeerd R. J.

2018-04-01

Nickel carbon based multi-layers are a viable route towards future hard X-ray and soft γ-ray focusing telescopes. Here, we study the Pulsed Laser Deposition growth conditions of such bilayers by Reflective High Energy Electron Diffraction, X-ray Reflectivity and Diffraction, Atomic Force Microscopy, X-ray Photoelectron Spectroscopy and cross-sectional Transmission Electron Microscopy analysis, with emphasis on optimization of process pressure and substrate temperature during growth. The thin multi-layers are grown on a treated SiO substrate resulting in Ni and C layers with surface roughnesses (RMS) of ≤0.2 nm. Small droplets resulting during melting of the targets surface increase the roughness, however, and cannot be avoided. The sequential process at temperatures beyond 300 °C results into intermixing between the two layers, being destructive for the reflectivity of the multi-layer.

Structural analysis of aluminium substituted nickel ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Singh, H. S.; Sangwa, Neha

2018-05-01

Aluminium substituted nickel ferrite nanoparticles were synthesized by High Energy Ball milling (HEBM) of the mixture of α-NiO, α-Al2O3 and α-Fe2O3 followed by annealing at 1000˚C. X-ray diffraction (XRD) and Energy dispersive spectroscopy analysis (EDS) characterization was done for Aluminium substituted nickel ferrite. The structural analysis reveals the formation of the single phase compound. The average grain size was estimated by X-ray diffraction technique ranges from 30 to 10 nm with the increasing concentration of Aluminium. EDS spectra conforms the homogeneous mixing and purity of ferrite.

Growth and characterization of organic NLO material: Clobetasol propionate

NASA Astrophysics Data System (ADS)

Purusothaman, R.; Rajesh, P.; Ramasamy, P.

2015-06-01

Single crystals of clobetasol propionate (CP) have been grown by slow evaporation solution technique using mixed solvent of methanol-acetone. The grown crystals were subjected to single crystal X-ray diffraction analysis to confirm their lattice parameter and space group. The powder X-ray diffraction pattern of the grown CP has been indexed. Thermal analysis was performed to study the thermal stability of the grown crystals. Photoluminescence spectrum shows broad emission peak observed at 421 nm. Nonlinear optical studies were carried out for the grown crystal and second harmonic generation (SHG) efficiency was found in the crystal.

Characterization of sodium phenytoin co-gelled with titania for a controlled drug-release system

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

Lopez, T.; Instituto Nacional de Neurologia y Neurocirugia 'MVS', Av. Insurgentes Sur 3877. Col. La Fama. P.O. Box 14269 Mexico D. F.; Quintana, P.

2007-08-15

Sodium phenytoin, C{sub 15}H{sub 11}N{sub 2}NaO{sub 2}, in several concentrations was co-gelled with titania (TiO{sub 2}), by a sol-gel process. This technique is a promising method to encapsulate several drugs, in this case, phenytoin is an anticonvulsant used to control epileptic seizures. Samples were prepared by adding different concentrations (X = 50, 100, 200 and 250 mg per 20 g of titania matrix) of sodium phenytoin (Ph) to a solution of titanium n-butoxide. The resulting titania-Ph-X materials were characterized by transmission electron microscopy (TEM), Fourier transformed infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and Brunauer-Emmet-Teller (BET) surface areas. The porous nanomaterialsmore » showed a wide range of particle size, from 10 to 210 nm, with a mean pore diameter of 5 nm. X-ray diffraction showed an amorphous structure of the prepared samples.« less

X-Ray diffraction and resonance shear measurement of nano-confined ionic liquids.

PubMed

Tomita, Kazuhito; Mizukami, Masashi; Nakano, Shinya; Ohta, Noboru; Yagi, Naoto; Kurihara, Kazue

2018-05-23

X-ray diffraction measurement at the SPring-8 synchrotron was employed to investigate the structures of two types of imidazolium-based ionic liquids (ILs), 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide ([C4mim][NTF2]) and 1-butyl-3-methylimidazolium tetrafluoroborate ([C4mim][BF4]), confined between silica surfaces by varying the surface separation distances of ca. 500 nm (bulk liquid), ca. 10 nm, and ca. 2 nm (hard wall thickness). The obtained diffraction profiles and intensities were discussed by considering the structures and properties of the nano-confined ILs between the silica surfaces investigated by resonance shear measurement (RSM) and molecular dynamics simulation (MD) in our previous reports. [C4mim][NTf2] showed two diffraction peaks at q = 8.8 nm-1 (spacing d = 0.71 nm) and at q = 14.0 nm-1 (spacing d = 0.45 nm) at the greatest distance (D = ca. 500 nm), which were assigned to the interval between the same ions (anion-anion or cation-cation) within the polar network of [C4mim][NTf2] and the interval between the neighboring anion-cation, respectively. The positions of these two peaks remained the same at D = ca. 10 nm and at the hard wall (D = ca. 2 nm) and their intensity factor increased, indicating that both the cation and anion existed in the same layer. This result was consistent with the checkerboard structure of [C4mim][NTf2] on the silica surface computer simulated in our previous studies. On the other hand, [C4mim][BF4] showed a peak at q = 15.4 nm-1 (spacing d = 0.41 nm) corresponding to the anion-cation interval at the greatest distance (D = ca. 500 nm). This peak became broader and weaker at D = ca. 12 nm and at D = ca. 2 nm.

Single-particle coherent diffractive imaging with a soft x-ray free electron laser: towards soot aerosol morphology

NASA Astrophysics Data System (ADS)

Bogan, Michael J.; Starodub, Dmitri; Hampton, Christina Y.; Sierra, Raymond G.

2010-10-01

The first of its kind, the Free electron LASer facility in Hamburg, FLASH, produces soft x-ray pulses with unprecedented properties (10 fs, 6.8-47 nm, 1012 photons per pulse, 20 µm diameter). One of the seminal FLASH experiments is single-pulse coherent x-ray diffractive imaging (CXDI). CXDI utilizes the ultrafast and ultrabright pulses to overcome resolution limitations in x-ray microscopy imposed by x-ray-induced damage to the sample by 'diffracting before destroying' the sample on sub-picosecond timescales. For many lensless imaging algorithms used for CXDI it is convenient when the data satisfy an oversampling constraint that requires the sample to be an isolated object, i.e. an individual 'free-standing' portion of disordered matter delivered to the centre of the x-ray focus. By definition, this type of matter is an aerosol. This paper will describe the role of aerosol science methodologies used for the validation of the 'diffract before destroy' hypothesis and the execution of the first single-particle CXDI experiments being developed for biological imaging. FLASH CXDI now enables the highest resolution imaging of single micron-sized or smaller airborne particulate matter to date while preserving the native substrate-free state of the aerosol. Electron microscopy offers higher resolution for single-particle analysis but the aerosol must be captured on a substrate, potentially modifying the particle morphology. Thus, FLASH is poised to contribute significant advancements in our knowledge of aerosol morphology and dynamics. As an example, we simulate CXDI of combustion particle (soot) morphology and introduce the concept of extracting radius of gyration of fractal aggregates from single-pulse x-ray diffraction data. Future upgrades to FLASH will enable higher spatially and temporally resolved single-particle aerosol dynamics studies, filling a critical technological need in aerosol science and nanotechnology. Many of the methodologies described for FLASH will directly translate to use at hard x-ray free electron lasers.

Femtosecond X-ray protein nanocrystallography

PubMed Central

Chapman, Henry N.; Fromme, Petra; Barty, Anton; White, Thomas A.; Kirian, Richard A.; Aquila, Andrew; Hunter, Mark S.; Schulz, Joachim; DePonte, Daniel P.; Weierstall, Uwe; Doak, R. Bruce; Maia, Filipe R. N. C.; Martin, Andrew V.; Schlichting, Ilme; Lomb, Lukas; Coppola, Nicola; Shoeman, Robert L.; Epp, Sascha W.; Hartmann, Robert; Rolles, Daniel; Rudenko, Artem; Foucar, Lutz; Kimmel, Nils; Weidenspointner, Georg; Holl, Peter; Liang, Mengning; Barthelmess, Miriam; Caleman, Carl; Boutet, Sébastien; Bogan, Michael J.; Krzywinski, Jacek; Bostedt, Christoph; Bajt, Saša; Gumprecht, Lars; Rudek, Benedikt; Erk, Benjamin; Schmidt, Carlo; Hömke, André; Reich, Christian; Pietschner, Daniel; Strüder, Lothar; Hauser, Günter; Gorke, Hubert; Ullrich, Joachim; Herrmann, Sven; Schaller, Gerhard; Schopper, Florian; Soltau, Heike; Kühnel, Kai-Uwe; Messerschmidt, Marc; Bozek, John D.; Hau-Riege, Stefan P.; Frank, Matthias; Hampton, Christina Y.; Sierra, Raymond G.; Starodub, Dmitri; Williams, Garth J.; Hajdu, Janos; Timneanu, Nicusor; Seibert, M. Marvin; Andreasson, Jakob; Rocker, Andrea; Jönsson, Olof; Svenda, Martin; Stern, Stephan; Nass, Karol; Andritschke, Robert; Schröter, Claus-Dieter; Krasniqi, Faton; Bott, Mario; Schmidt, Kevin E.; Wang, Xiaoyu; Grotjohann, Ingo; Holton, James M.; Barends, Thomas R. M.; Neutze, Richard; Marchesini, Stefano; Fromme, Raimund; Schorb, Sebastian; Rupp, Daniela; Adolph, Marcus; Gorkhover, Tais; Andersson, Inger; Hirsemann, Helmut; Potdevin, Guillaume; Graafsma, Heinz; Nilsson, Björn; Spence, John C. H.

2012-01-01

X-ray crystallography provides the vast majority of macromolecular structures, but the success of the method relies on growing crystals of sufficient size. In conventional measurements, the necessary increase in X-ray dose to record data from crystals that are too small leads to extensive damage before a diffraction signal can be recorded1-3. It is particularly challenging to obtain large, well-diffracting crystals of membrane proteins, for which fewer than 300 unique structures have been determined despite their importance in all living cells. Here we present a method for structure determination where single-crystal X-ray diffraction ‘snapshots’ are collected from a fully hydrated stream of nanocrystals using femtosecond pulses from a hard-X-ray free-electron laser, the Linac Coherent Light Source4. We prove this concept with nanocrystals of photosystem I, one of the largest membrane protein complexes5. More than 3,000,000 diffraction patterns were collected in this study, and a three-dimensional data set was assembled from individual photosystem I nanocrystals (~200 nm to 2 μm in size). We mitigate the problem of radiation damage in crystallography by using pulses briefer than the timescale of most damage processes6. This offers a new approach to structure determination of macromolecules that do not yield crystals of sufficient size for studies using conventional radiation sources or are particularly sensitive to radiation damage. PMID:21293373

A Medipix quantum area detector allows rotation electron diffraction data collection from submicrometre three-dimensional protein crystals

PubMed Central

Nederlof, Igor; van Genderen, Eric; Li, Yao-Wang; Abrahams, Jan Pieter

2013-01-01

When protein crystals are submicrometre-sized, X-ray radiation damage precludes conventional diffraction data collection. For crystals that are of the order of 100 nm in size, at best only single-shot diffraction patterns can be collected and rotation data collection has not been possible, irrespective of the diffraction technique used. Here, it is shown that at a very low electron dose (at most 0.1 e− Å−2), a Medipix2 quantum area detector is sufficiently sensitive to allow the collection of a 30-frame rotation series of 200 keV electron-diffraction data from a single ∼100 nm thick protein crystal. A highly parallel 200 keV electron beam (λ = 0.025 Å) allowed observation of the curvature of the Ewald sphere at low resolution, indicating a combined mosaic spread/beam divergence of at most 0.4°. This result shows that volumes of crystal with low mosaicity can be pinpointed in electron diffraction. It is also shown that strategies and data-analysis software (MOSFLM and SCALA) from X-ray protein crystallography can be used in principle for analysing electron-diffraction data from three-dimensional nanocrystals of proteins. PMID:23793148

A Next-Generation Hard X-Ray Nanoprobe Beamline for In Situ Studies of Energy Materials and Devices

NASA Astrophysics Data System (ADS)

Maser, Jörg; Lai, Barry; Buonassisi, Tonio; Cai, Zhonghou; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Jacobsen, Chris; Preissner, Curt; Roehrig, Chris; Rose, Volker; Shu, Deming; Vine, David; Vogt, Stefan

2014-01-01

The Advanced Photon Source is developing a suite of new X-ray beamlines to study materials and devices across many length scales and under real conditions. One of the flagship beamlines of the APS upgrade is the In Situ Nanoprobe (ISN) beamline, which will provide in situ and operando characterization of advanced energy materials and devices under varying temperatures, gas ambients, and applied fields, at previously unavailable spatial resolution and throughput. Examples of materials systems include inorganic and organic photovoltaic systems, advanced battery systems, fuel cell components, nanoelectronic devices, advanced building materials and other scientifically and technologically relevant systems. To characterize these systems at very high spatial resolution and trace sensitivity, the ISN will use both nanofocusing mirrors and diffractive optics to achieve spots sizes as small as 20 nm. Nanofocusing mirrors in Kirkpatrick-Baez geometry will provide several orders of magnitude increase in photon flux at a spatial resolution of 50 nm. Diffractive optics such as zone plates and/or multilayer Laue lenses will provide a highest spatial resolution of 20 nm. Coherent diffraction methods will be used to study even small specimen features with sub-10 nm relevant length scale. A high-throughput data acquisition system will be employed to significantly increase operations efficiency and usability of the instrument. The ISN will provide full spectroscopy capabilities to study the chemical state of most materials in the periodic table, and enable X-ray fluorescence tomography. In situ electrical characterization will enable operando studies of energy and electronic devices such as photovoltaic systems and batteries. We describe the optical concept for the ISN beamline, the technical design, and the approach for enabling a broad variety of in situ studies. We furthermore discuss the application of hard X-ray microscopy to study defects in multi-crystalline solar cells, one of the lines of inquiries for which the ISN is being developed.

Optical and structural properties of CsI thin film photocathode

NASA Astrophysics Data System (ADS)

Triloki; Rai, R.; Singh, B. K.

2015-06-01

In the present work, the performance of a cesium iodide thin film photocathode is studied in detail. The optical absorbance of cesium iodide films has been analyzed in the spectral range from 190 nm to 900 nm. The optical band gap energy of 500 nm thick cesium iodide film is calculated from the absorbance data using a Tauc plot. The refractive index is estimated from the envelope plot of transmittance data using Swanepoel's method. The absolute quantum efficiency measurement has been carried out in the wavelength range from 150 nm to 200 nm. The crystallographic nature and surface morphology are investigated by X-ray diffraction and transmission electron microscopy techniques. In addition, the elemental composition result obtained by energy dispersive X-ray analysis is also reported in the present work.

Room Temperature Ferromagnetism of Fe Doped Indium Tin Oxide Based on Dispersed Fe3O4 Nanoparticles

NASA Astrophysics Data System (ADS)

Okada, Koichi; Kohiki, Shigemi; Nishi, Sachio; Shimooka, Hirokazu; Deguchi, Hiroyuki; Mitome, Masanori; Bando, Yoshio; Shishido, Toetsu

2007-09-01

Transmission electron microscopy revealed that Fe3O4 nanoparticles with diameter of ≈200 nm dispersed in Fe doped indium tin oxide (Fe@ITO) powders exhibiting co-occurrence of room temperature ferromagnetism and superparamagnetism. Although we observed no X-ray diffraction peak from Fe related compounds for Fe0.19@ITO (ITO: In1.9Sn0.1O3) powders, the powders showed both hysteresis loop in field dependent magnetization at 300 K and divergence of zero-field-cooled magnetization from field-cooled magnetization. Scanning transmission electron microscopy with energy dispersive X-ray spectroscopy demonstrated that the nanoparticle with diameter of ≈200 nm consists of Fe and oxygen. Transmission electron diffraction revealed that crystal structure of the nanoparticle is inverse spinel type Fe3O4. The Fe3O4 crystalline phase by electron diffraction is consistent with the saturation magnetization of 1.3 μB/Fe and magnetic anomaly at ≈110 K observed for the powders.

Diffraction data of core-shell nanoparticles from an X-ray free electron laser

DOE PAGES

Li, Xuanxuan; Chiu, Chun -Ya; Wang, Hsiang -Ju; ...

2017-04-11

X-ray free-electron lasers provide novel opportunities to conduct single particle analysis on nanoscale particles. Coherent diffractive imaging experiments were performed at the Linac Coherent Light Source (LCLS), SLAC National Laboratory, exposing single inorganic core-shell nanoparticles to femtosecond hard-X-ray pulses. Each facetted nanoparticle consisted of a crystalline gold core and a differently shaped palladium shell. Scattered intensities were observed up to about 7 nm resolution. Analysis of the scattering patterns revealed the size distribution of the samples, which is consistent with that obtained from direct real-space imaging by electron microscopy. Furthermore, scattering patterns resulting from single particles were selected and compiledmore » into a dataset which can be valuable for algorithm developments in single particle scattering research.« less

Ultrathin IBAD MgO films for epitaxial growth on amorphous substrates and sub-50 nm membranes

DOE PAGES

Wang, Siming; Antonakos, C.; Bordel, C.; ...

2016-11-07

Here, a fabrication process has been developed for high energy ion beam assisted deposition (IBAD) biaxial texturing of ultrathin (~1 nm) MgO films, using a high ion-to-atom ratio and post-deposition annealing instead of a homoepitaxial MgO layer. These films serve as the seed layer for epitaxial growth of materials on amorphous substrates such as electron/X-ray transparent membranes or nanocalorimetry devices. Stress measurements and atomic force microscopy of the MgO films reveal decreased stress and surface roughness, while X-ray diffraction of epitaxial overlayers demonstrates the improved crystal quality of films grown epitaxially on IBAD MgO. The process simplifies the synthesis ofmore » IBAD MgO, fundamentally solves the “wrinkle” issue induced by the homoepitaxial layer on sub-50 nm membranes, and enables studies of epitaxial materials in electron/X-ray transmission and nanocalorimetry.« less

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.

Characterization of nanodimensional Ni-Zn ferrite prepared by mechanochemical and thermal methods

NASA Astrophysics Data System (ADS)

Manova, E.; Paneva, D.; Kunev, B.; Rivière, E.; Estournès, C.; Mitov, I.

2010-03-01

Nickel zinc ferrite nanoparticles, Ni1-xZnxFe2O4 (x = 0, 0.2, 0.5, 0.8, 1.0), with dimensions below 10 nm have been prepared by combining chemical precipitation with high-energy ball milling. For comparison, their analogues obtained by thermal synthesis have also been studied. Mössbauer spectroscopy, X-ray diffraction, and magnetic measurements are used for the characterization of the obtained materials. X-ray diffraction shows that after 3h of mechanical treatment ferrites containing zinc are formed, while 6h of treatment is needed to obtain NiFe2O4. The magnetic properties of the samples exhibit a strong dependence on the phase composition, particle size and preparation method.

Structural transformation in nano-structured CuAl{sub x}Cr{sub x}Fe{sub 2-2x}O{sub 4} system

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

Mehta, D. K., E-mail: daxabjoshi@gmail.com; Chhantbar, M. C.; Joshi, H. H.

Polycrystalline spinel ferrite system CuAl{sub x}Cr{sub x}Fe{sub 2-2x}O{sub 4} (x=0.2, 0.6) was synthesized by solid-state reaction route. Nanoparticles of the samples have been prepared by using high energy ball milling technique with different milling durations and characterized by X-ray Diffraction and Tunneling Electron Microscope. It is observed that the structural transformation occurred from Cubic to tetragonal and particle size varied between 29 nm -14 nm with increase of milling time.

Hydrothermal synthesis of tungsten doped tin dioxide nanocrystals

NASA Astrophysics Data System (ADS)

Zhou, Cailong; Li, Yufeng; Chen, Yiwen; Lin, Jing

2018-01-01

Tungsten doped tin dioxide (WTO) nanocrystals were synthesized through a one-step hydrothermal method. The structure, composition and morphology of WTO nanocrystals were characterized by x-ray diffraction, x-ray photoelectron spectroscopy, energy dispersive x-ray spectroscopy, UV-vis diffuse reflectance spectra, zeta potential analysis and high-resolution transmission electron microscopy. Results show that the as-prepared WTO nanocrystals were rutile-type structure with the size near 13 nm. Compared with the undoped tin dioxide nanocrystals, the WTO nanocrystals possessed better dispersity in ethanol phase and formed transparent sol.

Epitaxial graphene-encapsulated surface reconstruction of Ge(110)

NASA Astrophysics Data System (ADS)

Campbell, Gavin P.; Kiraly, Brian; Jacobberger, Robert M.; Mannix, Andrew J.; Arnold, Michael S.; Hersam, Mark C.; Guisinger, Nathan P.; Bedzyk, Michael J.

2018-04-01

Understanding and engineering the properties of crystalline surfaces has been critical in achieving functional electronics at the nanoscale. Employing scanning tunneling microscopy, surface x-ray diffraction, and high-resolution x-ray reflectivity experiments, we present a thorough study of epitaxial graphene (EG)/Ge(110) and report a Ge(110) "6 × 2" reconstruction stabilized by the presence of epitaxial graphene unseen in group-IV semiconductor surfaces. X-ray studies reveal that graphene resides atop the surface reconstruction with a 0.34 nm van der Waals (vdW) gap and provides protection from ambient degradation.

Conformational landscape of a virus by single-particle X-ray scattering

DOE PAGES

Hosseinizadeh, Ahmad; Mashayekhi, Ghoncheh; Copperman, Jeremy; ...

2017-08-14

Using a manifold-based analysis of experimental diffraction snapshots from an X-ray free electron laser, we determine the three-dimensional structure and conformational landscape of the PR772 virus to a detector-limited resolution of 9 nm. Our results indicate that a single conformational coordinate controls reorganization of the genome, growth of a tubular structure from a portal vertex and release of the genome. Furthermore, these results demonstrate that single-particle X-ray scattering has the potential to shed light on key biological processes.

X-ray focusing with efficient high-NA multilayer Laue lenses

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

Bajt, Sasa; Prasciolu, Mauro; Fleckenstein, Holger

Multilayer Laue lenses are volume diffraction elements for the efficient focusing of X-rays. With a new manufacturing technique that we introduced, it is possible to fabricate lenses of sufficiently high numerical aperture (NA) to achieve focal spot sizes below 10 nm. The alternating layers of the materials that form the lens must span a broad range of thicknesses on the nanometer scale to achieve the necessary range of X-ray deflection angles required to achieve a high NA. This poses a challenge to both the accuracy of the deposition process and the control of the materials properties, which often vary withmore » layer thickness. We introduced a new pair of materials—tungsten carbide and silicon carbide—to prepare layered structures with smooth and sharp interfaces and with no material phase transitions that hampered the manufacture of previous lenses. Using a pair of multilayer Laue lenses (MLLs) fabricated from this system, we achieved a two-dimensional focus of 8.4 × 6.8 nm 2 at a photon energy of 16.3 keV with high diffraction efficiency and demonstrated scanning-based imaging of samples with a resolution well below 10 nm. The high NA also allowed projection holographic imaging with strong phase contrast over a large range of magnifications. Furthermore, an error analysis indicates the possibility of achieving 1 nm focusing.« less

X-ray focusing with efficient high-NA multilayer Laue lenses

DOE PAGES

Bajt, Sasa; Prasciolu, Mauro; Fleckenstein, Holger; ...

2018-03-23

Multilayer Laue lenses are volume diffraction elements for the efficient focusing of X-rays. With a new manufacturing technique that we introduced, it is possible to fabricate lenses of sufficiently high numerical aperture (NA) to achieve focal spot sizes below 10 nm. The alternating layers of the materials that form the lens must span a broad range of thicknesses on the nanometer scale to achieve the necessary range of X-ray deflection angles required to achieve a high NA. This poses a challenge to both the accuracy of the deposition process and the control of the materials properties, which often vary withmore » layer thickness. We introduced a new pair of materials—tungsten carbide and silicon carbide—to prepare layered structures with smooth and sharp interfaces and with no material phase transitions that hampered the manufacture of previous lenses. Using a pair of multilayer Laue lenses (MLLs) fabricated from this system, we achieved a two-dimensional focus of 8.4 × 6.8 nm 2 at a photon energy of 16.3 keV with high diffraction efficiency and demonstrated scanning-based imaging of samples with a resolution well below 10 nm. The high NA also allowed projection holographic imaging with strong phase contrast over a large range of magnifications. Furthermore, an error analysis indicates the possibility of achieving 1 nm focusing.« less

Investigations on structural and photoluminescence mechanism of cerium doped L-Histidine hydrochloride mono hydrate single crystals for optical applications

NASA Astrophysics Data System (ADS)

Rajyalakshmi, S.; Ramachandra Rao, K.; Brahmaji, B.; Samatha, K.; Visweswara Rao, T. K.; Ramakrishna, Y.

2017-02-01

Semi organic nonlinear optical material of Ce3+ ion added L-Histidine hydrochloride monohydrate (LHHC) crystals have been grown successfully by the slow evaporation solution technique (SEST) as well as Sankaranarayanan-Ramasamy (SR) technique. Unit cell data have been measured from the single crystal X-ray diffraction analysis and High resolution X-ray diffraction analysis (HRXRD) study shows relatively a good crystalline perfection. Fourier transform infra-red spectroscopy (FTIR) spectra indicates that the Ce3+ ion is coordinated with carboxylate group of grown crystal. The lower UV-cutoff wavelength of the incorporation of Ce3+ ion in LHHC is 240 nm. The incorporation of Ce3+ ion in the crystal lattice was observed by energy dispersive X-ray analysis (EDAX). The nonlinear optical (NLO) efficiency of SR-grown crystal is 3.7 times greater with respect to potassium dihydrogen phosphate (KDP). We report first-time the photoluminescence (PL) mechanism of emission spectrum, which shows broad band located at 350 nm corresponding to 5d → 4f transition of Ce3+ ion and excited by 250 nm wavelength. The excitation spectrum shows a band at 258 nm due to the 4f → 5d transition of Ce3+ ion. The nature of decay curve of the grown crystal is bi-exponential with a long life time of τ2 is 8.8270 μs.

Interaction of atomic oxygen with thin film and bulk copper: An XPS, AES, XRD, and profilometer study

NASA Technical Reports Server (NTRS)

Raikar, Genesh N.; Gregory, John C.; Christl, Ligia C.; Peters, Palmer N.

1992-01-01

The University of Alabama in Huntsville (UAH) experiment A-0114 was designed primarily to study degradation of material surfaces due to low earth orbital (LEO) atmospheric oxygen. The experiment contained 128 one inch circular samples: metals, polymers, carbons, and semiconductors. Among metal samples, copper has shown some interesting new results. Two types of copper samples, a film sputter coated on fused silica and a bulk piece of OFHC copper, were characterized employing a variety of techniques such as X-ray and Auger electron spectroscopies, X-ray diffraction, and high resolution profilometry. Cu 2p core level spectra were used to characterize the presence of Cu2O and CuO in addition to Cu Auger LMM lines. These results are supported by our recent X-ray diffraction studies which clearly establish the presence of Cu oxides which we were unable to prove in our earlier work. Profilometry showed an increase in thickness of the film sample where exposed to 106.7 +/- 0.5 nm from an initial thickness of 74.2 +/- 1.1 nm. Further studies with SEM and ellipsometry are underway.

Sonochemical fabrication of 8-hydroxyquinoline aluminum (Alq3) nanoflowers with high electrogenerated chemiluminescence.

PubMed

Mao, Chang-Jie; Wang, Dan-Chen; Pan, Hong-Cheng; Zhu, Jun-Jie

2011-03-01

Well-defined Alq(3) nanoflowers were fabricated via a facile and fast sonochemical route. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the structure and shape of the as-prepared product. The results showed that the resulting Alq(3) was composed of nanobelts with thickness about 50 nm, average widths of 200 nm, and length up to 10 μm. The Alq(3) nanoflowers exhibited good electrogenerated chemiluminescence behavior. Copyright © 2010 Elsevier B.V. All rights reserved.

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

Jung, Min-Cherl; Zhang, Dongrong; Nikiforov, Gueorgui O.

Ultrathin (<6 nm) polycrystalline films of 6,13-bis(triisopropylsilylethynyl) pentacene (TIPS-P) are deposited with a two-step spin-coating process. The influence of spin-coating conditions on morphology of the resulting film was examined by atomic force microscopy. Film thickness and RMS surface roughness were in the range of 4.0–6.1 and 0.6–1.1 nm, respectively, except for small holes. Polycrystalline structure was confirmed by grazing incidence x-ray diffraction measurements. Near-edge x-ray absorption fine structure measurements suggested that the plane through aromatic rings of TIPS-P molecules was perpendicular to the substrate surface.

Fabrication of GaN doped ZnO nanocrystallines by laser ablation.

PubMed

Gopalakrishnan, N; Shin, B C; Bhuvana, K P; Elanchezhiyan, J; Balasubramanian, T

2008-08-01

Here, we present the fabrication of pure and GaN doped ZnO nanocrystallines on Si(111) substrates by KrF excimer laser. The targets for the ablation have been prepared by conventional ceramic method. The fabricated nanocrystallines have been investigated by X-ray diffraction, photoluminescence and atomic force microscopy. The X-ray diffraction analysis shows that the crystalline size of pure ZnO is 36 nm and it is 41 nm while doped with 0.8 mol% of GaN due to best stoichiometry between Zn and O. Photoluminescence studies reveal that intense deep level emissions have been observed for pure ZnO and it has been suppressed for the GaN doped ZnO structures. The images of atomic force microscope show that the rms surface roughness is 27 nm for pure ZnO and the morphology is improved with decrease in rms roughness, 18 nm with fine crystallines while doped with 1 mol% GaN. The improved structural, optical and morphological properties of ZnO nanocrystalline due to GaN dopant have been discussed in detail.

The Scherrer equation and the dynamical theory of X-ray diffraction.

PubMed

Muniz, Francisco Tiago Leitão; Miranda, Marcus Aurélio Ribeiro; Morilla Dos Santos, Cássio; Sasaki, José Marcos

2016-05-01

The Scherrer equation is a widely used tool to determine the crystallite size of polycrystalline samples. However, it is not clear if one can apply it to large crystallite sizes because its derivation is based on the kinematical theory of X-ray diffraction. For large and perfect crystals, it is more appropriate to use the dynamical theory of X-ray diffraction. Because of the appearance of polycrystalline materials with a high degree of crystalline perfection and large sizes, it is the authors' belief that it is important to establish the crystallite size limit for which the Scherrer equation can be applied. In this work, the diffraction peak profiles are calculated using the dynamical theory of X-ray diffraction for several Bragg reflections and crystallite sizes for Si, LaB6 and CeO2. The full width at half-maximum is then extracted and the crystallite size is computed using the Scherrer equation. It is shown that for crystals with linear absorption coefficients below 2117.3 cm(-1) the Scherrer equation is valid for crystallites with sizes up to 600 nm. It is also shown that as the size increases only the peaks at higher 2θ angles give good results, and if one uses peaks with 2θ > 60° the limit for use of the Scherrer equation would go up to 1 µm.

A data set from flash X-ray imaging of carboxysomes

NASA Astrophysics Data System (ADS)

Hantke, Max F.; Hasse, Dirk; Ekeberg, Tomas; John, Katja; Svenda, Martin; Loh, Duane; Martin, Andrew V.; Timneanu, Nicusor; Larsson, Daniel S. D.; van der Schot, Gijs; Carlsson, Gunilla H.; Ingelman, Margareta; Andreasson, Jakob; Westphal, Daniel; Iwan, Bianca; Uetrecht, Charlotte; Bielecki, Johan; Liang, Mengning; Stellato, Francesco; Deponte, Daniel P.; Bari, Sadia; Hartmann, Robert; Kimmel, Nils; Kirian, Richard A.; Seibert, M. Marvin; Mühlig, Kerstin; Schorb, Sebastian; Ferguson, Ken; Bostedt, Christoph; Carron, Sebastian; Bozek, John D.; Rolles, Daniel; Rudenko, Artem; Foucar, Lutz; Epp, Sascha W.; Chapman, Henry N.; Barty, Anton; Andersson, Inger; Hajdu, Janos; Maia, Filipe R. N. C.

2016-08-01

Ultra-intense femtosecond X-ray pulses from X-ray lasers permit structural studies on single particles and biomolecules without crystals. We present a large data set on inherently heterogeneous, polyhedral carboxysome particles. Carboxysomes are cell organelles that vary in size and facilitate up to 40% of Earth’s carbon fixation by cyanobacteria and certain proteobacteria. Variation in size hinders crystallization. Carboxysomes appear icosahedral in the electron microscope. A protein shell encapsulates a large number of Rubisco molecules in paracrystalline arrays inside the organelle. We used carboxysomes with a mean diameter of 115±26 nm from Halothiobacillus neapolitanus. A new aerosol sample-injector allowed us to record 70,000 low-noise diffraction patterns in 12 min. Every diffraction pattern is a unique structure measurement and high-throughput imaging allows sampling the space of structural variability. The different structures can be separated and phased directly from the diffraction data and open a way for accurate, high-throughput studies on structures and structural heterogeneity in biology and elsewhere.

X-ray diffraction gratings: Precise control of ultra-low blaze angle via anisotropic wet etching

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

Voronov, Dmitriy L.; Naulleau, Patrick; Gullikson, Eric M.

2016-07-25

Diffraction gratings are used from micron to nanometer wavelengths as dispersing elements in optical instruments. At shorter wavelengths, crystals can be used as diffracting elements, but due to the 3D nature of the interaction with light are wavelength selective rather than wavelength dispersing. There is an urgent need to extend grating technology into the x-ray domain of wavelengths from 1 to 0.1 nm, but this requires the use of gratings that have a faceted surface in which the facet angles are very small, typically less than 1°. Small facet angles are also required in the extreme ultra-violet and soft x-ray energymore » ranges in free electron laser applications, in order to reduce power density below a critical damage threshold. In this work, we demonstrate a technique based on anisotropic etching of silicon designed to produce very small angle facets with a high degree of perfection.« less

How temperature determines formation of maghemite nanoparticles

NASA Astrophysics Data System (ADS)

Girod, Matthias; Vogel, Stefanie; Szczerba, Wojciech; Thünemann, Andreas F.

2015-04-01

We report on the formation of polymer-stabilized superparamagnetic single-core and multi-core maghemite nanoparticles. The particle formation was carried out by coprecipitation of Fe(II) and Fe(III) sulfate in a continuous aqueous process using a micromixer system. Aggregates containing 50 primary particles with sizes of 2 nm were formed at a reaction temperature of 30 °C. These particles aggregated further with time and were not stable. In contrast, stable single-core particles with a diameter of 7 nm were formed at 80 °C as revealed by small-angle X-ray scattering (SAXS) coupled in-line with the micromixer for particle characterization. X-ray diffraction and TEM confirmed the SAXS results. X-ray absorption near-edge structure spectroscopy (XANES) identified the iron oxide phase as maghemite.

X-ray Diffraction from Membrane Protein Nanocrystals

PubMed Central

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

2011-01-01

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

Nanofocus x-ray diffraction and cathodoluminescence investigations into individual core-shell (In,Ga)N/GaN rod light-emitting diodes.

PubMed

Krause, Thilo; Hanke, Michael; Cheng, Zongzhe; Niehle, Michael; Trampert, Achim; Rosenthal, Martin; Burghammer, Manfred; Ledig, Johannes; Hartmann, Jana; Zhou, Hao; Wehmann, Hergo-Heinrich; Waag, Andreas

2016-08-12

Employing nanofocus x-ray diffraction, we investigate the local strain field induced by a five-fold (In,Ga)N multi-quantum well embedded into a GaN micro-rod in core-shell geometry. Due to an x-ray beam width of only 150 nm in diameter, we are able to distinguish between individual m-facets and to detect a significant in-plane strain gradient along the rod height. This gradient translates to a red-shift in the emitted wavelength revealed by spatially resolved cathodoluminescence measurements. We interpret the result in terms of numerically derived in-plane strain using the finite element method and subsequent kinematic scattering simulations which show that the driving parameter for this effect is an increasing indium content towards the rod tip.

Nanofocus x-ray diffraction and cathodoluminescence investigations into individual core-shell (In,Ga)N/GaN rod light-emitting diodes

NASA Astrophysics Data System (ADS)

Krause, Thilo; Hanke, Michael; Cheng, Zongzhe; Niehle, Michael; Trampert, Achim; Rosenthal, Martin; Burghammer, Manfred; Ledig, Johannes; Hartmann, Jana; Zhou, Hao; Wehmann, Hergo-Heinrich; Waag, Andreas

2016-08-01

Employing nanofocus x-ray diffraction, we investigate the local strain field induced by a five-fold (In,Ga)N multi-quantum well embedded into a GaN micro-rod in core-shell geometry. Due to an x-ray beam width of only 150 nm in diameter, we are able to distinguish between individual m-facets and to detect a significant in-plane strain gradient along the rod height. This gradient translates to a red-shift in the emitted wavelength revealed by spatially resolved cathodoluminescence measurements. We interpret the result in terms of numerically derived in-plane strain using the finite element method and subsequent kinematic scattering simulations which show that the driving parameter for this effect is an increasing indium content towards the rod tip.

Fluid synthesis and structure of a new polymorphic modification of boron nitride

NASA Astrophysics Data System (ADS)

Pokropivny, V. V.; Smolyar, A. S.; Ovsiannikova, L. I.; Pokropivny, A. V.; Kuts, V. A.; Lyashenko, V. I.; Nesterenko, Yu. V.

2013-04-01

A new previously unknown phase of boron nitride with a hardness of 0.41-0.63 GPa has been pre-pared by the supercritical fluid synthesis. The presence of a new phase is confirmed by the X-ray spectra and IR absorption spectra, where new reflections and bands are distinguished. The fundamental reflection of the X-ray diffraction pattern is d = 0.286-0.291 nm, and the characteristic band in the infrared absorption spectrum is observed at 704 cm-1. The X-ray diffraction pattern and the experimental and theoretical infrared absorption spectra show that a new synthesized boron nitride phase can be a cluster crystal (space group 211) with a simple cubic lattice. Cage clusters of a fullerene-like morphology B24N24 with point symmetry O are arranged in lattice sites.

Effect of Zn2+, Fe3+ and Cr3+ addition to hydroxyapatite for its application as an active constituent of sunscreens

NASA Astrophysics Data System (ADS)

de Araujo, T. S.; de Souza, S. O.; de Sousa, E. M. B.

2010-11-01

Biocompatible phosphate materials are used in different applications like bone and dental implants, drug delivery systems and others, but could also be applied in inorganic sunscreens. Using sunscreens is extremely necessary, because long time exposure to sun can cause skin cancer. In this work chemical precipitation method has been used to produce hydroxyapatite. Cr3+, Zn2+ and Fe3+ doped samples were characterized using powder X-Ray Diffraction (XRD) and Optical Absorption techniques. X-ray diffraction measurements confirmed the materials were in the expected crystalline structures. The crystallite size as measured from the X-ray pattern was 23-27 nm (±1). The absorption spectra in the ultraviolet and visible ranges indicate that appropriately doped and sized hydroxyapatite particles may have potential applications as active constituents of sunscreens.

Time-resolved structural dynamics of thin metal films heated with femtosecond optical pulses.

PubMed

Chen, Jie; Chen, Wei-Kan; Tang, Jau; Rentzepis, Peter M

2011-11-22

We utilize 100 fs optical pulses to induce ultrafast disorder of 35- to 150-nm thick single Au(111) crystals and observe the subsequent structural evolution using 0.6-ps, 8.04-keV X-ray pulses. Monitoring the picosecond time-dependent modulation of the X-ray diffraction intensity, width, and shift, we have measured directly electron/phonon coupling, phonon/lattice interaction, and a histogram of the lattice disorder evolution, such as lattice breath due to a pressure wave propagating at sonic velocity, lattice melting, and recrystallization, including mosaic formation. Results of theoretical simulations agree and support the experimental data of the lattice/liquid phase transition process. These time-resolved X-ray diffraction data provide a detailed description of all the significant processes induced by ultrafast laser pulses impinging on thin metallic single crystals.

Comment on Sub-15 nm Hard X-Ray Focusing with a New Total-Reflection Zone Plate

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

Specht, Eliot D

2011-01-01

Takano et al. report the focusing of 10-keV X-rays to a size of 14.4 nm using a total-reflection zone plate (TRZP). This focal size is at the diffraction limit for the optic's aperture. This would be a noteworthy result, since the TRZP was fabricated using conventional lithography techniques. Alternative nanofocusing optics require more demanding fabrication methods. However, as I will discuss in this Comment, the intensity distribution presented by Takano et al. (Fig. 4 of ref. 1) is more consistent with the random speckle pattern produced by the scattering of a coherent incident beam by a distorted optic than withmore » a diffraction-limited focus. When interpreted in this manner, the true focal spot size is {approx}70 nm: 5 times the diffraction limit. When a coherent photon beam illuminates an optic containing randomly distributed regions which introduce different phase shifts, the scattered diffraction pattern consists of a speckle pattern. Each speckle will be diffraction-limited: the peak width of a single speckle depends entirely on the source coherence and gives no information about the optic. The envelope of the speckle distribution corresponds to the focal spot which would be observed using incoherent illumination. The width of this envelope is due to the finite size of the coherently-diffracting domains produced by slope and position errors in the optic. The focal intensity distribution in Fig. 4 of ref. 1 indeed contains a diffraction-limited peak, but this peak contains only a fraction of the power in the focused, and forms part of a distribution of sharp peaks with an envelope {approx}70 nm in width, just as expected for a speckle pattern. At the 4mm focal distance, the 70 nm width corresponds to a slope error of 18 {micro}rad. To reach the 14 nm diffraction limit, the slope error must be reduced to 3 {micro}rad. Takano et al. have identified a likely source of this error: warping due to stress as a result of zone deposition. It will be interesting to see whether the use of a more rigid substrate gives improved results.« less

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

Amaya, Andrew J.; Pathak, Harshad; Modak, Viraj P.

Using an X-ray laser, we investigated the crystal structure of ice formed by homogeneous ice nucleation in deeply supercooled water nanodrops (r ≈ 10 nm) at ~225 K. The nanodrops were formed by condensation of vapor in a supersonic nozzle, and the ice was probed within 100 μs of freezing using femtosecond wide-angle X-ray scattering at the Linac Coherent Light Source free-electron X-ray laser. The X-ray diffraction spectra indicate that this ice has a metastable, predominantly cubic structure; the shape of the first ice diffraction peak suggests stacking-disordered ice with a cubicity value, χ, in the range of 0.78 ±more » 0.05. The cubicity value determined here is higher than those determined in experiments with micron-sized drops but comparable to those found in molecular dynamics simulations. Lastly, the high cubicity is most likely caused by the extremely low freezing temperatures and by the rapid freezing, which occurs on a ~1 μs time scale in single nanodroplets.« less

Filming nuclear dynamics of iodine using x-ray diffraction at the LCLS

NASA Astrophysics Data System (ADS)

Ware, Matthew; Natan, Adi; Glownia, James; Cryan, James; Bucksbaum, Phil

2017-04-01

We will provide an overview of our analysis of the nuclear dynamics of iodine. At the LCLS, we pumped a gas cell of iodine with a weak 520nm, 50 fs pulse, and the nuclear dynamics are then probed with 9 keV, 40 fs x-rays with variable time delay. This allows us to simultaneously image nuclear wavepackets on the dissociating A state, on the bound B state, and even Raman wavepackets in the ground electronic state. We will explain at length how we isolate each of these signals using a Legendre decomposition of our x-ray data and the selection rules for each of the transitions. Likewise, we will discuss how we convert the x-ray diffraction patterns into real-space movies of the nuclear dynamics. Research supported by the U.S. Department of Energy, Office of Basic Energy Sciences, Atomic, Molecular, and Optical Science Program. Use of LCLS supported under DOE Contract No. DE-AC02-76F00515.

How Cubic Can Ice Be?

DOE PAGES

Amaya, Andrew J.; Pathak, Harshad; Modak, Viraj P.; ...

2017-06-28

Using an X-ray laser, we investigated the crystal structure of ice formed by homogeneous ice nucleation in deeply supercooled water nanodrops (r ≈ 10 nm) at ~225 K. The nanodrops were formed by condensation of vapor in a supersonic nozzle, and the ice was probed within 100 μs of freezing using femtosecond wide-angle X-ray scattering at the Linac Coherent Light Source free-electron X-ray laser. The X-ray diffraction spectra indicate that this ice has a metastable, predominantly cubic structure; the shape of the first ice diffraction peak suggests stacking-disordered ice with a cubicity value, χ, in the range of 0.78 ±more » 0.05. The cubicity value determined here is higher than those determined in experiments with micron-sized drops but comparable to those found in molecular dynamics simulations. Lastly, the high cubicity is most likely caused by the extremely low freezing temperatures and by the rapid freezing, which occurs on a ~1 μs time scale in single nanodroplets.« less

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

Tahir, Dahlang, E-mail: dtahir@fmipa.unhas.ac.id; Bakri, Fahrul; Liong, Syarifuddin

We have studied the molecular properties, structural properties, and chemical composition of composites by Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) spectroscopy, and X-ray fluorescence (XRF) spectroscopy, respectively. FTIR spectra shows absorption band of hydroxyl group (-OH), methyl group (-CH{sub 3}) and aromatic group (C-C). The absorption band for aromatic group (C-C) shows the formation of carbonaceous in composites. XRF shows chemical composition of composites, which the main chemicals are SO{sub 3}, Cl, and ZnO. The loss on ignition value (LOI) of activated charcoal indicates high carbonaceous matter. The crystallite size for diffraction pattern from hydrogel polymer is aboutmore » 17 nm and for activated charcoal are about 19 nm. The crystallite size of the polymer is lower than that of activated charcoal, which make possible of the particle from filler in contact with each other to form continuous conducting polymer through polymer matrix.« less

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

NASA Astrophysics Data System (ADS)

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

2012-07-01

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

Trichoderma koningii assisted biogenic synthesis of silver nanoparticles and evaluation of their antibacterial activity

NASA Astrophysics Data System (ADS)

Tripathi, R. M.; Gupta, Rohit Kumar; Shrivastav, Archana; Singh, M. P.; Shrivastav, B. R.; Singh, Priti

2013-09-01

The present study demonstrates the biosynthesis of silver nanoparticles using Trichoderma koningii and evaluation of their antibacterial activity. Trichoderma koningii secretes proteins and enzymes that act as reducing and capping agent. The biosynthesized silver nanoparticles (AgNPs) were characterized by UV-Vis spectroscopy, dynamic light scattering (DLS), transmission electron microscopy (TEM) and x-ray diffraction (XRD). UV-Vis spectra showed absorbance peak at 413 nm corresponding to the surface plasmon resonance of silver nanoparticles. DLS was used to find out the size distribution profile. The size and morphology of the AgNPs was determined by TEM, which shows the formation of spherical nanoparticles in the size range of 8-24 nm. X-ray diffraction showed intense peaks corresponding to the crystalline silver. The antibacterial activity of biosynthesized AgNPs was evaluated by growth curve and inhibition zone and it was found that the AgNPs show potential effective antibacterial activity.

X-ray diffraction and Raman investigations of thickness dependent stress effects on Pb(ZrxTi1-x)O3 thin films

NASA Astrophysics Data System (ADS)

Lappalainen, Jyrki; Lantto, Vilho; Frantti, Johannes; Hiltunen, Jussi

2006-06-01

Microstructure, film orientation, and optical transmission spectra of polycrystalline Nd-modified Pb(ZrxTi1-x)O3 films were studied as a function of film thickness. Pulsed laser deposition was used for the fabrication of films with thickness from 80to465nm on single-crystal MgO(100) substrates. Raman spectroscopy, x-ray diffraction, and spectrophotometry measurements were utilized in the film characterization. With the decreasing film thickness, films first oriented with c axis perpendicular to film surface, and then, after some critical thickness, changed to a-axis orientation. At the same time, compressive stress increased up to 1.3GPa and a clear blueshift of the optical absorption edge was found in transmission spectra.

Enhanced UVB emission and analysis of chemical states of Ca5(PO4)3OH:Gd3+,Pr3+ phosphor prepared by co-precipitation

NASA Astrophysics Data System (ADS)

Mokoena, P. P.; Nagpure, I. M.; Kumar, Vinay; Kroon, R. E.; Olivier, E. J.; Neethling, J. H.; Swart, H. C.; Ntwaeaborwa, O. M.

2014-08-01

Hydroxyapatite (Ca5(PO4)3OH) is a well-known bioceramic material used in medical applications because of its ability to form direct chemical bonds with living tissues. This mineral is currently used as a host for rare-earth ions (e.g. Gd3+, Pr3+, Tb3+, etc.) to prepare phosphors that can be used in light emitting devices of different types. In this study Ca5(PO4)3OH:Gd3+,Pr3+ phosphors were prepared by the co-precipitation method and were characterised by x-ray diffraction, x-ray photoelectron spectroscopy, scanning electron microscopy, high resolution transmission electron microscopy, energy dispersive x-ray spectroscopy and photoluminescence spectroscopy. The x-ray diffraction pattern was consistent with the hexagonal phase of Ca5(PO4)3OH referenced in JCPDS card number 73-0293. The x-ray photoelectron spectroscopy data indicated that Ca2+ occupied two different lattice sites, referred to as Ca1 and Ca2. The photoluminescence data exhibited a narrowband emission located at 313 nm, which is associated with the 6P7/2→8S7/2 transition of the Gd3+ ion. This emission is classified as ultraviolet B and it is suitable for use in phototherapy lamps to treat various skin diseases. The photoluminescence intensity of the 313 nm emission was enhanced considerably by Pr3+ co-doping.

Preparation, characterization and X-ray attenuation property of Gd2O3-based nanocomposites

NASA Astrophysics Data System (ADS)

Jayakumar, Sangeetha; Saravanan, T.; Philip, John

2017-11-01

In an attempt to develop an alternate to lead-based X-ray shielding material, we describe the X-ray attenuation property of nanocomposites containing Gd2O3 as nanofiller and silicone resin as matrix, prepared by a simple solution-casting technique. Gd2O3 nanoparticles of size 30 and 56 nm are used at concentrations of 25 and 2.5 wt%. The nanoparticles and the nanocomposites are characterized using X-ray diffraction (XRD) studies, small angle X-ray spectroscopy (SAXS), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and atomic force microscopy (AFM). The X-ray attenuation property of nanocomposites, studied using an industrial X-ray unit, shows that nanocomposites containing nanoparticles of size 56 nm (G2) exhibit better attenuation than nanocomposites containing nanoparticles of size 30 nm (G1), which is attributed to the greater interfacial interaction between the G2 nanofillers and silicone matrix. In the case of nanocomposites containing G1 nanoparticles, the interfacial interaction between the nanofiller and the matrix is so weak that it results in pulling out of nanofillers, causing voids in the matrix, which act as X-ray transparent region, thereby reducing the overall X-ray attenuation property of G1 nanocomposites. This is further corroborated from the AFM images of the nanocomposites. The weight loss and heat flow curves of pure silicone matrix and the nanocomposites containing Gd2O3 nanoparticles of size 30 and 56 nm show the degradation of silicone resin, due to chain scission, between 403 and 622 °C. The same onset temperature (403 °C) of degradation of matrix with and without nanoparticles shows that the addition of nanofillers to the matrix does not deteriorate the thermal stability of the matrix. This confirms the thermal stability of nanocomposites. Therefore, our study shows that nanocomposites containing G2 nanoparticles are potential candidates for the development of X-ray opaque fabric material.

X-ray structural investigation of nonsymmetrically and symmetrically alkylated [1]benzothieno[3,2-b]benzothiophene derivatives in bulk and thin films.

PubMed

Gbabode, Gabin; Dohr, Michael; Niebel, Claude; Balandier, Jean-Yves; Ruzié, Christian; Négrier, Philippe; Mondieig, Denise; Geerts, Yves H; Resel, Roland; Sferrazza, Michele

2014-08-27

A detailed structural study of the bulk and thin film phases observed for two potential high-performance organic semiconductors has been carried out. The molecules are based on [1]benzothieno[3,2-b]benzothiophene (BTBT) as conjugated core and octyl side groups, which are anchored either symmetrically at both sides of the BTBT core (C8-BTBT-C8) or nonsymmetrically at one side only (C8-BTBT). Thin films of different thickness (8-85 nm) have been prepared by spin-coating for both systems and analyzed by combining specular and grazing incidence X-ray diffraction. In the case of C8-BTBT-C8, the known crystal structure obtained from single-crystal investigations is observed within all thin films, down to a film thickness of 9 nm. In the case of C8-BTBT, the crystal structure of the bulk phase has been determined from X-ray powder diffraction data with a consistent matching of experimental and calculated X-ray diffraction patterns (Rwp = 5.8%). The packing arrangement of C8-BTBT is similar to that of C8-BTBT-C8, that is, consisting of a lamellar structure with molecules arranged in a "herringbone" fashion, yet with lamellae composed of two head-to-head (or tail-to-tail as the structure is periodic) superimposed molecules instead of only one molecule for C8-BTBT-C8. As for C8-BTBT-C8, we demonstrate that the same phase is observed in bulk and thin films for C8-BTBT whatever the film thickness investigated.

Effect of La3+ Substitution on Electric, Dielectric and Magnetic Properties of Cobalt Nano-Ferrite

NASA Astrophysics Data System (ADS)

Kumar, Pawan; Singh, M.

2011-07-01

Ultrafine particles of CoLaxFe2-xO4 (x = 0, 0.20) were prepared by using co-precipitation method. X-ray diffraction studies show that the samples have cubic spinel structure and average crystallite size of x = 0 and x = 0.2 are 49.84 nm and 27.73 nm respectively. Dielectric and magnetic properties have been studied by impedance analyzer and magnetic properties of the ferrite system were studied using VSM respectively. La3+ ions modulate significantly the electric, dielectric and magnetic properties of cobalt spinel ferrites.

Crystal Structure, Magnetic and Optical Properties of Mn-Doped BiFeO₃ by Hydrothermal Synthesis.

PubMed

Zhang, Ning; Wei, Qinhua; Qin, Laishun; Chen, Da; Chen, Zhi; Niu, Feng; Wang, Jiangying; Huanag, Yuexiang

2017-01-01

In this paper, Mn doped BiFeO₃ were firstly synthesized by hydrothermal process. The influence of Mn doping on structural, optical and magnetic properties of BiFeO₃ was studied. The different amounts of Mn doping in BiFeO₃ were characterized by X-ray diffraction, Scanning Electron Microscope, Energy Dispersive X-ray Spectroscope, UV-Vis diffuse reflectance spectroscopy and magnetic measurements. The X-ray diffraction (XRD) patterns confirmed the formation of pure phase rhombohedral structure in BiFe(1−x) Mn (x) O₃ (x = 0.01, 0.03, 0.05, 0.07) samples. The morphologies and chemical compositions of as-prepared samples could be observed by Scanning Electron Microscope (SEM) and Energy Dispersive X-ray Spectroscope (EDS). A relative large saturated magnetization (Ms) of 0.53 emu/g for x = 0.07 sample was obtained at room temperature, which is considered to be Mn ions doping. UV-Vis diffuse reflectance spectroscopy showed strong absorption of light in the range of 200–1000 nm, indicating the optical band gap in the visible region for these samples. This implied that BiFe(1−x) Mn(x)O₃ may be a potential photocatalyst for utilizing solar energy.

Study of Inverse Ni-based Photonic Crystal using the Microradian X-ray Diffraction

NASA Astrophysics Data System (ADS)

Vasilieva, A. V.; Grigoryeva, N. A.; Mistonov, A. A.; Sapoletova, N. A.; Napolskii, K. S.; Eliseev, A. A.; Lukashin, A. V.; Tretyakov, Yu D.; Petukhov, A. V.; Byelov, D.; Chernyshov, D.; Okorokov, A. I.; Bouwman, W. G.; Grigoriev, S. V.

2010-10-01

Inverse photonic nickel-based crystal films formed by electrocrystallization of metal inside the voids of polymer artificial opal have been studied using the microradian X-ray diffraction. Analysis of the diffraction images agrees with an face-centred cubic (FCC) structure with the lattice constant a0 = 650 ± 10 nm and indicates two types of stacking sequences coexisting in the crystal (twins of ABCABC... and ACBACB... ordering motifs), the ratio between them being 4:5 The transverse structural correlation length Ltran is 2.4 ± 0.1 μm, which corresponds to a sample thickness of 6 layers. The in-plane structural correlation length Llong is 3.4 ± 0.2 μm, and the structure mosaic is of order of 10°.

High Pressure Structure and Electrical Resistance Measurements on Cadmium Sulfide Nanoparticles

NASA Astrophysics Data System (ADS)

Montgomery, J. M.; Stemshorn, A. K.; Stanishevsky, A.; Vohra, Y. K.; Weir, S. T.

2010-03-01

Room-temperature four-probe electrical resistance and synchrotron x-ray diffraction measurements have been performed on dried and aqueous suspensions of CdS nanoparticles (25 nm in diameter) to 35 GPa. Nanoparticles used in these experiments were synthesized using the reaction between a cadmium salt and thiourea under hydrothermal conditions without using any surfactants. While the x-ray structure data confirms the irreversible wurtzite -> rocksalt transition seen at 2.5 GPa in bulk CdS, the corresponding resistance drop was not observed in the measured range, indicating that the nanoparticle boundaries may prevent electronic communication between particles. Further studies on dry and aqueous 10 nm nano-spheres and 9 nm diameter nano-rods are planned, and the results of these experiments will be presented.

Ionic liquid-templated preparation of mesoporous silica embedded with nanocrystalline sulfated zirconia

NASA Astrophysics Data System (ADS)

Ward, Antony J.; Pujari, Ajit A.; Costanzo, Lorenzo; Masters, Anthony F.; Maschmeyer, Thomas

2011-12-01

A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route. The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy. Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm) polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%.

Large-Scale Synthesis of Tin-Doped Indium Oxide Nanofibers Using Water as Solvent

NASA Astrophysics Data System (ADS)

Altecor, Aleksey; Mao, Yuanbing; Lozano, Karen

2012-09-01

Here we report the successful fabrication of tin-doped indium oxide (ITO) nanofibers using a scalable Forcespinning™ method. In this environmentally-friendly process, water was used as the only solvent for both Polyvinylpyrrolidone (PVP, the sacrificial polymer) and the metal chloride precursor salts. The obtained precursor nanofiber mats were calcinated at temperatures ranging from 500-800°C to produce ITO nanofibers with diameters as small as 400 nm. The developed ITO nanofibers were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy and X-ray diffraction analysis.

Growth, morphological and optical characteristics of ZnSSe nanorods

NASA Astrophysics Data System (ADS)

Chen, Lin-Jer; Dai, Jia-Heng

2017-02-01

Zinc seledide sulfide (ZnSxSe1-x) nanorods with wurtzite structure were synthesized by a low temperature solvothermal pathway. In a typical condition of solvothermal at 180 °C for 8 h, the ZnSxSe1-x was composed of nanorods 10-15 nm in diameter and 50-75 nm length. These results indicate that the nanoscale of ZnSSe nanocrystals may contribute to the solvothermal process and exhibit a tunable photoluminescence (PL) and band gap that depends on the variation of reaction conditions. The work suggests a promising route to single-mode "mirror-less" amplified spontaneous emission (ASE) from inorganic nanomaterials with the Cholesteric liquid crystals (CLC) providing additional potential functionality. The obtained products are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-visible spectroscopy, and X-ray photoelectron spectroscopy (XPS). This approach for solvothermal growth can also be used with primary ZnSSe nanorods to achieve tunable optical properties and can likely be extended to nanomaterials of different shapes and other optical devices.

Solvent free tin oxide nanoparticle for gas sensing application

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

Ranjan, Pranay, E-mail: pranjan@iitp.ac.in; Thakur, Ajay D.; Centre for Energy and Environment, Indian Institute of Technology Patna, Patliputra, Patna 800013 India

2016-05-06

A new modified technique of synthesizing tin oxide nanoparticles with crystallite size of 2 nm to 6 nm has been developed. Surface area of the nanoparticle has been increased as we approached towards the Debye length. Such a techniques for approaching the Debye length is expected to bring remarkable changes in the properties of resistive based gas sensors. The technique used here is less toxic, economical and has high yield. Phase purity, size, shape and composition has been investigated using x-ray diffraction, micro Raman, scanning electron microscopy and energy dispersive x ray spectroscopy. While surface area has been calculated through Brunaur-Emmett-Teller (BET).

Synthesis and properties of nanocrystalline copper indium oxide thin films deposited by Rf magnetron sputtering.

PubMed

Singh, Mandeep; Singh, V N; Mehta, B R

2008-08-01

Nanocrystalline copper indium oxide (CuInO2) thin films with particle size ranging from 25 nm to 71 nm have been synthesized from a composite target using reactive Rf magnetron sputtering technique. X-ray photoelectron spectroscopy (XPS) combined with glancing angle X-ray diffraction (GAXRD) analysis confirmed the presence of delafossite CuInO2 phase in these films. The optical absorption studies show the presence of two direct band gaps at 3.3 and 4.3 eV, respectively. The resistance versus temperature measurements show thermally activated hopping with activation energy of 0.84 eV to be the conduction mechanism.

Synthesis, structure and magnetic properties of nanostructured La1-xAxFe0.5Mn0.5O3 (A = Ca, Sr and Pb; x = 0 & 0.25) perovskites

NASA Astrophysics Data System (ADS)

Hossain, Aslam; Ghosh, Debamalya; Dutta, Uma; Walke, Pravin S.; Mordvinova, Natalia E.; Lebedev, Oleg I.; Sinha, Bhavesh; Pal, Kamalesh; Gayen, Arup; Kundu, Asish K.; Seikh, Md. Motin

2017-12-01

The effect of hole doping on magnetic properties of LaFe0.5Mn0.5O3 have been investigated. All the ceramics samples La1-xAxFe0.5Mn0.5O3 (A = Ca, Sr and Pb; x = 0 & 0.25) were synthesized at 500 °C by sol-gel method and the particles size were found to be in nanodimension. The samples were characterized by X-ray and electron diffraction, HRTEM and both dc and ac-magnetization measurements. The X-ray and electron diffraction patterns were indexed by cubic Pm-3m space group. The particle size of the LaFe0.5Mn0.5O3 is ∼100 nm, whereas the Pb-doped sample is ∼50 nm and for Ca or Sr doped samples the size is ∼10-30 nm. Both dc and ac-susceptibility measurements suggest that the effect of hole doping and A-site cationic radius in LaFe0.5Mn0.5O3 have no significant role on magnetic properties. However, the particle size plays an important role on magnetic property due to the development of surface ferromagnetic cluster at nanoscale. The competing interactions lead to magnetic phase separation where local ferromagnetic clusters coexist within the antiferromagentic matrix in all the samples.

Effect of Cu2+ substitution on the structural, optical and magnetic behaviour ofchemically derived manganese ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Vasuki, G.; Balu, T.

2018-06-01

Mixed spinel copper manganese ferrite (CuXMn1‑XFe2O4, X = 0, 0.25, 0.5, 0.75, 1) nanoparticles were synthesized by chemical co-precipitation technique. From the powder x-ray diffraction analysis the lattice constant, volume of unit cell, x-ray density, hopping lengths, crystallite size, surface area, dislocation density and microstrain were calculated. The substitution of Cu2+ ions shows a considerable reduction in the crystallite size of manganese ferrite from 34 nm to 22 nm. Further a linear fit of Williamson-Hall plot has been drawn to determine the microstrain and crystallite size. The crystallite size and morphology were further observed through high resolution transmission electron microscope and scanning electron microscope. The diffraction rings observed from selected area electron diffraction pattern exhibits the crystalline nature of all the samples. The energy dispersive x-ray analysis shows the composition of all the elements incorporated in the synthesized nanomaterials. FTIR studies reveal the absorption peaks that correspond to the metal-oxygen vibrations in the tetrahedral and octahedral sites. From the UV–vis absorption spectra the band gap energy, refractive index and optical dielectric constant were determined. Magnetic studies carried out using vibrating sample magnetometer shows interesting behaviour in the variation of magnetisation and coercivity. Peculiar magnetic behaviour is observed when Cu2+ ions are substituted in manganese ferrites. All the synthesized materials have very low value of squareness ratio which attributes to the superparamagnetic behaviour.

X-ray diffraction from flight muscle with a headless myosin mutation: implications for interpreting reflection patterns

PubMed Central

Iwamoto, Hiroyuki; Trombitás, Károly; Yagi, Naoto; Suggs, Jennifer A.; Bernstein, Sanford I.

2014-01-01

Fruit fly (Drosophila melanogaster) is one of the most useful animal models to study the causes and effects of hereditary diseases because of its rich genetic resources. It is especially suitable for studying myopathies caused by myosin mutations, because specific mutations can be induced to the flight muscle-specific myosin isoform, while leaving other isoforms intact. Here we describe an X-ray-diffraction-based method to evaluate the structural effects of mutations in contractile proteins in Drosophila indirect flight muscle. Specifically, we describe the effect of the headless myosin mutation, Mhc10-Y97, in which the motor domain of the myosin head is deleted, on the X-ray diffraction pattern. The loss of general integrity of the filament lattice is evident from the pattern. A striking observation, however, is the prominent meridional reflection at d = 14.5 nm, a hallmark for the regularity of the myosin-containing thick filament. This reflection has long been considered to arise mainly from the myosin head, but taking the 6th actin layer line reflection as an internal control, the 14.5-nm reflection is even stronger than that of wild-type muscle. We confirmed these results via electron microscopy, wherein image analysis revealed structures with a similar periodicity. These observations have major implications on the interpretation of myosin-based reflections. PMID:25400584

Synthesis and characterization of Cu3Se2 nanofilms by an underpotential deposition based electrochemical codeposition technique

NASA Astrophysics Data System (ADS)

Aydın, Zehra Yazar; Abacı, Serdar

2017-12-01

The Cu3Se2 nanofilms were synthesized with underpotential deposition based electrochemical codeposition technique for the first time in the literature. The electrochemical behaviors of copper and selenium were investigated in 0.1 M H2SO4 on Au electrode. The effects of concentration and scan rate on the electrochemical behavior of selenium were studied. The electrochemical behaviors in underpotential deposition and bulk regions of the Cu-Se system were investigated in acidic solution by cyclic voltammetry and electrolysis techniques. X-ray photoelectron spectroscopy, scanning electron microscopy, atomic force microscopy, X-ray diffraction, Raman spectroscopy, and ultraviolet and visible absorption spectroscopy techniques were used for characterization of synthesized films. According to the X-ray photoelectron spectroscopy spectrum, Cu/Se ratio was determined to be approximately 3/2. Copper selenide nanofilms are two phases and polycrystalline according to X-ray diffraction. The films mainly formed tetragonal Cu3Se2 (umangite mineral structure) structure and the particle size was approximately 45.95 nm. Scanning electron microscopy images showed that Cu3Se2 nanofilms consisted of uniform, nano-sizes and two-dimensional. It was found through AFM that the surface roughness of the film was 6.173 nm, with a mean particle size of around 50 nm. Depending on the deposition time, the band gaps of the Cu3Se2 films were in the range of 2.86-3.20 eV. Three characteristic vibrational modes belonging to Cu3Se2 nanofilms were recorded in the Raman spectrum.

Synthesis and characterization of graphene oxide using modified Hummer's method

NASA Astrophysics Data System (ADS)

Kaur, Manpreet; Kaur, Harsimran; Kukkar, Deepak

2018-05-01

In the present study, a simple approach has been followed for the synthesis of graphene oxide (GO) using modified Hummers method in which graphite powder was oxidized in the presence of concentrated H2SO4 and KMnO4. The amount of NaNO3 and KMnO4 was varied to produce sheet like structure. The varied concentrations of NaNO3 and KMnO4 resulted in yielding large amount of the product. Structural, morphological and physicochemical features of the product were studied using UV-Visible spectrophotometer, Fourier Transform infrared spectroscopy (FTIR), and crystal structure was determined using X-ray powder diffraction (XRD). UV-Vis spectra of GO was observed at a maximum absorption of 230 nm due to (π-π*) transition of atomic carbon-carbon bonds. FTIR spectra revealed the presence of oxygen containing functional groups which ensures the complete exfoliation of graphite into graphene oxide X-ray powder diffraction pattern of the product showed the diffraction peak at (2θ = 26.7°) with an interlayer spacing of 0.334 nm. All the above characterizations successfully confirmed the formation of GO.

Microstructural investigation of nickel silicide thin films and the silicide-silicon interface using transmission electron microscopy.

PubMed

Bhaskaran, M; Sriram, S; Mitchell, D R G; Short, K T; Holland, A S; Mitchell, A

2009-01-01

This article discusses the results of transmission electron microscopy (TEM)-based investigation of nickel silicide (NiSi) thin films grown on silicon. Nickel silicide is currently used as the CMOS technology standard for local interconnects and in electrical contacts. Films were characterized with a range of TEM-based techniques along with glancing angle X-ray diffraction. The nickel silicide thin films were formed by vacuum annealing thin films of nickel (50 nm) deposited on (100) silicon. The cross-sectional samples indicated a final silicide thickness of about 110 nm. This investigation studied and reports on three aspects of the thermally formed thin films: the uniformity in composition of the film using jump ratio maps; the nature of the interface using high resolution imaging; and the crystalline orientation of the thin films using selected-area electron diffraction (SAED). The analysis highlighted uniform composition in the thin films, which was also substantiated by spectroscopy techniques; an interface exhibiting the desired abrupt transition from silicide to silicon; and desired and preferential crystalline orientation corresponding to stoichiometric NiSi, supported by glancing angle X-ray diffraction results.

Novel silica stabilization method for the analysis of fine nanocrystals using coherent X-ray diffraction imaging

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

Monteforte, Marianne; Estandarte, Ana K.; Chen, Bo

2016-06-23

High-energy X-ray Bragg coherent diffraction imaging (BCDI) is a well established synchrotron-based technique used to quantitatively reconstruct the three-dimensional morphology and strain distribution in nanocrystals. The BCDI technique has become a powerful analytical tool for quantitative investigations of nanocrystals, nanotubes, nanorods and more recently biological systems. BCDI has however typically failed for fine nanocrystals in sub-100?nm size regimes ? a size routinely achievable by chemical synthesis ? despite the spatial resolution of the BCDI technique being 20?30?nm. The limitations of this technique arise from the movement of nanocrystals under illumination by the highly coherent beam, which prevents full diffraction datamore » sets from being acquired. A solution is provided here to overcome this problem and extend the size limit of the BCDI technique, through the design of a novel stabilization method by embedding the fine nanocrystals into a silica matrix. Chemically synthesized FePt nanocrystals of maximum dimension 20?nm and AuPd nanocrystals in the size range 60?65?nm were investigated with BCDI measurement at beamline 34-ID-C of the APS, Argonne National Laboratory. Novel experimental methodologies to elucidate the presence of strain in fine nanocrystals are a necessary pre-requisite in order to better understand strain profiles in engineered nanocrystals for novel device development.« less

Novel silica stabilization method for the analysis of fine nanocrystals using coherent X-ray diffraction imaging.

PubMed

Monteforte, Marianne; Estandarte, Ana K; Chen, Bo; Harder, Ross; Huang, Michael H; Robinson, Ian K

2016-07-01

High-energy X-ray Bragg coherent diffraction imaging (BCDI) is a well established synchrotron-based technique used to quantitatively reconstruct the three-dimensional morphology and strain distribution in nanocrystals. The BCDI technique has become a powerful analytical tool for quantitative investigations of nanocrystals, nanotubes, nanorods and more recently biological systems. BCDI has however typically failed for fine nanocrystals in sub-100 nm size regimes - a size routinely achievable by chemical synthesis - despite the spatial resolution of the BCDI technique being 20-30 nm. The limitations of this technique arise from the movement of nanocrystals under illumination by the highly coherent beam, which prevents full diffraction data sets from being acquired. A solution is provided here to overcome this problem and extend the size limit of the BCDI technique, through the design of a novel stabilization method by embedding the fine nanocrystals into a silica matrix. Chemically synthesized FePt nanocrystals of maximum dimension 20 nm and AuPd nanocrystals in the size range 60-65 nm were investigated with BCDI measurement at beamline 34-ID-C of the APS, Argonne National Laboratory. Novel experimental methodologies to elucidate the presence of strain in fine nanocrystals are a necessary pre-requisite in order to better understand strain profiles in engineered nanocrystals for novel device development.

Focused ion beam direct micromachining of DOEs

NASA Astrophysics Data System (ADS)

Khan Malek, Chantal; Hartley, Frank T.; Neogi, Jayant

2000-09-01

We discuss here the capability of direct manufacture of various high- resolution diffractive optics, in particular regarding micromachining of DOEs in 3D. Preliminary demonstrations were made in 2-D using an automated FIB system operated at 30 KeV with a Gallium liquid metal ion source and equipped with a gas injection system (GIS). Gratings with a 20 nm line width and zone plates with 32 nm outer ring were milled in a reactive atmosphere (iodine) directly through 3.5 (mu) m and 800 nm of gold respectively. Plans for combining FIB and X-ray lithography to make diffractive optical elements (DOEs) for JPL are also mentioned.

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloy

NASA Astrophysics Data System (ADS)

Mori, A.; Mamiya, H.; Ohnuma, M.; Ilavsky, J.; Ohishi, K.; Woźniak, Jarosław; Olszyna, A.; Watanabe, N.; Suzuki, J.; Kitazawa, H.; Lewandowska, M.

2018-04-01

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and alloy contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small-angle X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 °C. Sintering at 1000 °C for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128 nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloys

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

Kowalska-Mori, A.; Mamiya, H.; Ohnuma, M.

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 ºC. Sintering at 1000 ºC for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128more » nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.« less

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloys

DOE PAGES

Kowalska-Mori, A.; Mamiya, H.; Ohnuma, M.; ...

2018-01-17

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 ºC. Sintering at 1000 ºC for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128more » nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.« less

Studying Ultradisperse Diamond Structure within Explosively Synthesized Samples via X-Ray Techniques

NASA Astrophysics Data System (ADS)

Sharkov, M. D.; Boiko, M. E.; Ivashevskaya, S. N.; Belyakova, N. S.

2013-08-01

XRD (X-Ray Diffraction) and SAXS (Small-Angle X-Ray Scattering) data have been measured for a pair of samples produced with the help of explosives. XRD peaks have shown the both samples to contain crystal diamond components as well as graphite ones. Basing on SAXS analysis, possible presence of grains with radii up to 30-50 nm within all the samples has been shown. Structure components with fractal dimension between 1 and 2 in the sample have been detected, this fact being in agreement with the assumption of diamond grain coating similarity to onion shells. In order to broad rocking curves analysis, the standard SAXS treatment technique has been complemented by a Fourier filtering procedure. For the sample #1, rocking curve components corresponding to individual interplanar distances with magnitudes from 5 nm up to 15 nm have been separated. A hypothesis relating these values to the distances between concentric onion-like shells of diamond grains has been formulated.

Influences of Co doping on the structural and optical properties of ZnO nanostructured

NASA Astrophysics Data System (ADS)

Majeed Khan, M. A.; Wasi Khan, M.; Alhoshan, Mansour; Alsalhi, M. S.; Aldwayyan, A. S.

2010-07-01

Pure and Co-doped ZnO nanostructured samples have been synthesized by a chemical route. We have studied the structural and optical properties of the samples by using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), field-emission transmission electron microscope (FETEM), energy-dispersive X-ray (EDX) analysis and UV-VIS spectroscopy. The XRD patterns show that all the samples are hexagonal wurtzite structures. Changes in crystallite size due to mechanical activation were also determined from X-ray measurements. These results were correlated with changes in particle size followed by SEM and TEM. The average crystallite sizes obtained from XRD were between 20 to 25 nm. The TEM images showed the average particle size of undoped ZnO nanostructure was about 20 nm whereas the smallest average grain size at 3% Co was about 15 nm. Optical parameters such as absorption coefficient ( α), energy band gap ( E g ), the refractive index ( n), and dielectric constants ( σ) have been determined using different methods.

Single mimivirus particles intercepted and imaged with an X-ray laser

PubMed Central

Seibert, M. Marvin; Ekeberg, Tomas; Maia, Filipe R. N. C.; Svenda, Martin; Andreasson, Jakob; Jönsson, Olof; Odić, Duško; Iwan, Bianca; Rocker, Andrea; Westphal, Daniel; Hantke, Max; DePonte, Daniel P.; Barty, Anton; Schulz, Joachim; Gumprecht, Lars; Coppola, Nicola; Aquila, Andrew; Liang, Mengning; White, Thomas A.; Martin, Andrew; Caleman, Carl; Stern, Stephan; Abergel, Chantal; Seltzer, Virginie; Claverie, Jean-Michel; Bostedt, Christoph; Bozek, John D.; Boutet, Sébastien; Miahnahri, A. Alan; Messerschmidt, Marc; Krzywinski, Jacek; Williams, Garth; Hodgson, Keith O.; Bogan, Michael J.; Hampton, Christina Y.; Sierra, Raymond G.; Starodub, Dmitri; Andersson, Inger; Bajt, Saša; Barthelmess, Miriam; Spence, John C. H.; Fromme, Petra; Weierstall, Uwe; Kirian, Richard; Hunter, Mark; Doak, R. Bruce; Marchesini, Stefano; Hau-Riege, Stefan P.; Frank, Matthias; Shoeman, Robert L.; Lomb, Lukas; Epp, Sascha W.; Hartmann, Robert; Rolles, Daniel; Rudenko, Artem; Schmidt, Carlo; Foucar, Lutz; Kimmel, Nils; Holl, Peter; Rudek, Benedikt; Erk, Benjamin; Hömke, André; Reich, Christian; Pietschner, Daniel; Weidenspointner, Georg; Strüder, Lothar; Hauser, Günter; Gorke, Hubert; Ullrich, Joachim; Schlichting, Ilme; Herrmann, Sven; Schaller, Gerhard; Schopper, Florian; Soltau, Heike; Kühnel, Kai-Uwe; Andritschke, Robert; Schröter, Claus-Dieter; Krasniqi, Faton; Bott, Mario; Schorb, Sebastian; Rupp, Daniela; Adolph, Marcus; Gorkhover, Tais; Hirsemann, Helmut; Potdevin, Guillaume; Graafsma, Heinz; Nilsson, Björn; Chapman, Henry N.; Hajdu, Janos

2014-01-01

X-ray lasers offer new capabilities in understanding the structure of biological systems, complex materials and matter under extreme conditions1–4. Very short and extremely bright, coherent X-ray pulses can be used to outrun key damage processes and obtain a single diffraction pattern from a large macromolecule, a virus or a cell before the sample explodes and turns into plasma1. The continuous diffraction pattern of non-crystalline objects permits oversampling and direct phase retrieval2. Here we show that high-quality diffraction data can be obtained with a single X-ray pulse from a non-crystalline biological sample, a single mimivirus particle, which was injected into the pulsed beam of a hard-X-ray free-electron laser, the Linac Coherent Light Source5. Calculations indicate that the energy deposited into the virus by the pulse heated the particle to over 100,000 K after the pulse had left the sample. The reconstructed exit wavefront (image) yielded 32-nm full-period resolution in a single exposure and showed no measurable damage. The reconstruction indicates inhomogeneous arrangement of dense material inside the virion. We expect that significantly higher resolutions will be achieved in such experiments with shorter and brighter photon pulses focused to a smaller area. The resolution in such experiments can be further extended for samples available in multiple identical copies. PMID:21293374

Development and calibration of mirrors and gratings for the Soft X-ray materials science beamline at the Linac Coherent Light Source free-electron laser

DOE PAGES

Soufli, Regina; Fernandez-Perea, Monica; Baker, Sherry L.; ...

2012-04-18

This article discusses the development and calibration of the x-ray reflective and diffractive elements for the Soft X-ray Materials Science (SXR) beamline of the Linac Coherent Light Source (LCLS) free-electron laser (FEL), designed for operation in the 500 – 2000 eV region. The surface topography of three Si mirror substrates and two Si diffraction grating substrates was examined by atomic force microscopy (AFM) and optical profilometry. The figure of the mirror substrates was also verified via surface slope measurements with a long trace profiler. A boron carbide (B 4C) coating especially optimized for the LCLS FEL conditions was deposited onmore » all SXR mirrors and gratings. Coating thickness uniformity of 0.14 nm root mean square (rms) across clear apertures extending to 205 mm length was demonstrated for all elements, as required to preserve the coherent wavefront of the LCLS source. The reflective performance of the mirrors and the diffraction efficiency of the gratings were calibrated at beamline 6.3.2 at the Advanced Light Source synchrotron. To verify the integrity of the nanometer-scale grating structure, the grating topography was examined by AFM before and after coating. This is to our knowledge the first time B 4C-coated diffraction gratings are demonstrated for operation in the soft x-ray region.« less

Real-time and sub-wavelength ultrafast coherent diffraction imaging in the extreme ultraviolet.

PubMed

Zürch, M; Rothhardt, J; Hädrich, S; Demmler, S; Krebs, M; Limpert, J; Tünnermann, A; Guggenmos, A; Kleineberg, U; Spielmann, C

2014-12-08

Coherent Diffraction Imaging is a technique to study matter with nanometer-scale spatial resolution based on coherent illumination of the sample with hard X-ray, soft X-ray or extreme ultraviolet light delivered from synchrotrons or more recently X-ray Free-Electron Lasers. This robust technique simultaneously allows quantitative amplitude and phase contrast imaging. Laser-driven high harmonic generation XUV-sources allow table-top realizations. However, the low conversion efficiency of lab-based sources imposes either a large scale laser system or long exposure times, preventing many applications. Here we present a lensless imaging experiment combining a high numerical aperture (NA = 0.8) setup with a high average power fibre laser driven high harmonic source. The high flux and narrow-band harmonic line at 33.2 nm enables either sub-wavelength spatial resolution close to the Abbe limit (Δr = 0.8λ) for long exposure time, or sub-70 nm imaging in less than one second. The unprecedented high spatial resolution, compactness of the setup together with the real-time capability paves the way for a plethora of applications in fundamental and life sciences.

Structural, Morphological, Differential Scanning Calorimetric and Thermogravimetric Studies of Ball Milled Fe Doped Nanoscale La0.67Sr0.33MnO3 Manganite

NASA Astrophysics Data System (ADS)

Astik, Nidhi; Jha, Prafulla K.; Pratap, Arun

2018-03-01

The ball milling route has been used to produce the La0.67Sr0.33Mn0.85Fe0.15O3 (LSMFO) nanocrystalline sample from oxide precursors. The sample was characterized using x-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDAX), differential scanning calorimetry (DSC) and thermogravimetric (TGA) measurements. The x-ray diffraction confirms the phase purity of sample and shows that the sample crystallizes in the rhombohedral perovskite structure with a R-3c space group. The scanning electron micrograph shows the presence of well-faceted crystallites of LSMFO. The EDAX spectrum demonstrates the molar ratio of different elements of nanocrystalline LSMFO. Furthermore, the crystallite size using the Debye-Scherrer formula and William-Hall analysis has been found as 24 nm and 29 nm, respectively. Our results support the idea that a good quality nanocrystalline LSMFO sample can be obtained using the ball milling route. We also discuss the DSC and TGA curves and analyse the results in terms of phase transition, calcination temperature and activation barrier energies.

Green biosynthesis of silver nanoparticles using Curcuma longa tuber powder

PubMed Central

Shameli, Kamyar; Ahmad, Mansor Bin; Zamanian, Ali; Sangpour, Parvanh; Shabanzadeh, Parvaneh; Abdollahi, Yadollah; Zargar, Mohsen

2012-01-01

Green synthesis of noble metal nanoparticles is a vastly developing area of research. Metallic nanoparticles have received great attention from chemists, physicists, biologists, and engineers who wish to use them for the development of a new-generation of nanodevices. In this study, silver nanoparticles were biosynthesized from aqueous silver nitrate through a simple and eco-friendly route using Curcuma longa tuber-powder extracts, which acted as a reductant and stabilizer simultaneously. Characterizations of nanoparticles were done using different methods, which included ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray fluorescence spectrometry, and Fourier-transform infrared spectroscopy. The ultraviolet-visible spectrum of the aqueous medium containing silver nanoparticles showed an absorption peak at around 415 nm. Transmission electron microscopy showed that mean diameter and standard deviation for the formation of silver nanoparticles was 6.30 ± 2.64 nm. Powder X-ray diffraction showed that the particles are crystalline in nature, with a face-centered cubic structure. The most needed outcome of this work will be the development of value-added products from C. longa for biomedical and nanotechnology-based industries. PMID:23341739

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

Hosseinizadeh, Ahmad; Mashayekhi, Ghoncheh; Copperman, Jeremy

Using a manifold-based analysis of experimental diffraction snapshots from an X-ray free electron laser, we determine the three-dimensional structure and conformational landscape of the PR772 virus to a detector-limited resolution of 9 nm. Our results indicate that a single conformational coordinate controls reorganization of the genome, growth of a tubular structure from a portal vertex and release of the genome. Furthermore, these results demonstrate that single-particle X-ray scattering has the potential to shed light on key biological processes.

Enhancement of soft X-ray reflectivity and interface stability in nitridated Pd/Y multilayer mirrors.

PubMed

Xu, Dechao; Huang, Qiushi; Wang, Yiwen; Li, Pin; Wen, Mingwu; Jonnard, Philippe; Giglia, Angelo; Kozhevnikov, Igor V; Wang, Kun; Zhang, Zhong; Wang, Zhanshan

2015-12-28

Pd/Y multilayer mirrors operating in the soft X-ray region are characterized by a high theoretical reflectance, reaching 65% at normal incidence in the 8-12 nm wavelength range. However, a severe intermixing of neighboring Pd and Y layers results in an almost total disappearance of the interfaces inside the multilayer structures fabricated by direct current magnetron sputtering and thus a dramatic reflectivity decrease. Based on grazing incidence X-ray reflectometry and X-ray photoelectron spectroscopy, we demonstrate that the stability of the interfaces in Pd/Y multilayer structures can be essentially improved by adding a small amount of nitrogen (4-8%) to the working gas (Ar). High resolution transmission electron microscopy shows that the interlayer width is only 0.9 nm and 0.6 nm for Y(N)-on-Pd(N) and Pd(N)-on-Y(N) interfaces, respectively. A well-defined crystalline texture of YN (200) is observed on the electron diffraction pattern. As a result, the measured reflectance of the Pd(N)/Y(N) multilayer achieves 30% at λ = 9.3 nm. The peak reflectivity value is limited by the remaining interlayers and the formation of the YN compound inside the yttrium layers, resulting in an increased absorption.

Dopant concentration dependent optical and X-Ray induced photoluminescence in Eu3+ doped La2Zr2O7

NASA Astrophysics Data System (ADS)

Pokhrel, Madhab; Brik, Mikhail; Mao, Yuanbing

2015-03-01

Herein, we will be presenting the dopant (Eu) concentration dependent high density La2Zr2O7 nanoparticles for optical and X-ray scintillation applications by use of X - ray diffraction, Raman, FTIR, scanning electron microscope (SEM), transmission electron microscopy (TEM), optically and X-ray excited photoluminescence (PL). Several theoretical methods have been used in order to investigate the structural, electronic, optical, elastic, dynamic properties of Eu doped La2Zr2O7. It is observed that Eu: La2Zr2O7 shows an intense red luminescence under 258, 322, 394 and 465 nm excitation. The optical intensity of Eu: La2Zr2O7 depends on the dopant concentration of Eu3+. Following high energy excitation with X-rays, Eu: La2Zr2O7 shows an atypical Eu PL response (scintillation) with a red emission. The intense color emission of Eu obtained under 258 nm excitation, the X-ray induced luminescence property along with reportedly high density of La2Zr2O7, makes these nanomaterials attractive for optical and X-ray applications. The authors thank the support from the Defense Threat Reduction Agency (DTRA) of the U.S. Department of Defense (Award #HDTRA1-10-1-0114).

Diffraction leveraged modulation of X-ray pulses using MEMS-based X-ray optics

DOEpatents

Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

2016-08-09

A method and apparatus are provided for implementing Bragg-diffraction leveraged modulation of X-ray pulses using MicroElectroMechanical systems (MEMS) based diffractive optics. An oscillating crystalline MEMS device generates a controllable time-window for diffraction of the incident X-ray radiation. The Bragg-diffraction leveraged modulation of X-ray pulses includes isolating a particular pulse, spatially separating individual pulses, and spreading a single pulse from an X-ray pulse-train.

ZnS nanostructured thin-films deposited by successive ionic layer adsorption and reaction

NASA Astrophysics Data System (ADS)

Deshmukh, S. G.; Jariwala, Akshay; Agarwal, Anubha; Patel, Chetna; Panchal, A. K.; Kheraj, Vipul

2016-04-01

ZnS thin films were grown on glass substrate using successive ionic layer adsorption and reaction (SILAR) technique at room temperature. Aqueous solutions of ZnCl2 and Na2S were used as precursors. The X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), Raman spectroscopy and optical absorption measurements were applied to study the structural, surface morphology and optical properties of as-deposited ZnS thin films. The X-ray diffraction profiles revealed that ZnS thin films consist of crystalline grains with cubic phase. Spherical nano grains of random size and well covered on the glass substrate were observed from FESEM. The average grain size were found to be 77 nm, 100 nm and 124 nm for 20 cycles, 40 cycles and 60 cycles samples respectively. For 60 cycle sample, Raman spectra show two prominent peaks at 554 cm-1 and 1094 cm-1. The optical band gap values were found to be 3.76 eV, 3.72 eV and 3.67 eV for 20 cycle, 40 cycle and 60 cycle samples respectively.

In Vitro Sustained Release Study of Gallic Acid Coated with Magnetite-PEG and Magnetite-PVA for Drug Delivery System

PubMed Central

Kura, Aminu Umar; Hussein-Al-Ali, Samer Hasan; Bin Hussein, Mohd Zobir; Fakurazi, Sharida; Shaari, Abdul Halim; Ahmad, Zalinah

2014-01-01

The efficacy of two nanocarriers polyethylene glycol and polyvinyl alcohol magnetic nanoparticles coated with gallic acid (GA) was accomplished via X-ray diffraction, infrared spectroscopy, magnetic measurements, thermal analysis, and TEM. X-ray diffraction and TEM results showed that Fe3O4 nanoparticles were pure iron oxide having spherical shape with the average diameter of 9 nm, compared with 31 nm and 35 nm after coating with polyethylene glycol-GA (FPEGG) and polyvinyl alcohol-GA (FPVAG), respectively. Thermogravimetric analyses proved that after coating the thermal stability was markedly enhanced. Magnetic measurements and Fourier transform infrared (FTIR) revealed that superparamagnetic iron oxide nanoparticles could be successfully coated with two polymers (PEG and PVA) and gallic acid as an active drug. Release behavior of gallic acid from two nanocomposites showed that FPEGG and FPVAG nanocomposites were found to be sustained and governed by pseudo-second-order kinetics. Anticancer activity of the two nanocomposites shows that the FPEGG demonstrated higher anticancer effect on the breast cancer cell lines in almost all concentrations tested compared to FPVAG. PMID:24737969

Coherent X-Ray Diffraction Imaging of Chloroplasts from Cyanidioschyzon merolae by Using X-Ray Free Electron Laser.

PubMed

Takayama, Yuki; Inui, Yayoi; Sekiguchi, Yuki; Kobayashi, Amane; Oroguchi, Tomotaka; Yamamoto, Masaki; Matsunaga, Sachihiro; Nakasako, Masayoshi

2015-07-01

Coherent X-ray diffraction imaging (CXDI) is a lens-less technique for visualizing the structures of non-crystalline particles with the dimensions of submicrometer to micrometer at a resolution of several tens of nanometers. We conducted cryogenic CXDI experiments at 66 K to visualize the internal structures of frozen-hydrated chloroplasts of Cyanidioschyzon merolae using X-ray free electron laser (XFEL) as a coherent X-ray source. Chloroplast dispersed specimen disks at a number density of 7/(10×10 µm(2)) were flash-cooled with liquid ethane without staining, sectioning or chemical labeling. Chloroplasts are destroyed at atomic level immediately after the diffraction by XFEL pulses. Thus, diffraction patterns with a good signal-to-noise ratio from single chloroplasts were selected from many diffraction patterns collected through scanning specimen disks to provide fresh specimens into the irradiation area. The electron density maps of single chloroplasts projected along the direction of the incident X-ray beam were reconstructed by using the iterative phase-retrieval method and multivariate analyses. The electron density map at a resolution of 70 nm appeared as a C-shape. In addition, the fluorescence image of proteins stained with Flamingo™ dye also appeared as a C-shape as did the autofluorescence from Chl. The similar images suggest that the thylakoid membranes with an abundance of proteins distribute along the outer membranes of chloroplasts. To confirm the present results statistically, a number of projection structures must be accumulated through high-throughput data collection in the near future. Based on the results, we discuss the feasibility of XFEL-CXDI experiments in the structural analyses of cellular organelles. © The Author 2015. Published by Oxford University Press on behalf of Japanese Society of Plant Physiologists. All rights reserved. For permissions, please email: journals.permissions@oup.com.

Three-Dimensional Reconstruction of the Giant Mimivirus Particle with an X-Ray Free-Electron Laser (CXIDB ID 30)

DOE Data Explorer

Ekeberg, Tomas

2015-05-26

This dataset contains the diffraction patterns that were used for the first three-dimensional reconstruction of a virus using FEL data. The sample was the giant mimivirus particle, which is one of the largest known viruses with a diameter of 450 nm. The dataset consists of the 198 diffraction patterns that were used in the analysis.

Transmission Grating and Optics Technology Development for the Arcus Explorer Mission

NASA Astrophysics Data System (ADS)

Heilmann, Ralf; Arcus Team

2018-01-01

Arcus is a high-resolution x-ray spectroscopy MIDEX mission selected for a Phase A concept study. It is designed to explore structure formation through measurements of hot baryon distributions, feedback from black holes, and the formation and evolution of stars, disks, and exoplanet atmospheres. The design provides unprecedented sensitivity in the 1.2-5 nm wavelength band with effective area above 450 sqcm and spectral resolution R > 2500. The Arcus technology is based on 12 m-focal length silicon pore optics (SPO) developed for the European Athena mission, and critical-angle transmission (CAT) x-ray diffraction gratings and x-ray CCDs developed at MIT. The modular design consists of four parallel channels, each channel holding an optics petal, followed by a grating petal. CAT gratings are lightweight, alignment insensitive, high-efficiency x-ray transmission gratings that blaze into high diffraction orders, leading to high spectral resolution. Each optics petal represents an azimuthal sub-aperture of a full Wolter optic. The sub-aperturing effect increases spectral resolving power further. Two CCD readout strips receive photons from each channel, including higher-energy photons in 0th order. Each optics petal holds 34 SPO modules. Each grating petal holds 34 grating windows, and each window holds 4-6 grating facets. A grating facet consists of a silicon grating membrane, bonded to a flexure frame that interfaces with the grating window. We report on a sequence of tests with increasing complexity that systematically increase the Technology Readiness Level (TRL) for the combination of CAT gratings and SPOs towards TLR 6. CAT gratings have been evaluated in x rays for diffraction efficiency (> 30% at 2.5 nm) and for resolving power (R> 10,000). A CAT grating/SPO combination was measured at R ~ 3100 at blaze angles smaller than design values, exceeding Arcus requirements. Efficiency and resolving power were not impacted by vibration and thermal testing of gratings. A pair of large (32 mm x 32 mm) gratings was aligned using laser metrology, and alignment was verified under x rays. We present results on simultaneous illumination of the aligned grating pair, and describe our progress towards further tests.

Coherent x-ray diffraction

NASA Astrophysics Data System (ADS)

Pitney, John Allen

Conventional x-ray diffraction has historically been done under conditions such that the measured signal consists of an incoherent addition of scattering which is coherent only on a length scale determined by the properties of the beam. The result of the incoherent summation is a statistical averaging over the whole illuminated volume of the sample, which yields certain kinds of information with a high degree of precision and has been key to the success of x-ray diffraction in a variety of applications. Coherent x-ray scattering techniques, such as coherent x-ray diffraction (CXD) and x-ray intensity fluctuation spectroscopy (XIFS), attempt to reduce or eliminate any incoherent averaging so that specific, local structures couple to the measurement without being averaged out. In the case of XIFS, the result is analogous to dynamical light scattering, but with sensitivity to length scales less than 200 nm and time scales from 10-3 s to 103 s. When combined with phase retrieval, CXD represents an imaging technique with the penetration, in situ capabilities, and contrast mechanisms associated with x-rays and with a spatial resolution ultimately limited by the x-ray wavelength. In practice, however, the spatial resolution of CXD imaging is limited by exposure to about 100 A. This thesis describes CXD measurements of the binary alloy Cu3Au and the adaptation of phase retrieval methods for the reconstruction of real-space images of Cu3Au antiphase domains. The theoretical foundations of CXD are described in Chapter 1 as derived from the kinematical formulation for x-ray diffraction and from the temporal and spatial coherence of radiation. The antiphase domain structure of Cu 3Au is described, along with the associated reciprocal-space structure which is measured by CXD. CXD measurements place relatively stringent requirements on the coherence properties of the beam and on the detection mechanism of the experiment; these requirements and the means by which they have been met are delineated in Chapter 2. The results and interpretation of a set of Cu 3Au measurements are presented in Chapter 3. Chapter 4 describes the Gerchberg-Saxton and the hybrid input-output (HIO) algorithms for phase retrieval and shows the results of image reconstruction tests with simulated Cu 3Au CXD, including the effect of oversampling in reciprocal space.

Determination of dislocation density by electron backscatter diffraction and X-ray line profile analysis in ferrous lath martensite

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

Berecz, Tibor, E-mail: berecz@eik.bme.hu; Jenei, Péter, E-mail: jenei@metal.elte.hu; Csóré, András, E-mail: csorean@gmail.com

2016-03-15

The microstructure and the dislocation density in as-quenched ferrous lath martensite were studied by different methods. The blocks, packets and variants formed due to martensitic transformation were identified and their sizes were determined by electron backscatter diffraction (EBSD). Concomitant transmission electron microscopy (TEM) investigation revealed that the laths contain subgrains with the size between 50 and 100 nm. A novel evaluation procedure of EBSD images was elaborated for the determination of the density and the space distribution of geometrically necessary dislocations from the misorientation distribution. The total dislocation density obtained by X-ray diffraction line profile analysis was in good agreementmore » with the value determined by EBSD, indicating that the majority of dislocations formed due to martensitic transformation during quenching are geometrically necessary dislocations.« less

Epitaxially Grown Films of Standing and Lying Pentacene Molecules on Cu(110) Surfaces

PubMed Central

2011-01-01

Here, it is shown that pentacene thin films (30 nm) with distinctively different crystallographic structures and molecular orientations can be grown under essentially identical growth conditions in UHV on clean Cu(110) surfaces. By X-ray diffraction, we show that the epitaxially oriented pentacene films crystallize either in the “thin film” phase with standing molecules or in the “single crystal” structure with molecules lying with their long axes parallel to the substrate. The morphology of the samples observed by atomic force microscopy shows an epitaxial alignment of pentacene crystallites, which corroborates the molecular orientation observed by X-ray diffraction pole figures. Low energy electron diffraction measurements reveal that these dissimilar growth behaviors are induced by subtle differences in the monolayer structures formed by slightly different preparation procedures. PMID:21479111

Size effect on multiferroic TbMn{sub 2}O{sub 5} nanorods

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

Yang, Chun-Chuen, E-mail: chunchuenyang@cycu.edu.tw; Tung, Yung-Hsiang; Hsu, Ting-Wei

2015-05-07

The effect of the size of TbMn{sub 2}O{sub 5} on their magnetoelectric properties is studied using a field emission transmission electron microscope, ac magnetic susceptibility, relative dielectric constant, specific heat capacity, and x-ray diffraction at various temperatures. A bulk sample and nanorods with two axial lengths, 〈L{sub C}〉, are investigated. Nanorods with 〈L{sub C}〉 of 216 nm and 64 nm crystallize with orthorhombic Pbam symmetry as the bulk material. The axial direction of the two sizes of nanorod is parallel to the c axis of the crystal. No particular radial direction is observed. The critical size for the magnetic ordering of TbMn{submore » 2}O{sub 5} is found to be between 〈L{sub C}〉 = 64 nm and 216 nm. Experiments on specific heat capacity verified these results. No similar phenomenon concerning the ferroelectric property is observed. At T = 30 K and 35 K, the 〈L{sub C}〉 = 216 nm sample yields a charge-ordering-like x-ray diffraction peak, which may be associated with the magnetically induced charge ordering superlattice.« less

The Circularization of Amyloid Fibrils Formed by Apolipoprotein C-II

PubMed Central

Hatters, Danny M.; MacRaild, Christopher A.; Daniels, Rob; Gosal, Walraj S.; Thomson, Neil H.; Jones, Jonathan A.; Davis, Jason J.; MacPhee, Cait E.; Dobson, Christopher M.; Howlett, Geoffrey J.

2003-01-01

Amyloid fibrils have historically been characterized by diagnostic dye-binding assays, their fibrillar morphology, and a “cross-β” x-ray diffraction pattern. Whereas the latter demonstrates that amyloid fibrils have a common β-sheet core structure, they display a substantial degree of morphological variation. One striking example is the remarkable ability of human apolipoprotein C-II amyloid fibrils to circularize and form closed rings. Here we explore in detail the structure of apoC-II amyloid fibrils using electron microscopy, atomic force microscopy, and x-ray diffraction studies. Our results suggest a model for apoC-II fibrils as ribbons ∼2.1-nm thick and 13-nm wide with a helical repeat distance of 53 nm ± 12 nm. We propose that the ribbons are highly flexible with a persistence length of 36 nm. We use these observed biophysical properties to model the apoC-II amyloid fibrils either as wormlike chains or using a random-walk approach, and confirm that the probability of ring formation is critically dependent on the fibril flexibility. More generally, the ability of apoC-II fibrils to form rings also highlights the degree to which the common cross-β superstructure can, as a function of the protein constituent, give rise to great variation in the physical properties of amyloid fibrils. PMID:14645087

Luminescent silver(I) tert-butylethynide compounds with nicotinic/isonicotinic acid as ligands

NASA Astrophysics Data System (ADS)

Xie, Yi-Ming; Fan, Yue-Yue; Lin, Fu-Lin; Hu, Ting; Liu, Jia; Lu, Can-Zhong

2017-12-01

Solvothermal reaction of tBuC≡CAg, AgBF4 and nicotinic/isonicotinic acid in acetonitrile afforded two new silver(I) tert-butylethynide double salts, namely [(tBuC≡CAg)(AgL1)3] (HL1 = nicotinic acid) (1) and [(tBuC≡CAg)(AgL1)2] (HL2 = isonicotinic acid) (2). These compounds have been characterized by elemental analysis, infrared spectra, single-crystal X-ray analysis, X-ray powder diffraction, thermogravimetric analysis, UV-visible absorption spectra, and luminescent measurement. 1 exhibits a two-dimensional coordination network, and 2 features a three-dimensional coordination architecture. Luminescence measurements indicate that 1 shows a fluorescent emission band centered at 568 nm, and 2 exhibits an intense emission maximum at 550 nm and a shoulder peak at 436 nm.

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.; ...

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

Ionic liquid-templated preparation of mesoporous silica embedded with nanocrystalline sulfated zirconia

PubMed Central

2011-01-01

A series of mesoporous silicas impregnated with nanocrystalline sulphated zirconia was prepared by a sol-gel process using an ionic liquid-templated route. The physicochemical properties of the mesoporous sulphated zirconia materials were studied using characterisation techniques such as inductively coupled optical emission spectroscopy, X-ray diffraction, transmission electron microscopy, energy-dispersive X-ray microanalysis, elemental analysis and X-ray photoelectron spectroscopy. Analysis of the new silicas indicates isomorphous substitution of silicon with zirconium and reveals the presence of extremely small (< 10 nm) polydispersed zirconia nanoparticles in the materials with zirconium loadings from 27.77 to 41.4 wt.%. PMID:21711725

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

NASA Astrophysics Data System (ADS)

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

2013-10-01

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

Rietveld analysis of the cubic crystal structure of Na-stabilized zirconia

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

Fagherazzi, G.; Canton, P.; Benedetti, A.

Using x-ray Rietveld analysis the fcc (fluorite-type) structure of a Na-containing nanocrystalline zirconia powder (9.5 nm estimated of crystallite size) obtained by precipitation and subsequent calcination has been confirmed. The result shows that using conventional x-ray diffraction techniques the cubic crystallographic form of ZrO{sub 2} from the tetragonal one in nanosized powders. These conclusions are supported by the findings of independent Raman scattering experiments. {copyright} {ital 1997 Materials Research Society.}

Pressure-induced phase transition in GaN nanocrystals

NASA Astrophysics Data System (ADS)

Cui, Q.; Pan, Y.; Zhang, W.; Wang, X.; Zhang, J.; Cui, T.; Xie, Y.; Liu, J.; Zou, G.

2002-11-01

High-pressure in situ energy-dispersive x-ray diffraction experiments on GaN nanocrystals with 50 nm diameter have been carried out using a synchrotron x-ray source and a diamond-anvil cell up to about 79 GPa at room temperature. A pressure-induced first-order structural phase transition from the wurtzite-type structure to the rock-salt-type structure starts at about 48.8 GPa. The rock-salt-type phase persists to the highest pressure in our experimental range.

Laser-driven powerful kHz hard x-ray source

NASA Astrophysics Data System (ADS)

Li, Minghua; Huang, Kai; Chen, Liming; Yan, Wenchao; Tao, Mengze; Zhao, Jiarui; Ma, Yong; Li, Yifei; Zhang, Jie

2017-08-01

A powerful hard x-ray source based on laser plasma interaction is developed. By introducing the kHz, 800 nm pulses onto a rotating molybdenum (Mo) disk target, intense Mo Kα x-rays are emitted with suppressed bremsstrahlung background. Results obtained with different laser intensities suggest that the dominant absorption mechanism responsible for the high conversion efficiency is vacuum heating (VH). The high degree of spatial coherence is verified. With the high average flux and a source size comparable to the laser focus spot, absorption contrast imaging and phase contrast imaging are carried out to test the imaging capability of the source. Not only useful for imaging application, this compact x-ray source is also holding great potential for ultrafast x-ray diffraction (XRD) due to the intrinsic merits such as femtosecond pulse duration and natural synchronization with the driving laser pulses.

Fabrication of luminescent SrWO{sub 4} thin films by a novel electrochemical method

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

Chen Lianping; Gao Yuanhong

2007-10-02

Highly crystallized SrWO{sub 4} thin films with single scheelite structure were prepared within 60 min by a cell electrochemical method. X-ray diffraction analysis shows that SrWO{sub 4} thin films have a tetragonal structure. Scanning electron microscopy examinations reveal that SrWO{sub 4} grains grow well in tetragonal tapers and grains like flowers or bunches, which can usually form by using the electrolysis electrochemical method, have disappeared under cell electrochemical conditions. X-ray photoelectron spectra and energy dispersive X-ray microanalysis examinations demonstrate that the composition of the film is consistent with its stoichiometry. These SrWO{sub 4} films show a single blue emission peakmore » (located at 460 nm) using an excitation wave of 230 nm. The speed of cell electrochemical method can be controlled by changing temperature. The optimum treatment temperature is about 50-60 deg. C.« less

High numerical aperture multilayer Laue lenses

DOE PAGES

Morgan, Andrew J.; Prasciolu, Mauro; Andrejczuk, Andrzej; ...

2015-06-01

The ever-increasing brightness of synchrotron radiation sources demands improved X-ray optics to utilise their capability for imaging and probing biological cells, nanodevices, and functional matter on the nanometer scale with chemical sensitivity. Here we demonstrate focusing a hard X-ray beam to an 8 nm focus using a volume zone plate (also referred to as a wedged multilayer Laue lens). This lens was constructed using a new deposition technique that enabled the independent control of the angle and thickness of diffracting layers to microradian and nanometer precision, respectively. This ensured that the Bragg condition is satisfied at each point along themore » lens, leading to a high numerical aperture that is limited only by its extent. We developed a phase-shifting interferometric method based on ptychography to characterise the lens focus. The precision of the fabrication and characterisation demonstrated here provides the path to efficient X-ray optics for imaging at 1 nm resolution.« less

Nanoparticles of nickel oxide: growth and organization on zinc-substituted anionic clay matrix by one-pot route at room temperature

NASA Astrophysics Data System (ADS)

Carja, Gabriela; Nakajima, Akira; Dranca, Cristian; Okada, Kiyoshi

2010-10-01

A room temperature nanocarving strategy is developed for the fabrication of nanoparticles of nickel oxide on zinc-substituted anionic clay matrix (Ni/ZnLDH). It is based on the growth and organization of nanoparticles of nickel oxide which occur during the structural reconstruction of the layered structure of the anionic clay in NiSO4 aqueous solution. No organic compounds are used during the fabrication. The described material was characterized by X-ray diffraction (XRD), IR spectroscopy (FTIR), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) spectroscopy, and X-ray photoelectron spectroscopy (XPS). Results show that the nickel-clay nanoarchitecture consists of small nanoparticles of nickel oxide (average size 7 nm) deposited on the larger nanoparticles (average size 90 nm) of zinc-substituted clay. The optical properties of the new nickel-zinc formulation are studied by UV-Vis.

Spectral characterization and white light generation by yttrium silicate nanopowders undoped and doped with Ytterbium(III) at different concentrations when excited by a laser diode at 975 nm

NASA Astrophysics Data System (ADS)

Cinkaya, Hatun; Eryurek, Gonul; Bilir, Gokhan; Collins, John; Di Bartolo, Baldassare

2017-01-01

We have studied nanophosphors of yttrium silicate (YSO) undoped and doped with different concentration of ytterbium (Yb3+) synthesized by using the sol-gel method. Structural and luminescence properties of the nanophosphors were studied experimentally by using different analytical techniques. For the structural analysis, we performed X-ray diffraction (XRD), Transmission Electron Microscopy (TEM) and Energy Dispersive X-ray Spectrometry (EDS) measurements. Upconversion (UC) and the white light (WL) emission properties were investigated by using the near infrared cw laser excitation of 975 nm. The spectral properties have been found to depend on several physical parameters.

Plasma in-liquid method for reduction of zinc oxide in zinc nanoparticle synthesis

NASA Astrophysics Data System (ADS)

Amaliyah, Novriany; Mukasa, Shinobu; Nomura, Shinfuku; Toyota, Hiromichi; Kitamae, Tomohide

2015-02-01

Metal air-batteries with high-energy density are expected to be increasingly applied in electric vehicles. This will require a method of recycling air batteries, and reduction of metal oxide by generating plasma in liquid has been proposed as a possible method. Microwave-induced plasma is generated in ethanol as a reducing agent in which zinc oxide is dispersed. Analysis by energy-dispersive x-ray spectrometry (EDS) and x-ray diffraction (XRD) reveals the reduction of zinc oxide. According to images by transmission electron microscopy (TEM), cubic and hexagonal metallic zinc particles are formed in sizes of 30 to 200 nm. Additionally, spherical fiber flocculates approximately 180 nm in diameter are present.

Soft x-ray coherent diffraction imaging on magnetic nanostructures

NASA Astrophysics Data System (ADS)

Shi, Xiaowen; Lee, James; Mishra, Shrawan; Parks, Daniel; Tyliszczak, Tolek; Shapiro, David; Roy, Sujoy; Kevan, Steve; Stxm Team At Als Collaboration; Soft X-Ray Microscopy Group At Als Collaboration; Soft X-ray scattering at ALS, LBL Team

2014-03-01

Coherent soft X-rays diffraction imaging enable coherent magnetic resonance scattering at transition metal L-edge to be probed so that magnetic domains could be imaged with very high spatial resolution with phase contrast, reaching sub-10nm. One of the overwhelming advantages of using coherent X-rays is the ability to resolve phase contrast images with linearly polarized light with both phase and absorption contrast comparing to real-space imaging, which can only be studied with circularly polarized light with absorption contrast only. Here we report our first results on high-resolution of magnetic domains imaging of CoPd multilayer thin film with coherent soft X-ray ptychography method. We are aiming to resolve and understand magnetic domain wall structures with the highest obtainable resolution here at Advanced Light Source. In principle types of magnetic domain walls could be studied so that Neel or Bloch walls can be distinguished by imaging. This work at LBNL was supported by the Director, Office of Science, Office of Basic Energy Sciences, of the US Department of Energy (contract no. DE-AC02- 05CH11231).

A next-generation in-situ nanoprobe beamline for the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Maser, Jörg; Lai, Barry; Buonassisi, Tonio; Cai, Zhonghou; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Harder, Ross; Jacobsen, Chris; Liu, Wenjun; Murray, Conal; Preissner, Curt; Roehrig, Chris; Rose, Volker; Shu, Deming; Vine, David; Vogt, Stefan

2013-09-01

The Advanced Photon Source is currently developing a suite of new hard x-ray beamlines, aimed primarily at the study of materials and devices under real conditions. One of the flagship beamlines of the APS Upgrade is the In-Situ Nanoprobe beamline (ISN beamline), which will provide in-situ and operando characterization of advanced energy materials and devices under change of temperature and gases, under applied fields, in 3D. The ISN beamline is designed to deliver spatially coherent x-rays with photon energies between 4 keV and 30 keV to the ISN instrument. As an x-ray source, a revolver-type undulator with two interchangeable magnetic structures, optimized to provide high brilliance throughout the range of photon energies of 4 keV - 30 keV, will be used. The ISN instrument will provide a smallest hard x-ray spot of 20 nm using diffractive optics, with sensitivity to sub-10 nm sample structures using coherent diffraction. Using nanofocusing mirrors in Kirkpatrick-Baez geometry, the ISN will also provide a focus of 50 nm with a flux of 8·1011 Photons/s at a photon energy of 10 keV, several orders of magnitude larger than what is currently available. This will allow imaging of trace amounts of most elements in the periodic table, with a sensitivity to well below 100 atoms for most metals in thin samples. It will also enable nanospectroscopic studies of the chemical state of most materials relevant to energy science. The ISN beamline will be primarily used to study inorganic and organic photovoltaic systems, advanced batteries and fuel cells, nanoelectronics devices, and materials and systems diesigned to reduce the environmental impact of combustion.

Measuring and modeling diffuse scattering in protein X-ray crystallography

PubMed Central

Van Benschoten, Andrew H.; Liu, Lin; Gonzalez, Ana; Brewster, Aaron S.; Sauter, Nicholas K.; Wall, Michael E.

2016-01-01

X-ray diffraction has the potential to provide rich information about the structural dynamics of macromolecules. To realize this potential, both Bragg scattering, which is currently used to derive macromolecular structures, and diffuse scattering, which reports on correlations in charge density variations, must be measured. Until now, measurement of diffuse scattering from protein crystals has been scarce because of the extra effort of collecting diffuse data. Here, we present 3D measurements of diffuse intensity collected from crystals of the enzymes cyclophilin A and trypsin. The measurements were obtained from the same X-ray diffraction images as the Bragg data, using best practices for standard data collection. To model the underlying dynamics in a practical way that could be used during structure refinement, we tested translation–libration–screw (TLS), liquid-like motions (LLM), and coarse-grained normal-modes (NM) models of protein motions. The LLM model provides a global picture of motions and was refined against the diffuse data, whereas the TLS and NM models provide more detailed and distinct descriptions of atom displacements, and only used information from the Bragg data. Whereas different TLS groupings yielded similar Bragg intensities, they yielded different diffuse intensities, none of which agreed well with the data. In contrast, both the LLM and NM models agreed substantially with the diffuse data. These results demonstrate a realistic path to increase the number of diffuse datasets available to the wider biosciences community and indicate that dynamics-inspired NM structural models can simultaneously agree with both Bragg and diffuse scattering. PMID:27035972

Measuring and modeling diffuse scattering in protein X-ray crystallography

DOE PAGES

Van Benschoten, Andrew H.; Liu, Lin; Gonzalez, Ana; ...

2016-03-28

X-ray diffraction has the potential to provide rich information about the structural dynamics of macromolecules. To realize this potential, both Bragg scattering, which is currently used to derive macromolecular structures, and diffuse scattering, which reports on correlations in charge density variations, must be measured. Until now, measurement of diffuse scattering from protein crystals has been scarce because of the extra effort of collecting diffuse data. Here, we present 3D measurements of diffuse intensity collected from crystals of the enzymes cyclophilin A and trypsin. The measurements were obtained from the same X-ray diffraction images as the Bragg data, using best practicesmore » for standard data collection. To model the underlying dynamics in a practical way that could be used during structure refinement, we tested translation–libration–screw (TLS), liquid-like motions (LLM), and coarse-grained normal-modes (NM) models of protein motions. The LLM model provides a global picture of motions and was refined against the diffuse data, whereas the TLS and NM models provide more detailed and distinct descriptions of atom displacements, and only used information from the Bragg data. Whereas different TLS groupings yielded similar Bragg intensities, they yielded different diffuse intensities, none of which agreed well with the data. In contrast, both the LLM and NM models agreed substantially with the diffuse data. In conclusion, these results demonstrate a realistic path to increase the number of diffuse datasets available to the wider biosciences community and indicate that dynamics-inspired NM structural models can simultaneously agree with both Bragg and diffuse scattering.« less

Synthesis and spectroscopic study of CdS nanoparticles using hydrothermal method

NASA Astrophysics Data System (ADS)

AL-Mamoori, Mohammed H. K.; Mahdi, Dunia K.; Al-Shrefi, Saif M.

2018-05-01

In this work, cadmium sulfide nanoparticles (powder) with diameter 50.8 nm was prepared using hydrothermal method. The structural and optical properties of CdS nanoparticles was studied by X-ray diffraction, FESEM, EDS, FTIR, UV-Diffuse Reflectance spectroscopy and Photoluminance spectrum. X-ray diffraction reveal the formation the purity of prepared phase of CdS particles with hexagonal wurtzite structure with particle size 31.8nm by using sheerer equation. The energy dispersion scattering (EDS) examination explains that the sample is composed of a large amount of Cd and S which are exactly CdS nanoparticles and there is a very small trace of (Zn) and (O) element observed because of there is a small pollutions in the measurement place of samples. FESEM shows the spherical shape of nanoparticles with around 50.8 nm diameter. The optical absorption spectral study identified the red shift of the sample in comparison to bulk ZnO in three dimensions. Photoluminance spectrum (PL) at room temperature showed that there are two luminescence peaks at 433.14 nm and 518.21nm. Samples demonstrate a sharp emission band at around 433.18 nm, which is attributed to the typical exciton luminescence. The broad band at 518.21nm which were attributed to the trapped luminescence. The green emission band at 518.21 nm was associated with the emission due to electronic transition from the conduction band to an accepter level due to interstitial sulphur ion.

Structural analysis of nanocrystalline ZnTe alloys synthesized by melt quenching technique

NASA Astrophysics Data System (ADS)

Singh, Harinder; Singh, Tejbir; Thakur, Anup; Sharma, Jeewan

2018-05-01

Nanocrystalline ZnxTe100-x (x=0, 5, 20, 30, 40, 50) alloys have been synthesized using melt quenching technique. Energy-dispersive X-Ray spectroscopy (EDS) has been used to verify the elemental composition of samples. Various absorption modes are recorded from Fourier transform infrared spectroscopy (FTIR) confirming the formation of ZnTe. The structural study has been performed using X-Ray Diffraction (XRD) method. All synthesized samples have been found to be nanocrystalline in nature with average crystallite size in the range from 49.3 nm to 77.1 nm. Results have shown that Zn0Te100 exhibits hexagonal phase that transforms into a cubic ZnTe phase as the amount of zinc is increased. Pure ZnTe phase has been obtained for x = 50. The texture coefficient (Tc) has been calculated to find the prominent orientations of different planes.

XRD analysis of undoped and Fe doped TiO{sub 2} nanoparticles by Williamson Hall method

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

Bharti, Bandna; Barman, P. B.; Kumar, Rajesh, E-mail: rajesh.kumar@juit.ac.in

2015-08-28

Undoped and Fe doped titanium dioxide (TiO{sub 2}) nanoparticles were synthesized by sol-gel method at room temperature. The synthesized samples were annealed at 500°C. For structural analysis, the prepared samples were characterized by X-ray diffraction (XRD). The crystallite size of TiO{sub 2} and Fe doped TiO{sub 2} nanoparticles were calculated by Scherer’s formula, and was found to be 15 nm and 11 nm, respectively. Reduction in crystallite size of TiO{sub 2} with Fe doping was observed. The anatase phase of Fe-doped TiO{sub 2} nanoparticles was also confirmed by X-ray diffraction. By using Williamson-Hall method, lattice strain and crystallite size weremore » also calculated. Williamson–Hall plot indicates the presence of compressive strain for TiO{sub 2} and tensile strain for Fe-TiO{sub 2} nanoparticles annealed at 500°C.« less

A simple and low temperature process for super-hydrophilic rutile TiO 2 thin films growth

NASA Astrophysics Data System (ADS)

Mane, R. S.; Joo, Oh-Shim; Min, Sun-Ki; Lokhande, C. D.; Han, Sung-Hwan

2006-11-01

We investigate an environmentally friendly aqueous solution system for rutile TiO2 violet color nanocrystalline thin films growth on ITO substrate at room temperature. Film shows considerable absorption in visible region with excitonic maxima at 434 nm. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-vis, water surface contact angle and energy dispersive X-ray analysis (EDX) techniques in addition to actual photo-image that shows purely rutile phase of TiO2 with violet color, super-hydrophilic and densely packed nanometer-sized spherical grains of approximate diameter 3.15 ± 0.4 nm, characterize the films. Band gap energy of 4.61 eV for direct transition was obtained for the rutile TiO2 films. Film surface shows super-hydrophilic behavior, as exhibited water contact angle was 7°. Strong visible absorption (not due to chlorine) leaves future challenge to use these films in extremely thin absorber (ETA) solar cells.

Cadmium sulfide rod-bundle structures decorated with nanoparticles from an inorganic/organic composite

NASA Astrophysics Data System (ADS)

Pan, Jun; Xi, Baojuan; Li, Jingfa; Yan, Yan; Li, Qianwen; Qian, Yitai

2011-08-01

We report a new morphology of wurzite cadmium sulfide with nanoparticles decorated on rod-bundle structures, which were synthesized via calcinations of an inorganic/organic composite at 400 °C in air. The composite was hydrothermally synthesized at 180 °C using thioglycolic acid (TGA) and cadmium acetate as starting materials. The structure, composition, and morphology of the prepared material were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscope, FT-IR spectrometry, photoluminescence spectrometry, and UV-visible spectrometry. Results indicated that the composite could be defined as CdS 0.65/Cd-TGA0.35. X-ray diffraction revealed that the annealed product is CdS with wurtizite phase. The diameter of the rod is about 150-400 nm and the length from the top to the bottom of the decorated nanoparticle is about 100 nm. The composite showed high intensity of photoluminescence with similar peak position, compared to that of wurtzite CdS, because of the structure defects.

Structural and optical properties of ZnO thin films prepared by RF sputtering at different thicknesses

NASA Astrophysics Data System (ADS)

Hammad, Ahmed H.; Abdel-wahab, M. Sh.; Vattamkandathil, Sajith; Ansari, Akhalakur Rahman

2018-07-01

Hexagonal nanocrystallites of ZnO in the form of thin films were prepared by radio frequency sputtering technique. X-ray diffraction analysis reveals two prominent diffraction planes (002) and (103) at diffraction angles around 34.3 and 62.8°, respectively. The crystallite size increases through (103) plane from 56.1 to 64.8 Å as film thickness changed from 31 nm up to 280 nm while crystallites growth through (002) increased from 124 to 136 Å as film thickness varies from 31 to 107 nm and dropped to 115.8 Å at thickness 280 nm. The particle shape changes from spherical to longitudinal form. The particle size is 25 nm for films of thickness below 107 nm and increases at higher thicknesses (134 and 280 nm) from 30 to 40 nm, respectively. Optical band gap is deduced to be direct with values varied from 3.22 to 3.28 eV and the refractive index are evaluated based on the optical band values according to Moss, Ravindra-Srivastava, and Dimitrov-Sakka models. All refractive index models gave values around 2.3.

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

Singh, Paviter; Kaur, Manpreet; Singh, Bikramjeet

Boron-carbon core shell structures have been synthesized by solvo-thermal synthesis route. The synthesized material is highly pure. X-ray diffraction analysis confirms the reduction of reactants in to boron and carbon. Scanning Electron Microscopy (SEM) analysis showed that the shell is uniform with average thickness of 340 nm. Photo luminescence studies showed that the material is blue light emitting with CIE color coordinates: x=0.16085, y=0.07554.

Structural and photoluminescence properties of Ni doped CdS nanoparticles synthesis by sol gel method

NASA Astrophysics Data System (ADS)

Mahdi, Hadeel Salih; Parveen, Azra; Azam, Ameer

2018-05-01

Ni doped CdS nanoparticles have been successfully synthesized by sol-gel method. Nickel nitrate, cadmium nitrate, sodium sulfide has been used as precursors for the preparation of these Ni-doped CdS nanoparticles. The structural properties were studied by X-ray diffraction analysis. Surface morphology and the composition of the samples were studied by scanning electron microscope (SEM). The X-ray diffraction results revealed that the Ni-doped CdS nanoparticles were in hexagonal structure. The crystallite size was determined from Debye-Scherer equation and showed that the particle size increases with the doping of Ni. Optical absorption spectra of Ni doped CdS also was studied by Photoluminescence spectroscopy in the range of 200-600 nm.

Structural and optical properties of nanostructured nickel

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

Singh, J., E-mail: jaiveer24singh@gmail.com; Pandey, J.; Gupta, R.

2016-05-06

Metal nanoparticles are attractive because of their special structure and better optical properties. Nickel nanoparticles (Ni-Np) have been synthesized successfully by thermal decomposition method in the presence of trioctyl phosphine (TOP) and oleylamine (OAm). The samples were characterized by X-ray diffraction (XRD), Zetapotential measurement and Fourier transforms infrared (FTIR) spectroscopy. The size of Ni nanoparticles can be readily tuned from 13.86 nm. As-synthesized Ni nanoparticles have hexagonal closed pack (hcp) cubic structure as characterized by power X-ray diffraction (XRD) prepared at 280°C. The possible formation mechanism has also been phenomenological proposed for as synthesized Ni-Np. The value of Zeta potential wasmore » found 12.25 mV.« less

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

Berenguer de la Cuesta, Felisa; Wenger, Marco P.E.; Bean, Richard J.

Coherent X-ray diffraction has been applied in the imaging of inorganic materials with great success. However, its application to biological specimens has been limited to some notable exceptions, due to the induced radiation damage and the extended nature of biological samples, the last limiting the application of most part of the phasing algorithms. X-ray ptychography, still under development, is a good candidate to overcome such difficulties and become a powerful imaging method for biology. We describe herein the feasibility of applying ptychography to the imaging of biological specimens, in particular collagen rich samples. We report here speckles in diffraction patternsmore » from soft animal tissue, obtained with an optimized small angle X-ray setup that exploits the natural coherence of the beam. By phasing these patterns, dark field images of collagen within tendon, skin, bone, or cornea will eventually be obtained with a resolution of 60-70 nm. We present simulations of the contrast mechanism in collagen based on atomic force microscope images of the samples. Simulations confirmed the 'speckled' nature of the obtained diffraction patterns. Once inverted, the patterns will show the disposition and orientation of the fibers within the tissue, by enhancing the phase contrast between protein and no protein regions of the sample. Our work affords the application of the most innovative coherent X-ray diffraction tools to the study of biological specimens, and this approach will have a significant impact in biology and medicine because it overcomes many of the limits of current microscopy techniques.« less

X-ray diffraction microscopy on frozen hydrated specimens

NASA Astrophysics Data System (ADS)

Nelson, Johanna

X-rays are excellent for imaging thick samples at high resolution because of their large penetration depth compared to electrons and their short wavelength relative to visible light. To image biological material, the absorption contrast of soft X-rays, especially between the carbon and oxygen K-shell absorption edges, can be utilized to give high contrast, high resolution images without the need for stains or labels. Because of radiation damage and the desire for high resolution tomography, live cell imaging is not feasible. However, cells can be frozen in vitrified ice, which reduces the effect of radiation damage while maintaining their natural hydrated state. X-ray diffraction microscopy (XDM) is an imaging technique which eliminates the limitations imposed by current focusing optics simply by removing them entirely. Far-field coherent diffraction intensity patterns are collected on a pixelated detector allowing every scattered photon to be collected within the limits of the detector's efficiency and physical size. An iterative computer algorithm is then used to invert the diffraction intensity into a real space image with both absorption and phase information. This technique transfers the emphasis away from fabrication and alignment of optics, and towards data processing. We have used this method to image a pair of freeze-dried, immuno-labeled yeast cells to the highest resolution (13 nm) yet obtained for a whole eukaryotic cell. We discuss successes and challenges in working with frozen hydrated specimens and efforts aimed at high resolution imaging of vitrified eukaryotic cells in 3D.

A comparison investigation of optical, structural and luminescence properties of CdOxTe1-x and CdTexSe1-x nanoparticles prepared by a simple one pot method

NASA Astrophysics Data System (ADS)

Kiprotich, Sharon; Onani, Martin O.; Dejene, Francis B.

2018-04-01

We present L-cysteine capped CdOXTe1-X and CdTeXSe1-X nanoparticles (NPs) prepared in one pot. The as-prepared CdOXTe1-X NPs were found to have a hexagonal crystal structure of CdTe with a cubic phase of CdO. There was, however, change in phase to cubic type when 2 mM of Se was introduced into the CdTe at 60 min of reaction time. The average crystallite sizes obtained from X-ray diffraction analysis for CdOXTe1-X and CdTeXSe1-X NPs were in the range of 10-36 nm. The diffraction peaks shifted to higher diffraction angle with longer growth time. Scanning electron microscope images display change in shape and size as reaction progress. Photoluminescence (PL) emission was observed to shift from 510-566 nm and 620-653 nm for CdOXTe1-X and CdTeXSe1-X NPs respectively followed by variation in the peak intensities. The emission spectra displayed a good symmetry and a narrow full width at half maximum ranging from 41 to 100 nm in both cases. The absorbance analysis of the as-prepared NPs displayed well-resolved absorption bands. The optical band gaps of the as-prepared NPs were found to decrease with increase in reaction time. Reaction parameters such as pH, reaction time, reaction temperature and the molar concentration could have major effects on the optical properties of the as-prepared nanoparticles hence their need to control them.

Crystallographic Texture and Elemental Composition Mapped in Bovine Root Dentin at the 200 nm Level

PubMed Central

Deymier-Black, A. C.; Veis, A.; Cai, Z.; Stock, S. R.

2015-01-01

Summary The relationship between the mineralization of peritubular dentin (PTD) and intertubular dentin (ITD) is not well understood. Tubules are quite small, diameter ~2 μm, and this makes the near-tubule region of dentin difficult to study. Here, advanced characterization techniques are applied in a novel way to examine what organic or nanostructural signatures may indicate the end of ITD or the beginning of PTD mineralization. X-ray fluorescence intensity (Ca, P, and Zn) and X-ray diffraction patterns from carbonated apatite (cAp) were mapped around dentintubules at resolutions ten times smaller than the feature size (200 nm pixels), representing a 36% increase in resolution over earlier work. In the near tubule volumes of near-pulp, root dentin, Zn intensity was higher than in ITD remote from the tubules. This increase in Zn2+, as determined by X-ray absorption near edge structure analysis, may indicate the presence of metalloenzymes or transcription factors important to ITD or PTD mineralization. The profiles of the cAp 00.2 X-ray diffraction rings were fitted with a pseudo-Voigt function, and the spatial and azimuthal distribution of these rings’ integrated intensities indicated that the cAp platelets were arranged with their c-axes aligned tangential to the edge of the tubule lumen. This texture was continuous throughout the dentin indicating a lack of structural difference between in the Zn rich near-tubular region and the remote ITD. PMID:23630059

Simulations of single-particle imaging of hydrated proteins with x-ray free-electron lasers

NASA Astrophysics Data System (ADS)

Fortmann-Grote, C.; Bielecki, J.; Jurek, Z.; Santra, R.; Ziaja-Motyka, B.; Mancuso, A. P.

2017-08-01

We employ start-to-end simulations to model coherent diffractive imaging of single biomolecules using x-ray free electron lasers. This technique is expected to yield new structural information about biologically relevant macromolecules thanks to the ability to study the isolated sample in its natural environment as opposed to crystallized or cryogenic samples. The effect of the solvent on the diffraction pattern and interpretability of the data is an open question. We present first results of calculations where the solvent is taken into account explicitly. They were performed with a molecular dynamics scheme for a sample consisting of a protein and a hydration layer of varying thickness. Through R-factor analysis of the simulated diffraction patterns from hydrated samples, we show that the scattering background from realistic hydration layers of up to 3 Å thickness presents no obstacle for the resolution of molecular structures at the sub-nm level.

Thickness and annealing effects on thermally evaporated InZnO thin films for gas sensors and blue, green and yellow emissive optical devices

NASA Astrophysics Data System (ADS)

Sugumaran, Sathish; Jamlos, Mohd Faizal; Ahmad, Mohd Noor; Bellan, Chandar Shekar; Sivaraj, Manoj

2016-08-01

Indium zinc oxide (InZnO) thin films with thicknesses of 100 nm and 200 nm were deposited on glass plate by thermal evaporation technique. Fourier transform infrared spectra showed a strong metal-oxide bond. X-ray diffraction patterns revealed amorphous nature for as-deposited film whereas polycrystalline structure for annealed films. Scanning electron microscope images showed a uniform distribution of spherical shape grains. Grain size was found to be higher for 200 nm film than 100 nm film. The presence of elements (In, Zn and O) was confirmed from energy dispersive X-ray analysis. Photoluminescence study of 200 nm film showed a blue, blue-green and blue-yellow emission whereas 100 nm film showed a broad green and green-yellow emissions. Both 100 nm and 200 nm films showed good oxygen sensitivity from room temperature to 400 °C. The observed optical and sensor results indicated that the prepared InZnO films are highly potential for room temperature gas sensor and blue, green and yellow emissive opto-electronic devices.

Coriandrum sativum mediated synthesis of silver nanoparticles and evaluation of their biological characteristics

NASA Astrophysics Data System (ADS)

Senthilkumar, N.; Aravindhan, V.; Ruckmani, K.; Vetha Potheher, I.

2018-05-01

Silver (Ag) nanoparticles (NPs) were prepared by percolated green synthesis method using Coriandrum sativum leaf, root, seed and stem extracts and reported its antibacterial activity. The synthesized Ag NPs were confirmed by UV–visible Spectroscopy, Powder x-ray Diffraction (PXRD), Fourier Transform Infra Red (FT-IR) Spectroscopy analyzes. The Maximum absorbance observed around 400–450 nm reveal the characteristic absorbance of Ag NPs. The Dynamic Light Scattering (DLS) analysis shows the stability of synthesized NPs with average size varying from 35 to 53 nm and also zeta potential stability varying from ‑20 to ‑30 mV. The cubic structure, crystalline nature and purity of the material was confirmed by powder x-ray diffraction studies. FT-IR spectrum shows the presence of various functional groups in the resultant material. The Field Emission Scanning Electron Microscopy (FESEM) image shows the surface morphology of the synthesized NPs and the Energy Dispersive x-ray Analysis (EDAX) confirms the presence of silver metal ions. The Coriandrum sativum aqueous extract exhibited excellent antimicrobial activity against Klebsiella pneumoniae (Gram -ve) bacteria. Numerous studies have been made previously in our field of study but optimization has not been carried out by both extract (different parts like leaf, root, seed and stem) and without addition of any external source such as chemicals, heat etc.

Extended asymmetric-cut multilayer X-ray gratings.

PubMed

Prasciolu, Mauro; Haase, Anton; Scholze, Frank; Chapman, Henry N; Bajt, Saša

2015-06-15

The fabrication and characterization of a large-area high-dispersion blazed grating for soft X-rays based on an asymmetric-cut multilayer structure is reported. An asymmetric-cut multilayer structure acts as a perfect blazed grating of high efficiency that exhibits a single diffracted order, as described by dynamical diffraction throughout the depth of the layered structure. The maximum number of grating periods created by cutting a multilayer deposited on a flat substrate is equal to the number of layers deposited, which limits the size of the grating. The size limitation was overcome by depositing the multilayer onto a substrate which itself is a coarse blazed grating and then polish it flat to reveal the uniformly spaced layers of the multilayer. The number of deposited layers required is such that the multilayer thickness exceeds the step height of the substrate structure. The method is demonstrated by fabricating a 27,060 line pairs per mm blazed grating (36.95 nm period) that is repeated every 3,200 periods by the 120-μm period substrate structure. This preparation technique also relaxes the requirements on stress control and interface roughness of the multilayer film. The dispersion and efficiency of the grating is demonstrated for soft X-rays of 13.2 nm wavelength.

Diamagnetism to ferromagnetism in Sr-substituted epitaxial BaTiO{sub 3} thin films

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

Singamaneni, Srinivasa Rao, E-mail: ssingam@ncsu.edu; Prater, John T.; Department of Materials Science and Engineering, North Carolina State University, Raleigh, North Carolina 27695

2016-04-04

We report on the ferromagnetic-like behavior in otherwise diamagnetic BaTiO{sub 3} (BTO) thin films upon doping with non-magnetic element Sr having the composition Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} (BST). The epitaxial integration of BST (∼800 nm) thick films on Si (100) substrate was achieved using MgO (40 nm) and TiN (20 nm) as buffer layers to prepare BST/MgO/TiN/Si (100) heterostructure by pulsed laser deposition. The c-axis oriented and cube-on-cube epitaxial BST is formed on Si (100) as evidenced by the in-plane and out-of-plane X-ray diffraction. All the deposited films are relaxed through domain matching epitaxy paradigm as observed from X-ray diffraction pattern and A{submore » 1}TO{sub 3} mode (at 521.27 cm{sup −1}) of Raman spectra. As-deposited BST thin films reveal ferromagnetic-like properties, which persist up to 400 K. The magnetization decreases two-fold upon oxygen annealing. In contrast, as-deposited un-doped BTO films show diamagnetism. Electron spin resonance measurements reveal no evidence of external magnetic impurities. XRD and X-ray photoelectron spectroscopy spectra show significant changes influenced by Sr doping in BTO. The ferromagnetic-like behavior in BST could be due to the trapped electron donors from oxygen vacancies resulting from Sr-doping.« less

Growth and luminescent properties of Yb:YAG and Ca co-doped Yb:YAG ultrafast scintillation crystals

NASA Astrophysics Data System (ADS)

Zhu, Maodong; Qi, Hongji; Pan, Mingyan; Hou, Qing; Jiang, Benxue; Jin, Yaxue; Han, Hetong; Song, Zhaohui; Zhang, Hui

2018-05-01

In this work, Yb-doped Y3Al5O12 [yttrium aluminum garnet (YAG)] crystals and Ca co-doped Yb:YAG crystals were grown by the Czochralski (CZ) method. The chemical formulas of the two crystals are (Yb0.1Y0.9)3Al5O12 and (Ca0.001Yb0.1Y0.899)3Al5O12, respectively. The structural, optical and luminescent properties of the Yb:YAG and Ca, Yb:YAG crystals were investigated by X-ray rocking curve, X-ray diffraction, Raman spectra, UV-Visble-NIR absorption spectra and X-ray fluorescence. X-ray fluorescence spectrum with two emission peaks at 330 nm and 490 nm were observed in the two kinds of crystals, which would increase slightly after the annealing. Comparing to the Yb:YAG crystal, Ca co-doped Yb:YAG crystal behaved the better luminescent intensity without changing the crystal structure and vibrational modes. This indicates that by doping Ca2+ in Yb:YAG crystal may be an appropriate way to enhance the luminescent property of the scintillation crystal.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Study of magnetic behavior in hexagonal-YMn1-xFexO3 (x=0 and 0.2) nanoparticles using remanent magnetization curves

NASA Astrophysics Data System (ADS)

Chauhan, Samta; Singh, Amit Kumar; Srivastava, Saurabh Kumar; Chandra, Ramesh

2016-09-01

We have studied the magnetic behavior of YMn1-xFexO3 (x=0 and 0.2) nanoparticles synthesized by conventional solid state reaction method. The as-synthesized nanoparticles were found to have hexagonal phase with P63cm space group confirmed by X-Ray diffraction. The particle size was found to be ~70 nm as confirmed by both X-Ray diffraction and Transmission Electron Microscopy. DC magnetization and memory effect measurements imply that the h-YMnO3 nanoparticles bear a resemblance to super spin-glass state following de Almeida-Thouless like behavior which is being suppressed by Fe-doping. The Fe-doping in YMnO3 enhances the antiferromagnetic (AFM) transition temperature TN to ~79 K and induces a new magnetic state due to the surface spins which is realized as diluted antiferromagnet in a field (DAFF) as explored by the thermoremanent and isothermoremanent magnetization measured with different applied magnetic field.

Dynamic X-ray diffraction imaging of the ferroelectric response in bismuth ferrite

DOE PAGES

Laanait, Nouamane; Saenrang, Wittawat; Zhou, Hua; ...

2017-03-21

In this study, X-ray diffraction imaging is rapidly emerging as a powerful technique by which one can capture the local structure of crystalline materials at the nano- and meso-scale. Here, we present investigations of the dynamic structure of epitaxial monodomain BiFeO 3 thin-films using a novel full-field Bragg diffraction imaging modality. By taking advantage of the depth penetration of hard X-rays and their exquisite sensitivity to the atomic structure, we imaged in situ and in operando, the electric field-driven structural responses of buried BiFeO 3 epitaxial thin-films in micro-capacitor devices, with sub-100 nm lateral resolution. These imaging investigations were carriedmore » out at acquisition frame rates that reached up to 20 Hz and data transfer rates of 40 MB/s, while accessing diffraction contrast that is sensitive to the entire three-dimensional unit cell configuration. We mined these large datasets for material responses by employing matrix decomposition techniques, such as independent component analysis. We found that this statistical approach allows the extraction of the salient physical properties of the ferroelectric response of the material, such as coercive fields and transient spatiotemporal modulations in their piezoelectric response, and also facilitates their decoupling from extrinsic sources that are instrument specific.« less

Micro X-ray diffraction analysis of thin films using grazing-exit conditions.

PubMed

Noma, T; Iida, A

1998-05-01

An X-ray diffraction technique using a hard X-ray microbeam for thin-film analysis has been developed. To optimize the spatial resolution and the surface sensitivity, the X-ray microbeam strikes the sample surface at a large glancing angle while the diffracted X-ray signal is detected with a small (grazing) exit angle. Kirkpatrick-Baez optics developed at the Photon Factory were used, in combination with a multilayer monochromator, for focusing X-rays. The focused beam size was about 10 x 10 micro m. X-ray diffraction patterns of Pd, Pt and their layered structure were measured. Using a small exit angle, the signal-to-background ratio was improved due to a shallow escape depth. Under the grazing-exit condition, the refraction effect of diffracted X-rays was observed, indicating the possibility of surface sensitivity.

Stereospecific growth of densely populated rutile mesoporous TiO2 nanoplate films: a facile low temperature chemical synthesis approach

NASA Astrophysics Data System (ADS)

Lee, Go-Woon; Ambade, Swapnil B.; Cho, Young-Jin; Mane, Rajaram S.; Shashikala, V.; Yadav, Jyotiprakash; Gaikwad, Rajendra S.; Lee, Soo-Hyoung; Jung, Kwang-Deog; Han, Sung-Hwan; Joo, Oh-Shim

2010-03-01

We report for the first time, using a simple and environmentally benign chemical method, the low temperature synthesis of densely populated upright-standing rutile TiO2 nanoplate films onto a glass substrate from a mixture of titanium trichloride, hydrogen peroxide and thiourea in triply distilled water. The rutile TiO2 nanoplate films (the phase is confirmed from x-ray diffraction analysis, selected area electron diffraction, energy-dispersive x-ray analysis, and Raman shift) are 20-35 nm wide and 100-120 nm long. The chemical reaction kinetics for the growth of these upright-standing TiO2 nanoplate films is also interpreted. Films of TiO2 nanoplates are optically transparent in the visible region with a sharp absorption edge close to 350 nm, confirming an indirect band gap energy of 3.12 eV. The Brunauer-Emmet-Teller surface area, Barret-Joyner-Halenda pore volume and pore diameter, obtained from N2 physisorption studies, are 82 m2 g - 1, 0.0964 cm3 g - 1 and 3.5 nm, respectively, confirming the mesoporosity of scratched rutile TiO2 nanoplate powder that would be ideal for the direct fabrication of nanoscaled devices including upcoming dye-sensitized solar cells and gas sensors.

Effect of Annealing Temperature on Structural and Optical Properties of Sol-Gel-Derived ZnO Thin Films

NASA Astrophysics Data System (ADS)

Arif, Mohd.; Sanger, Amit; Vilarinho, Paula M.; Singh, Arun

2018-04-01

Nanocrystalline ZnO thin films were deposited on glass substrate via sol-gel dip-coating technique then annealed at 300°C, 400°C, and 500°C for 1 h. Their optical, structural, and morphological properties were studied using ultraviolet-visible (UV-Vis) spectrophotometry, x-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM). XRD diffraction revealed that the crystalline nature of the thin films increased with increasing annealing temperature. The c-axis orientation improved, and the grain size increased, as indicated by increased intensity of the (002) plane peak at 2θ = 34.42° corresponding to hexagonal ZnO crystal. The average crystallite size of the thin films ranged from 13 nm to 23 nm. Increasing the annealing temperature resulted in larger crystallite size and higher crystallinity with increased surface roughness. The grain size according to SEM analysis was in good agreement with the x-ray diffraction data. The optical bandgap of the thin films narrowed with increasing annealing temperature, lying in the range of 3.14 eV to 3.02 eV. The transmission of the thin films was as high as 94% within the visible region. The thickness of the thin films was 400 nm, as measured by ellipsometry, after annealing at the different temperatures of 300°C, 400°C, and 500°C.

Interlaced zone plate optics for hard X-ray imaging in the 10 nm range

DOE PAGES

Mohacsi, Istvan; Vartiainen, Ismo; Rosner, Benedikt; ...

2017-03-08

Multi-keV X-ray microscopy has been particularly successful in bridging the resolution gap between optical and electron microscopy. However, resolutions below 20 nm are still considered challenging, as high throughput direct imaging methods are limited by the availability of suitable optical elements. In order to bridge this gap, we present a new type of Fresnel zone plate lenses aimed at the sub-20 and the sub-10 nm resolution range. By extending the concept of double-sided zone plate stacking, we demonstrate the doubling of the effective line density and thus the resolution and provide large aperture, single- chip optical devices with 15 andmore » 7 nm smallest zone widths. The detailed characterization of these lenses shows excellent optical properties with focal spots down to 7.8 nm. Furthermore, beyond wave front characterization, the zone plates also excel in typical imaging scenarios, verifying their resolution close to their diffraction limited optical performance.« less

Interlaced zone plate optics for hard X-ray imaging in the 10 nm range

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

Mohacsi, Istvan; Vartiainen, Ismo; Rosner, Benedikt

Multi-keV X-ray microscopy has been particularly successful in bridging the resolution gap between optical and electron microscopy. However, resolutions below 20 nm are still considered challenging, as high throughput direct imaging methods are limited by the availability of suitable optical elements. In order to bridge this gap, we present a new type of Fresnel zone plate lenses aimed at the sub-20 and the sub-10 nm resolution range. By extending the concept of double-sided zone plate stacking, we demonstrate the doubling of the effective line density and thus the resolution and provide large aperture, single- chip optical devices with 15 andmore » 7 nm smallest zone widths. The detailed characterization of these lenses shows excellent optical properties with focal spots down to 7.8 nm. Furthermore, beyond wave front characterization, the zone plates also excel in typical imaging scenarios, verifying their resolution close to their diffraction limited optical performance.« less

Interlaced zone plate optics for hard X-ray imaging in the 10 nm range

PubMed Central

Mohacsi, Istvan; Vartiainen, Ismo; Rösner, Benedikt; Guizar-Sicairos, Manuel; Guzenko, Vitaliy A.; McNulty, Ian; Winarski, Robert; Holt, Martin V.; David, Christian

2017-01-01

Multi-keV X-ray microscopy has been particularly successful in bridging the resolution gap between optical and electron microscopy. However, resolutions below 20 nm are still considered challenging, as high throughput direct imaging methods are limited by the availability of suitable optical elements. In order to bridge this gap, we present a new type of Fresnel zone plate lenses aimed at the sub-20 and the sub-10 nm resolution range. By extending the concept of double-sided zone plate stacking, we demonstrate the doubling of the effective line density and thus the resolution and provide large aperture, singlechip optical devices with 15 and 7 nm smallest zone widths. The detailed characterization of these lenses shows excellent optical properties with focal spots down to 7.8 nm. Beyond wave front characterization, the zone plates also excel in typical imaging scenarios, verifying their resolution close to their diffraction limited optical performance.

Interlaced zone plate optics for hard X-ray imaging in the 10 nm range

NASA Astrophysics Data System (ADS)

Mohacsi, Istvan; Vartiainen, Ismo; Rösner, Benedikt; Guizar-Sicairos, Manuel; Guzenko, Vitaliy A.; McNulty, Ian; Winarski, Robert; Holt, Martin V.; David, Christian

2017-03-01

Multi-keV X-ray microscopy has been particularly successful in bridging the resolution gap between optical and electron microscopy. However, resolutions below 20 nm are still considered challenging, as high throughput direct imaging methods are limited by the availability of suitable optical elements. In order to bridge this gap, we present a new type of Fresnel zone plate lenses aimed at the sub-20 and the sub-10 nm resolution range. By extending the concept of double-sided zone plate stacking, we demonstrate the doubling of the effective line density and thus the resolution and provide large aperture, singlechip optical devices with 15 and 7 nm smallest zone widths. The detailed characterization of these lenses shows excellent optical properties with focal spots down to 7.8 nm. Beyond wave front characterization, the zone plates also excel in typical imaging scenarios, verifying their resolution close to their diffraction limited optical performance.

Structural and magnetic properties of ultra-thin Fe films on metal-organic chemical vapour deposited GaN(0001)

NASA Astrophysics Data System (ADS)

Kim, Jun-Young; Ionescu, Adrian; Mansell, Rhodri; Farrer, Ian; Oehler, Fabrice; Kinane, Christy J.; Cooper, Joshaniel F. K.; Steinke, Nina-Juliane; Langridge, Sean; Stankiewicz, Romuald; Humphreys, Colin J.; Cowburn, Russell P.; Holmes, Stuart N.; Barnes, Crispin H. W.

2017-01-01

Structural and magnetic properties of 1-10 nm thick Fe films deposited on GaN(0001) were investigated. In-situ reflecting high energy electron diffraction images indicated a α-Fe(110)/GaN(0001) growth of the 3D Volmer-Weber type. The α-Fe(110) X-ray diffraction peak showed a 1° full-width at half-maximum, indicating ≈20 nm grain sizes. A significant reduction in Fe atomic moment from its bulk value was observed for films thinner than 4 nm. Both GaN/Fe interface roughness and Fe film coercivity increased with Fe thickness, indicating a possible deterioration of Fe crystalline quality. Magnetic anisotropy was mainly uniaxial for all films while hexagonal anisotropies appeared for thicknesses higher than 3.7 nm.

Spectral properties of Dy3+ doped ZnAl2O4 phosphor

NASA Astrophysics Data System (ADS)

Prakash, Ram; Kumar, Sandeep; Mahajan, Rubby; Khajuria, Pooja; Kumar, Vinay; Choudhary, R. J.; Phase, D. M.

2018-05-01

Herein, Dy3+ doped ZnAl2O4 phosphor was synthesized by the solution combustion method. The synthesized phosphor was characterized by X-ray diffraction (XRD), photoluminescence (PL) spectroscopy, UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS). The phase purity of the phosphor was confirmed by the XRD studies that showed cubic symmetry of the synthesized phosphor. Under UV excitation (388 nm) the PL emission spectrum of the phosphor shows characteristic transition from the Dy3+ ion. A band gap of 5.2 eV was estimated from the diffused reflectance spectroscopy. The surface properties of the phosphor were studied using the X-ray photoelectron spectroscopy.

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.

Synthesis and characterization of nanocrystalline LaMnO3 modified BaTiO3 ferroelectric ceramics prepared by chemical route

NASA Astrophysics Data System (ADS)

Dhak, Prasanta; Adak, Mrinal Kanti; Dhak, Debasis

2016-02-01

Nanocrystalline Ba1-3xTi1-3xLa2xMn4xO3, [x = 0.006, 0.008, 0.01 and 0.05] (abbreviated hereafter as BTLM) by chemical route. The phase formation and purity were checked by X-ray diffraction (XRD) study and transmission electron microscopy (TEM). The grain morphology after sintering was studied by scanning electron microscopy (SEM). The crystallite sizes range from 21 nm to 30 nm, while the particle size ranges between 27 nm and 38 nm. The grain size 212 nm and grain density 96.8% were found to be maximum for BTLM x = 0.05 and x = 0.01, respectively. The temperature dependence of dielectric constants was found to be more diffused and the peak value of the dielectric constant was decreased and more flat with the increase of the substituent concentration. The tangent loss was found to be decreased and reached to the minimum value of 0.032 for BTLM x = 0.05. The remnant polarization Pr, was 10 μC/cm2 for BTLM x = 0.01.

ZnS nanostructured thin-films deposited by successive ionic layer adsorption and reaction

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

Deshmukh, S. G., E-mail: deshmukhpradyumn@gmail.com; Jariwala, Akshay; Agarwal, Anubha

ZnS thin films were grown on glass substrate using successive ionic layer adsorption and reaction (SILAR) technique at room temperature. Aqueous solutions of ZnCl{sub 2} and Na{sub 2}S were used as precursors. The X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), Raman spectroscopy and optical absorption measurements were applied to study the structural, surface morphology and optical properties of as-deposited ZnS thin films. The X-ray diffraction profiles revealed that ZnS thin films consist of crystalline grains with cubic phase. Spherical nano grains of random size and well covered on the glass substrate were observed from FESEM. The average grainmore » size were found to be 77 nm, 100 nm and 124 nm for 20 cycles, 40 cycles and 60 cycles samples respectively. For 60 cycle sample, Raman spectra show two prominent peaks at 554 cm{sup −1} and 1094 cm{sup −1}. The optical band gap values were found to be 3.76 eV, 3.72 eV and 3.67 eV for 20 cycle, 40 cycle and 60 cycle samples respectively.« less

As-synthesis of nanostructure AgCl/Ag/MCM-41 composite

NASA Astrophysics Data System (ADS)

Sohrabnezhad, Sh.; Pourahmad, A.

2012-02-01

In this work, we present the simple synthetic route for silver chloride/silver nanoparticles (AgCl/Ag-NPs) using as-synthesis method. The structure, composition and optical properties of such material were investigated by transmission electron microscopy (TEM), UV-visible diffuse reflectance spectroscopy (UV-vis DRS), X-ray diffraction (XRD) and FTIR. Powder X-ray diffraction showed that when AgNO 3 content is below 0.1 wt.% in synthetic gel, the guest AgCl/Ag-NPs is formed on the silica channel wall, and lower exists in the crystalline state. When AgNO 3 content exceeds this value, AgCl/Ag nanoparticles can be observed in high crystalline state. The absorption at 327 nm ascribed to the characteristic absorption of the AgCl semiconductor. Ag nanoparticles have been shown to exist in the nanocomposite at 375 nm. When AgNO 3 content is above 0.1 wt.% in synthetic gel, spectra exhibited stronger absorption at 450-700 nm that was attributed to the surface plasmonic resonance of silver nanoparticles. The obtained AgCl/Ag/MCM-41 sample exhibit enhanced photocatalytic activity for the degradation of methylene blue under visible-light irradiation.

Single-crystal films of a combination of materials (co-crystal) involving DAST and IR-125 for electro-optic applications

NASA Astrophysics Data System (ADS)

Narayanan, A.; Titus, J.; Rajagopalan, H.; Vippa, P.; Thakur, M.

2006-03-01

Single-crystal film of DAST (4'-dimethylamino-N-methyl-4-stilbazolium tosylate) has been shown [1] to have exceptionally large electro-optic coefficients (r11 ˜ 770 pm/V at 633 nm). In this report, single crystal film of a combination of materials (co-crystal) involving DAST and a dye molecule IR-125 will be discussed. Modified shear method was used to prepare the co-crystal films. The film has been characterized using polarized optical microscopy, optical absorption spectroscopy and x-ray diffraction. The optical absorption spectrum has two major bands: one at about 350--600 nm corresponding to DAST and the other at about 600-900 nm corresponding to IR-125. The x-ray diffraction results show peaks involving the presence of DAST and IR-125 within the co-crystal film. Since the co-crystal has strong absorption at longer wavelengths it is expected to show higher electro-optic coefficients at longer wavelengths. Preliminary measurements at 1.55 μm indicate a high electro-optic coefficient of the co-crystal film. [1] Swamy, Kutty, Titus, Khatavkar, Thakur, Appl. Phys. Lett. 2004, 85, 4025; Kutty, Thakur, Appl. Phys. Lett. 2005, 87, 191111.

Synthesis of silver nanoparticles using leaves of Catharanthus roseus Linn. G. Don and their antiplasmodial activities

PubMed Central

Ponarulselvam, S; Panneerselvam, C; Murugan, K; Aarthi, N; Kalimuthu, K; Thangamani, S

2012-01-01

Objective To develop a novel approach for the green synthesis of silver nanoparticles using aqueous leaves extracts of Catharanthus roseus (C. roseus) Linn. G. Don which has been proven active against malaria parasite Plasmodium falciparum (P. falciparum). Methods Characterizations were determined by using ultraviolet-visible (UV-Vis) spectrophotometry, scanning electron microscopy (SEM), energy dispersive X-ray and X-ray diffraction. Results SEM showed the formation of silver nanoparticles with an average size of 35–55 nm. X-ray diffraction analysis showed that the particles were crystalline in nature with face centred cubic structure of the bulk silver with the broad peaks at 32.4, 46.4 and 28.0. Conclusions It can be concluded that the leaves of C. roseus can be good source for synthesis of silver nanoparticle which shows antiplasmodial activity against P. falciparum. The important outcome of the study will be the development of value added products from medicinal plants C. roseus for biomedical and nanotechnology based industries. PMID:23569974

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

Zheng, Pengyuan; Ozsdolay, Brian D.; Gall, Daniel, E-mail: galld@rpi.edu

Smooth single crystal W(001) layers were grown on MgO(001) substrates by magnetron sputtering at 900 °C. X-ray diffraction ω–2θ scans, ω-rocking curves, pole figures, and reciprocal space maps indicate a 45°-rotated epitaxial relationship: (001){sub W}‖(001){sub MgO} and [010]{sub W}‖[110]{sub MgO}, and a relaxed lattice constant of 3.167 ± 0.001 nm. A residual in-plane biaxial compressive strain is primarily attributed to differential thermal contraction after growth and decreases from −0.012 ± 0.001 to −0.001 ± 0.001 with increasing layer thickness d = 4.8–390 nm, suggesting relaxation during cooling by misfit dislocation growth through threading dislocation glide. The in-plane x-ray coherence length increases from 3.4 to 33.6 nm for d = 4.8–390 nm, while the out-of-plane x-raymore » coherence length is identical to the layer thickness for d ≤ 20 nm, but is smaller than d for d ≥ 49.7 nm, indicating local strain variations along the film growth direction. X-ray reflectivity analyses indicate that the root-mean-square surface roughness increases from 0.50 ± 0.05 to 0.95 ± 0.05 nm for d = 4.8–19.9 nm, suggesting a roughness exponent of 0.38, but remains relatively constant for d > 20 nm with a roughness of 1.00 ± 0.05 nm at d = 47.9 nm.« less

Synthesis of Mn doped ZnS nanocrystals: Crystallographic and morphological study

NASA Astrophysics Data System (ADS)

Shaikh, Azharuddin Z.; Shirsath, Narendra B.; Sonawane, Prabhakar S.

2018-05-01

The influence of doping concentration on the physical properties of ZnS nanocrystals synthesized using coprecipitation method at room temperature is reported in this paper. In particular, we have studied the structural properties of Zn1-xMnxS where (x=0.01, 0.03, 0.05) by X-ray diffraction. X-ray peak broadening analysis used to calculate the crystalline sizes, lattice parameters, number of unit cell per particle and volume of unit cell. Crystalline ZnS with a cubic structure is confirmed by XRD results. The grain size of pure and Mn doped samples were found in the range of 7nm to 9nm. All the physical parameters of cubic ZnS nanocrystals were calculated are similar with standard values. The scanning electron microscope (SEM) which revealed that the synthesized nanocrystals are well-crystalline and possessing cubic phase.

Electron Diffraction Using Transmission Electron Microscopy

PubMed Central

Bendersky, Leonid A.; Gayle, Frank W.

2001-01-01

Electron diffraction via the transmission electron microscope is a powerful method for characterizing the structure of materials, including perfect crystals and defect structures. The advantages of electron diffraction over other methods, e.g., x-ray or neutron, arise from the extremely short wavelength (≈2 pm), the strong atomic scattering, and the ability to examine tiny volumes of matter (≈10 nm3). The NIST Materials Science and Engineering Laboratory has a history of discovery and characterization of new structures through electron diffraction, alone or in combination with other diffraction methods. This paper provides a survey of some of this work enabled through electron microscopy. PMID:27500060

Amorphous iron–chromium oxide nanoparticles with long-term stability

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

Iacob, Mihail; Institute of Chemistry of ASM, Academiei str. 3, Chisinau 2028, Republic of Moldova; Cazacu, Maria, E-mail: mcazacu@icmpp.ro

2015-05-15

Highlights: • Fe–Cr oxide nanoparticles with pre-established metals ratio were obtained. • The amorphous state and its long-term stability were highlighted by X-ray diffraction. • The average diameter of dried nanoparticles was 3.5 nm, as was estimated by TEM, AFM. • In hexane dispersion, nanoparticles with diameter in the range 2.33–4.85 nm were found. • Superparamagnetic state of NPs co-exists with diamagnetism of the organic layer. - Abstract: Iron–chromium nanoparticles (NPs) were obtained through the thermal decomposition of μ{sub 3}-oxo heterotrinuclear (FeCr{sub 2}O) acetate in the presence of sunflower oil and dodecylamine (DA) as surfactants. The average diameter of themore » NPs was 3.5 nm, as estimated on the basis of transmission electron microscopy and atomic force microscopy images. Both techniques revealed the formation of roughly approximated spheres with some irregularities and agglomerations in larger spherical assemblies of 50–100 nm. In hexane, NPs with diameters in the 2.33–4.85 nm range are individually dispersed, as emphasized by dynamic light scattering measurements. The amorphous nature of the product was emphasized by X-ray powder diffraction. The study of the magnetic properties shows the presence of superparamagnetic state of iron–chromium oxide NPs and the diamagnetic contribution from DA layer forming a shell of NPs.« less

MOVPE growth of (GaIn)As/Ga(AsSb)/(GaIn)As type-II heterostructures on GaAs substrate for near infrared laser applications

NASA Astrophysics Data System (ADS)

Fuchs, C.; Beyer, A.; Volz, K.; Stolz, W.

2017-04-01

The growth of high quality (GaIn)As/Ga(AsSb)/(GaIn)As "W"-quantum well heterostructures is discussed with respect to their application in 1300 nm laser devices. The structures are grown using metal organic vapor phase epitaxy and characterized using high-resolution X-ray diffraction, scanning transmission electron microscopy and photoluminescence measurements. The agreement between experimental high-resolution X-ray diffraction patterns and full dynamical simulations is verified for these structurally challenging heterostructures. Scanning transmission electron microscopy is used to demonstrate that the structure consists of well-defined quantum wells and forms the basis for future improvements of the optoelectronic quality of this materials system. By altering the group-V gas phase ratio, it is possible to cover a large spectral range between 1200 nm and 1470 nm using a growth temperature of 550 °C and a V/III ratio of 7.5. A comparison of a sample with a photoluminescence emission wavelength at 1360 nm with single quantum well material reference samples proves the type-II character of the emission. A further optimization of these structures for application in 1300 nm lasers by applying different V/III ratios yields a stable behavior of the photoluminescence intensity using a growth temperature of 550 °C.

Synthesis, crystal structure and characterization of a new organic-inorganic hybrid material 4-(ammonium methyl) pipyridinium hexachloro stanate (II) trihydrate

NASA Astrophysics Data System (ADS)

Lassoued, Mohamed Saber; Abdelbaky, Mohammed S. M.; Lassoued, Abdelmajid; Ammar, Salah; Gadri, Abdellatif; Ben Salah, Abdelhamid; García-Granda, Santiago

2018-03-01

The present paper undertakes the study of (C6H16N2) SnCl6·3H2O which is a new hybrid compound. It was prepared and characterized by single crystal X-ray diffraction, X-ray powder, Hirshfeld surface, Spectroscopy measurement, thermal study and photoluminescence properties. The single crystal X-ray diffraction studies revealed that the compound crystallizes in monoclinic Cc space group with cell parameters a = 8.3309(9) Å, b = 22.956(2) Å, c = 9.8381(9) Å, β = 101.334(9) ° and Z = 4. The atomic arrangement shows an alternation of organic and inorganic entities. The cohesion between these entities is performed via Nsbnd H⋯Cl, Nsbnd H⋯O, Osbnd H⋯Cl and Osbnd H⋯O hydrogen bonding to form a three-dimensional network. Hirshfeld surface analysis was used to investigate intermolecular interactions, as well 2D finger plots were conducted to reveal the contribution of these interactions in the crystal structure quantitatively. The X-ray powder is in agreement with the X-ray structure. Scanning electron microscope (SEM) was carried out. Furthermore, the room temperature infrared (IR) spectrum of the title compound was recorded and analyzed on the basis of data found in the literature. Solid state 13C NMR spectrum shows four signals, confirming the solid state structure determined by X-ray diffraction. Besides, the thermal analysis studies were performed, but no phase transition was found in the temperature range between 30 and 450 °C. The optical and PL properties of the compound were investigated in the solid state at room temperature and exhibited three bands at 348 and 401 cm-1 and a strong fluorescence at 480 nm.

A simple method to synthesize polyhedral hexagonal boron nitride nanofibers

NASA Astrophysics Data System (ADS)

Lin, Liang-xu; Zheng, Ying; Li, Zhao-hui; shen, Xiao-nv; Wei, Ke-mei

2007-12-01

Hexagonal boron nitride (h-BN) fibers with polyhedral morphology were synthesized with a simple-operational, large-scale and low-cost method. The sample obtained was studied by X-ray photoelectron spectrometer (XPS), electron energy lose spectroscopy (EELS), X-ray powder diffraction (XRD), Fourier transformation infrared spectroscopy (FT-IR), etc., which matched with h-BN. Environment scanning electron microscopy (ESEM) and transmission electron microscope (TEM) indicated that the BN fibers possess polyhedral morphology. The diameter of the BN fibers is mainly in the range of 100-500 nm.

A Highly Efficient and Facile Approach for Fabricating Graphite Nanoplatelets

NASA Astrophysics Data System (ADS)

Van Thanh, Dang; Van Thien, Nguyen; Thang, Bui Hung; Van Chuc, Nguyen; Hong, Nguyen Manh; Trang, Bui Thi; Lam, Tran Dai; Huyen, Dang Thi Thu; Hong, Phan Ngoc; Minh, Phan Ngoc

2016-05-01

In this study, we report a highly efficient, convenient, and cost-effective technique for producing graphite nanoplatelets (GNPs) from plasma-expanded graphite oxides (PEGOs) obtained directly from low-cost, recycled graphite electrodes of used batteries, x-ray diffraction, Raman spectroscopy, and x-ray photoelectron spectroscopy confirmed the successful preparation of GNPs. Scanning electron microscopy revealed that the GNPs have lateral width from several hundreds of nanometers to 1.5 μm with an approximate thickness of 20-50 nm. These GNPs can serve as a precursor for the preparation of GNPs-based nanocomposite.

Ultrafast nanoscale imaging using high order harmonic generation (Conference Presentation)

NASA Astrophysics Data System (ADS)

Merdji, Hamed

2017-05-01

Ultrafast coherent diffraction using soft and hard X-rays is actually revolutionizing imaging science thanks to new sources recently available. This powerful technique extends standard X-ray diffraction towards imaging of non-crystalline objects and leads actually to a strong impact in physics, chemistry and biology. New ultrashort pulses recently available hold the promise of watching matter evolving with unprecedented space and time resolution. Femtosecond coherent and intense radiation in the soft X-ray (λ = 10-40 nm) is currently produced in our laboratory, from highly non linear frequency conversion (high harmonic generation). A high intensity UV-X coherent beam is obtained using a loose focusing geometry, which allows coupling a very high amount of Ti:Sapphire laser system energy in the HHG process. Using a long gas cell and a long focal length lens, the emitting volume can be increased by orders of magnitude compared to standard HHG set-ups. This approach, allows reaching up to 1x1011 photons per shot for the 25th harmonic (λ=32nm). We have already demonstrated nanoscale imaging in a single shot mode reaching 70 nm spatial resolution and 20 femtoseconds snapshot [1]. We then implemented a recently proposed holographic technique using extended references. This technique, easy to implement, allows a direct non iterative image reconstruction. In the single shot regime, we demonstrated a spatial resolution of 110nm [2].This opens fascinating perspectives in imaging dynamical phenomena to be spread over a large scientific community. I will present recent results in the investigation of femtosecond phase spin-reversals of magnetic nano-domains [3]. Finally, I will report on recent development on noise sensitivity of the technique and perspectives in attosecond coherent imaging [4]. [1] A. Ravasio et al., Physical Review Letters 103, 028104 (2009). [2] D. Gauthier et al., Physical Review Letters 105, 093901 (2010). [3] Vodungbo et al., Nature Communications 3, 999 (2012) [4] Williams et al., Optics Letters 40 (13), 3205 (2015)

Effect of different conventional melt quenching technique on purity of lithium niobate (LiNbO3) nano crystal phase formed in lithium borate glass

NASA Astrophysics Data System (ADS)

Kashif, Ismail; Soliman, Ashia A.; Sakr, Elham M.; Ratep, Asmaa

2012-01-01

The glass system (45Li2O + 45B2O3 + 10Nb2O5) was fabricated by the conventional melt quenching technique poured in water, at air, between two hot plates and droplets at the cooled surface. The glass and glass ceramics were studied by differential thermal analysis (DTA) and X-ray diffraction (XRD). The as quenched samples poured in water and between two hot plates were amorphous. The samples poured at air and on cooled surface were crystalline as established via X-ray powder diffraction (XRD) studies. Differential thermal analysis was measured. The glass transition temperature (Tg) and the crystallization temperatures were calculated. Lithium niobate (LiNbO3) was the main phase in glass ceramic poured at air, droplets at the cooled surface and the heat treated glass sample at 500, 540 and 580 °C in addition to traces from LiNb3O8. Crystallite size of the main phases determined from the X-ray diffraction peaks is in the range of <100 nm. The fraction of crystalline (LiNbO3) phase decreases with increase in the heat treatment temperature.

Radiation-induced melting in coherent X-ray diffractive imaging at the nanoscale

PubMed Central

Ponomarenko, O.; Nikulin, A. Y.; Moser, H. O.; Yang, P.; Sakata, O.

2011-01-01

Coherent X-ray diffraction techniques play an increasingly significant role in the imaging of nanoscale structures, ranging from metallic and semiconductor to biological objects. In material science, X-rays are usually considered to be of a low-destructive nature, but under certain conditions they can cause significant radiation damage and heat loading on the samples. The qualitative literature data concerning the tolerance of nanostructured samples to synchrotron radiation in coherent diffraction imaging experiments are scarce. In this work the experimental evidence of a complete destruction of polymer and gold nanosamples by the synchrotron beam is reported in the case of imaging at 1–10 nm spatial resolution. Numerical simulations based on a heat-transfer model demonstrate the high sensitivity of temperature distribution in samples to macroscopic experimental parameters such as the conduction properties of materials, radiation heat transfer and convection. However, for realistic experimental conditions the calculated rates of temperature rise alone cannot explain the melting transitions observed in the nanosamples. Comparison of these results with the literature data allows a specific scenario of the sample destruction in each particular case to be presented, and a strategy for damage reduction to be proposed. PMID:21685675

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

NASA Astrophysics Data System (ADS)

Murphy, Michael Wayne

2010-06-01

Various II-VI semiconducting nanomaterials such as ZnO-ZnS nanoribbons (NRs), CdSxSe1-x nanostructures, ZnS:Mn NRs, ZnS:Mn,Eu nanoprsims (NPs), ZnO:Mn nanopowders, and ZnO:Co nanopowders were synthesized for study. These materials were characterized by techniques such as scanning electron microscopy, transmission electron microscopy, element dispersive X-ray spectroscopy, selected area electron diffraction, and X-ray diffraction. The electronic and optical properties of these nanomaterials were studied by X-ray absorption fine structure (XAFS) spectroscopy and X-ray excited optical luminescence (XEOL) techniques, using tuneable soft X-rays from a synchrotron light source. The complementary nature ofthe XAFS and XEOL techniques give site, element and chemical specific measurements which allow a better understanding of the interplay and role of each element in the system. Chemical vapour deposition (CVD) of ZnS powder in a limited oxygen environment resulted in side-by-side biaxial ZnO-ZnS NR heterostructures. The resulting NRs contained distinct wurtzite ZnS and wurtzite ZnO components with widths of 10--100 nm and 20 --500 nm, respectively and a uniform interface region of 5-15 nm. XAFS and XEOL measurements revealed the luminescence of ZnO-ZnS NRs is from the ZnO component. The luminescence of CdSxSe1-x nanostructures is shown to be dependent on the S to Se ratio, with the band-gap emission being tunable between that of pure CdS and CdSe. Excitation of the CdSxSe 1-x nanostructures by X-ray in XEOL has revealed new de-excitation channels which show a defect emission band not seen by laser excitation. CVD of Mn2+ doped ZnS results in nanostructures with luminescence dominated by the yellow Mn2+ emission due to energy transfer from the ZnS host to the Mn dopant sites. The addition of EuCl3 to the reactants in the CVD process results in a change in morphology from NR to NP. Zn1-xMnxO and Zn1-xCOxO nanopowders were prepared by sol-gel methods at dopant concentrations of 0, 1,3, and 10% and annealed at 400, 600 and 800°C in air. XAFS spectra show that low dopant concentrations and low processing temperatures limit the amount of secondary phase formation. The nanopowders did not show roomtemperature ferromagnetism and increased secondary phase formation increases the paramagnetic character of the hysteresis curves at 5°K. Keywords: X-ray absorption fine structures (XAFS), X-ray absorption near-edge structures (XANES), extended X-ray absorption fine structure (EXAFS), X-ray absorption spectroscopy(XAS), X-ray excited optical luminescence (XEOL), time-resolved, II-VI semiconductors, nanostructure, nanomaterial, nanoribbon, nanowire, nanopartic1e, heterostructure, ZnO, ZnS, ZnO-ZnS, CdS, CdSe, CdSSe, ZnO:Mn, ZnO:Co, ZnS:Mn, dilute magnetic semiconductor (DMS), dilute magnetic oxide (DMO), spintronics, magnetism, paramagnetism, ferromagnetism.

Low-temperature growth and photoluminescence property of ZnS nanoribbons.

PubMed

Zhang, Zengxing; Wang, Jianxiong; Yuan, Huajun; Gao, Yan; Liu, Dongfang; Song, Li; Xiang, Yanjuan; Zhao, Xiaowei; Liu, Lifeng; Luo, Shudong; Dou, Xinyuan; Mou, Shicheng; Zhou, Weiya; Xie, Sishen

2005-10-06

At a low temperature of 450 degrees C, ZnS nanoribbons have been synthesized on Si and KCl substrates by a simple chemical vapor deposition (CVD) method with a two-temperature-zone furnace. Zinc and sulfur powders are used as sources in the different temperature zones. X-ray diffraction (XRD), selected area electron diffraction (SEAD), and transmission electron microscopy (TEM) analysis show that the ZnS nanoribbons are the wurtzite structure, and there are two types-single-crystal and bicrystal nanoribbons. Photoluminescence (PL) spectrum shows that the spectrum mainly includes two parts: a purple emission band centering at about 390 nm and a blue emission band centering at about 445 nm with a weak green shoulder around 510 nm.

X-ray diffraction from shock-loaded polycrystals.

PubMed

Swift, Damian C

2008-01-01

X-ray diffraction was demonstrated from shock-compressed polycrystalline metals on nanosecond time scales. Laser ablation was used to induce shock waves in polycrystalline foils of Be, 25-125 microm thick. A second laser pulse was used to generate a plasma x-ray source by irradiation of a Ti foil. The x-ray source was collimated to produce a beam of controllable diameter, which was directed at the Be sample. X-rays were diffracted from the sample, and detected using films and x-ray streak cameras. The diffraction angle was observed to change with shock pressure. The diffraction angles were consistent with the uniaxial (elastic) and isotropic (plastic) compressions expected for the loading conditions used. Polycrystalline diffraction will be used to measure the response of the crystal lattice to high shock pressures and through phase changes.

Perylene and Perylene-Derivative Nano-Cocrystals: Preparation and Physicochemical Property

NASA Astrophysics Data System (ADS)

Baba, Koichi; Konta, Sayaka; Oliveira, Daniel; Sugai, Kenji; Onodera, Tsunenobu; Masuhara, Akito; Kasai, Hitoshi; Oikawa, Hidetoshi; Nakanishi, Hachiro

2012-12-01

Organic nano-cocrystals of functional dyes of perylene and a perylene derivative were successfully prepared by the reprecipitation method. The particle sizes, optical properties, and powder X-ray diffraction patterns of nano-cocrystals were evaluated. Typically, the size with size distribution of nano-cocrystals was 55±15 nm when the molar ratio of perylene to the perylene derivative was 50:50. The particular intermolecular electronic interaction between perylene and the perylene derivative in the nano-cocrystal state was observed by absorption and fluorescence spectra measurements. The powder X-ray diffraction pattern analysis confirmed that the structure of nano-cocrystals was different from those prepared from perylene and the perylene derivative. The nano-cocrystal having unique physicochemical properties will be potentially classified as a new type of functional nanomaterial.

Fabrication and characterization of high-efficiency double-sided blazed x-ray optics.

PubMed

Mohacsi, Istvan; Vartiainen, Ismo; Guizar-Sicairos, Manuel; Karvinen, Petri; Guzenko, Vitaliy A; Müller, Elisabeth; Kewish, Cameron M; Somogyi, Andrea; David, Christian

2016-01-15

The focusing efficiency of conventional diffractive x-ray lenses is fundamentally limited due to their symmetric binary structures and the corresponding symmetry of their focusing and defocusing diffraction orders. Fresnel zone plates with asymmetric structure profiles can break this limitation; yet existing implementations compromise either on resolution, ease of use, or stability. We present a new way for the fabrication of such blazed lenses by patterning two complementary binary Fresnel zone plates on the front and back sides of the same membrane chip to provide a compact, inherently stable, single-chip device. The presented blazed double-sided zone plates with 200 nm smallest half-pitch provide up to 54.7% focusing efficiency at 6.2 keV, which is clearly beyond the value obtainable by their binary counterparts.

X-ray diffraction, FTIR, UV-VIS and SEM studies on chromium (III) complexes

NASA Astrophysics Data System (ADS)

Mishra, Ashutosh; Dwivedi, Jagrati; Shukla, Kritika

2015-06-01

Five Chromium (III) complexes have been prepared using Schiff base ligands which derived from benzoin and five different amino acids (H2N-R). Samples were characterized by XRD, FTIR, UV-VIS and SEM method. X-Ray diffraction pattern analyzed that all chromium (III) complexes have hexagonal structure and crystalline, in nature, using Bruker D8 Advance instrument. Using VERTAX 70, FTIR spectroscopy reveals that Samples have (C=N), (C-O), (M-N) and (M-O) bonds in the range of 4000-400cm-1. UV-VIS spectroscopy give information that samples absorb the visible light which is in the range of 380-780nm. For this, Lambda 960 spectrometer used. SEM is designed for studying of the solid objects, using JEOL JSM 5600 instrument.

Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

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

Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.

2016-08-15

Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from themore » sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10{sup 7} molybdenum Kα photons.« less

Preparation and Characterization of Niobium Doped Lead-Telluride Glass Ceramics

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

Sathish, M.; Eraiah, B.; Anavekar, R. V.

2011-07-15

Niobium-lead-telluride glass ceramics of composition xNb{sub 2}O{sub 5}-(20-x) pbO-80TeO{sub 2}(where x = 0.1 mol% to 0.5 mol%) were prepared by using conventional melt quenching method. The prepared glass samples were initially amorphous in nature after annealed at 400 deg. c all samples were crystallized. This was confined by X-ray diffraction and scanning electron microscopy. The particle size of these glass ceramics have been calculated by using Debye-Scherer formula and the particle size is in the order of 15 nm to 60 nm. The scanning electron microscopy (SEM) photograph shows the presence of needle-like crystals in these samples.

Structural studies of a green-emitting terbium doped calcium zinc phosphate phosphor

NASA Astrophysics Data System (ADS)

Ramesh, B.; Dillip, G. R.; Rambabu, B.; Joo, S. W.; Raju, B. Deva Prasad

2018-03-01

In this study, a new green emitting CaZn2(PO4)2:Tb3+ phosphors were synthesized through solid-state reaction route. The phosphors were characterized structurally by X-ray diffraction, Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS). All the synthesized phosphors were crystallized in triclinic crystal structure with P 1 bar space group. The phosphate groups in the phosphors were confirmed by FTIR analysis. The surface elements O 1s, P 2p, Ca 2p, Zn 2p and Tb 3d were studied by high-resolution XPS spectra. Upon excitation at 378 nm, the dominant green emission of CaZn2(PO4)2:Tb3+ phosphors at 542 nm were noticed in the emission spectra. For various emission wavelengths (at 435 and 489 nm) and constant excitation wavelength (at 378 nm), the decay curves have shown two different decay dynamics of phosphors. The lighting properties such as Commission International de l'Eclairage (x = 0.319, y = 0.398) and color temperature (5995 K) were calculated.

Synthesis and optical properties of silver nanoparticles

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

Singh, Jaiveer; Kaurav, Netram, E-mail: netramkaurav@yahoo.co.uk; Choudhary, K. K.

The preparation of stable, uniform silver nanoparticles by reduction of silver acetate by ethylene glycol (EG) is reported in the present paper. It is a simple process of recent interest for obtaining silver nanoparticles. The samples were characterized by X-Ray diffraction (XRD), which reveals an average particle size (D) of 38 nm. The UV/Vis spectra show that an absorption peak, occurring due to surface plasmon resonance (SPR), exists at 319 nm.

Comparative dielectric studies of nanostructured BaTiO{sub 3}, CaCu{sub 3}Ti{sub 4}O{sub 12} and 0.5BaTiO{sub 3}⋅ 0.5CaCu{sub 3}Ti{sub 4}O{sub 12} nano-composites synthesized by modified sol–gel and solid state methods

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

Singh, Laxman; Rai, Uma Shanker; Mandal, Kam Deo

2014-10-15

BaTiO{sub 3} (BTO), CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) and 0.5BaTiO{sub 3}·0.5CaCu{sub 3}Ti{sub 4}O{sub 12} (BTO–CCTO), as a new nano-composite ceramic, were successfully designed and fabricated by a semi-wet gel route and a modified solid state method. The dielectric properties of the BTO–CCTO ceramic were compared to those of the BTO and CCTO ceramics at lower sintering temperatures and durations. The X-ray diffraction analysis revealed that the BTO and CCTO ceramics form a single crystalline phase and the average crystalline sizes calculated from X-ray diffraction data were in the range of 40–65 nm. The particle sizes of the BTO, CCTO, andmore » BTO–CCTO ceramics obtained from transmission electron microscopy images were in the ranges of 40–65 nm, 80–110 nm, and 70–95 nm, respectively. The phase composition and microstructure were studied by X-ray diffraction and scanning electron microscopy. The energy dispersive X-ray results demonstrated the purity and stoichiometry of the BTO–CCTO nano-composite. The grain sizes of the BTO, CCTO and BTO–CCTO ceramics were found to be in the ranges of 500 nm–1 μm, 4–24 μm, and 250 nm–4 μm, respectively. The AC conductivity as a function of frequency confirmed the semiconducting nature of all of the ceramics and obeyed the Jonscher's power law. The impedance spectrum measurement result showed that the CCTO ceramic possessed an exceptional grain boundary resistance, which supports the internal barrier layer capacitance (IBLC) mechanism present in this ceramic and is responsible for the high ε{sub r} values. - Highlights: • Nanostructured BaTiO{sub 3}, CaCu{sub 3}Ti{sub 4}O{sub 12}, and 0.5BaTiO{sub 3}⋅ 0.5CaCu{sub 3}Ti{sub 4}O{sub 12} have been synthesized. • XRD and TEM analysis confirmed the formation of nanoparticles, 40–65 and 50–90 nm. • Impedance analysis shows high grain-boundary resistance present in CCTO ceramic. • AC conductivity as a function of frequency confirms the semiconducting nature.« less

ID16B: a hard X-ray nanoprobe beamline at the ESRF for nano-analysis

PubMed Central

Martínez-Criado, Gema; Villanova, Julie; Tucoulou, Rémi; Salomon, Damien; Suuronen, Jussi-Petteri; Labouré, Sylvain; Guilloud, Cyril; Valls, Valentin; Barrett, Raymond; Gagliardini, Eric; Dabin, Yves; Baker, Robert; Bohic, Sylvain; Cohen, Cédric; Morse, John

2016-01-01

Within the framework of the ESRF Phase I Upgrade Programme, a new state-of-the-art synchrotron beamline ID16B has been recently developed for hard X-ray nano-analysis. The construction of ID16B was driven by research areas with major scientific and societal impact such as nanotechnology, earth and environmental sciences, and bio-medical research. Based on a canted undulator source, this long beamline provides hard X-ray nanobeams optimized mainly for spectroscopic applications, including the combination of X-ray fluorescence, X-ray diffraction, X-ray excited optical luminescence, X-ray absorption spectroscopy and 2D/3D X-ray imaging techniques. Its end-station re-uses part of the apparatus of the earlier ID22 beamline, while improving and enlarging the spectroscopic capabilities: for example, the experimental arrangement offers improved lateral spatial resolution (∼50 nm), a larger and more flexible capability for in situ experiments, and monochromatic nanobeams tunable over a wider energy range which now includes the hard X-ray regime (5–70 keV). This paper describes the characteristics of this new facility, short-term technical developments and the first scientific results. PMID:26698084

Synthesis and x-ray characterization of sputtered bi-alkali antimonide photocathodes

DOE PAGES

Gaowei, M.; Ding, Z.; Schubert, S.; ...

2017-11-10

Advanced photoinjectors, which are critical to many next generation accelerators, open the door to new ways of material probing, both as injectors for free electron lasers and for ultra-fast electron diffraction. For these applications, the nonuniformity of the electric field near the cathode caused by surface roughness can be the dominant source of beam emittance. Therefore, improving the photocathode roughness while maintaining quantum efficiency is essential to the improvement of beam brightness. Here in this article, we report the demonstration of a bi-alkali antimonide photocathode with an order of magnitude improved roughness by sputter deposition from a K 2CsSb sputtermore » target, using in situ and operando X-ray characterizations. We found that a surface roughness of 0.5 nm for a sputtered photocathode with a final thickness of 42 nm can be achieved while still yielding a quantum efficiency of 3.3% at 530 nm wavelength.« less

Synthesis and x-ray characterization of sputtered bi-alkali antimonide photocathodes

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

Gaowei, M.; Ding, Z.; Schubert, S.

Advanced photoinjectors, which are critical to many next generation accelerators, open the door to new ways of material probing, both as injectors for free electron lasers and for ultra-fast electron diffraction. For these applications, the nonuniformity of the electric field near the cathode caused by surface roughness can be the dominant source of beam emittance. Therefore, improving the photocathode roughness while maintaining quantum efficiency is essential to the improvement of beam brightness. Here in this article, we report the demonstration of a bi-alkali antimonide photocathode with an order of magnitude improved roughness by sputter deposition from a K 2CsSb sputtermore » target, using in situ and operando X-ray characterizations. We found that a surface roughness of 0.5 nm for a sputtered photocathode with a final thickness of 42 nm can be achieved while still yielding a quantum efficiency of 3.3% at 530 nm wavelength.« less

Interfacial Electronic Structures of Photodetectors Based on C8BTBT/Perovskite.

PubMed

Li, Lin; Tong, Sichao; Zhao, Yuan; Wang, Can; Wang, Shitan; Lyu, Lu; Huang, Yingbao; Huang, Han; Yang, Junliang; Niu, Dongmei; Liu, Xiaoliang; Gao, Yongli

2018-06-07

Comprehensive measurements of ultraviolet photoemission spectroscopy, X-ray photoemission spectroscopy, X-ray diffraction, and atomic force microscopy are adopted to investigate the corelevance of energy level alignment, molecular orientation, and film growth of Au/C8BTBT/perovskite interfaces. A small energy offset of valence band maximum of 0.06 eV between perovskite and C8BTBT makes hole transportation feasible. About 0.65 eV upward shift of energy levels is observed with the deposition of the Au film on C8BTBT, which enhances hole transportation to the Au electrode. The observations from the interface analysis are supported by a prototype photodetector of Au (80 nm)/C8BTBT (20 nm)/perovskite (100 nm) that exhibits excellent performances whose responsivity can reach up to 2.65 A W -1 , 4 times higher than the best CH 3 NH 3 PbI 3 photodetectors.

Thermoelectric properties of CuS/Ag{sub 2}S nanocomposites synthesed by modified polyol method

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

Tarachand,, E-mail: tarachand@csr.res.in; Sharma, Vikash; Ganesan, V.

This is the report on successful synthesis of Ag doped CuS nanostructures by modified polyol method. The resulting samples were characterized by powder X-ray diffraction (XRD), energy dispersive X-ray (EDX), atomic force microscopy (AFM) and dynamic light scattering (DLS). Particle size of pure CuS nanoparticles (NPs) was 17 nm, 38 nm and 97 nm as determined from Scherrer formula, AFM and DLS, respectively. Introduction of Ag led to formation of CuS/Ag{sub 2}S composites. A transition at 55 K in thermopower is ascribed to structural transformation from hexagonal to orthorhombic structure. Further, their thermoelectric properties exhibit remarkable change owing to Agmore » doping in CuS nanostructures. The power factor improves with increasing Ag content. They reveal that CuS/Ag{sub 2}S nanocomposites are some of the potential candidates for generation of thermoelectricity in future.« less

Combustion synthesis and characterization of blue long lasting phosphor CaAl2O4: Eu2+, Dy3+ and its novel application in latent fingerprint and lip mark detection

NASA Astrophysics Data System (ADS)

Sharma, Vishal; Das, Amrita; Kumar, Vijay; Kumar, Vinay; Verma, Kartikey; Swart, H. C.

2018-04-01

This work investigates the structural, optical and photometric characterization of a Eu2+/Dy3+ doped calcium aluminates phosphor (CaAl2O4: Eu2+/Dy3+) for finger and lip print detections. Synthesis of CaAl2O4: Eu2+/Dy3+ (CAED) phosphors were carried out via a combustion synthesis method with urea as a fuel. Eu2+/Dy3+ doped CaAl2O4 phosphors have been studied with X-ray diffraction (XRD, Energy Dispersive X-Ray Spectroscopy Selected Area Diffraction (SAED) and High resolution Transmission Electron Microscope (HR-TEM). The XRD pattern shows that the synthesized Eu2+/Dy3+ doped CaAl2O4 phosphor have a single monoclinic structure and show that the addition of the dopant/co-dopants didn't change the crystal structure. The formation of monoclinic phase was confirmed by the selected area diffraction pattern. The TEM micrograph displays the morphology of the synthesized Eu2+/Dy3+ doped CaAl2O4 phosphors as spherical particles with an average particle size of 33 nm. The optical band gap was calculated using the diffuse reflectance for the synthesized nanophosphor powders. The photoluminescence emission spectra was recorded for the synthesized powder, with an excitation wavelength of 326 nm and the major bands was recorded at 447 nm corresponding to the blue color and two minor bands were recorded at 577 nm and 616 nm. To the best of our knowledge, this work is the first to show the use of CaAl2O4: Eu2+/Dy3+ nanophosphor in developing latent fingerprint and lip print effectively.

Mulberry leaf extract mediated synthesis of gold nanoparticles and its anti-bacterial activity against human pathogens

NASA Astrophysics Data System (ADS)

Adavallan, K.; Krishnakumar, N.

2014-06-01

Gold nanoparticles (Au-NPs) were synthesized at room temperature using Morus alba (mulberry) leaf extract as reducing and stabilizing agent. The development of plant mediated synthesis of nanoparticles is gaining importance due to its simplicity, low cost, non-toxicity, eco-friendliness, long term stability and reproducible aqueous synthesis method to obtain a self-assembly of nearly monodispersed Au-NPs. The formation and morphology of biosynthesized nanoparticles are investigated with the help of UV-Vis spectroscopy, dynamic light scattering (DLS), transmission electron microscopy (TEM), atomic force microscopy (AFM), x-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR) techniques. Au-NPs formation was screened by UV-Vis spectroscopy through color conversion due to surface plasmon resonance band at 538 nm for Au-NPs. DLS studies revealed that the average size of Au-NPs was 50 nm. TEM studies showed the particles to be nearly spherical with few irregular shapes and particle size ranges 15-53 nm. The AFM image clearly shows the surface morphology of the well-dispersed Au-NPs with less than 50 nm. The high crystallinity of nanoparticles is evident from bright circular spots in the selected area electron diffraction (SAED) pattern. X-ray diffraction pattern showed high purity and face-centered cubic structure of Au-NPs. The FT-IR results indicate the presence of different functional groups present in the biomolecule capping the nanoparticles. Further, biosynthesized Au-NPs show strong zone of inhibition against Vibrio cholera (gram-negative) and Staphylococcus aureus (gram-positive) whereas, chemically synthesized Au-NPs and mulberry leaf extract exhibit a fair zone of inhibition.

The preparation and cathodoluminescence of ZnS nanowires grown by chemical vapor deposition

NASA Astrophysics Data System (ADS)

Huang, Meng-Wen; Cheng, Yin-Wei; Pan, Ko-Ying; Chang, Chen-Chuan; Shieu, F. S.; Shih, Han C.

2012-11-01

Single crystal ZnS nanowires were successfully synthesized in large quantities on Si (1 0 0) substrates by simple thermal chemical vapor deposition without using any catalyst. The morphology, composition, and crystal structure were characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and cathodoluminescence (CL) spectroscopy. SEM observations show that the nanowires have diameters about 20-50 nm and lengths up to several tens of micrometers. XRD and TEM results confirmed that the nanowires exhibited both wurtzite and zinc blende structures with growth directions aligned along [0 0 0 2] and [1 1 1], respectively. The CL spectrum revealed emission bands in the UV and blue regions. The blue emissions at 449 and ˜581 nm were attributed to surface states and impurity-related defects of the nanowires, respectively. The perfect crystal structure of the nanowires indicates their potential applications in nanotechnology and in the fabrication of nanodevices.

X-Ray Diffraction Apparatus

NASA Technical Reports Server (NTRS)

Blake, David F. (Inventor); Bryson, Charles (Inventor); Freund, Friedmann (Inventor)

1996-01-01

An x-ray diffraction apparatus for use in analyzing the x-ray diffraction pattern of a sample is introduced. The apparatus includes a beam source for generating a collimated x-ray beam having one or more discrete x-ray energies, a holder for holding the sample to be analyzed in the path of the beam, and a charge-coupled device having an array of pixels for detecting, in one or more selected photon energy ranges, x-ray diffraction photons produced by irradiating such a sample with said beam. The CCD is coupled to an output unit which receives input information relating to the energies of photons striking each pixel in the CCD, and constructs the diffraction pattern of photons within a selected energy range striking the CCD.

Analysis of energy dispersive x-ray diffraction profiles for material identification, imaging and system control

NASA Astrophysics Data System (ADS)

Cook, Emily Jane

2008-12-01

This thesis presents the analysis of low angle X-ray scatter measurements taken with an energy dispersive system for substance identification, imaging and system control. Diffraction measurements were made on illicit drugs, which have pseudo- crystalline structures and thus produce diffraction patterns comprising a se ries of sharp peaks. Though the diffraction profiles of each drug are visually characteristic, automated detection systems require a substance identification algorithm, and multivariate analysis was selected as suitable. The software was trained with measured diffraction data from 60 samples covering 7 illicit drugs and 5 common cutting agents, collected with a range of statistical qual ities and used to predict the content of 7 unknown samples. In all cases the constituents were identified correctly and the contents predicted to within 15%. Soft tissues exhibit broad peaks in their diffraction patterns. Diffraction data were collected from formalin fixed breast tissue samples and used to gen erate images. Maximum contrast between healthy and suspicious regions was achieved using momentum transfer windows 1.04-1.10 and 1.84-1.90 nm_1. The resulting images had an average contrast of 24.6% and 38.9% compared to the corresponding transmission X-ray images (18.3%). The data was used to simulate the feedback for an adaptive imaging system and the ratio of the aforementioned momentum transfer regions found to be an excellent pa rameter. Investigation into the effects of formalin fixation on human breast tissue and animal tissue equivalents indicated that fixation in standard 10% buffered formalin does not alter the diffraction profiles of tissue in the mo mentum transfer regions examined, though 100% unbuffered formalin affects the profile of porcine muscle tissue (a substitute for glandular and tumourous tissue), though fat is unaffected.

Alternating current magnetic susceptibility and heat dissipation by Mn1-xZnxFe2O4 nanoparticles for hyperthermia treatment

NASA Astrophysics Data System (ADS)

Kondo, T.; Mori, K.; Hachisu, M.; Yamazaki, T.; Okamoto, D.; Watanabe, M.; Gonda, K.; Tada, H.; Hamada, Y.; Takano, M.; Ohuchi, N.; Ichiyanagi, Y.

2015-05-01

Mn-Zn ferrite, Mn1-xZnxFe2O4 nanoparticles encapsulated in amorphous SiO2 were prepared using our original wet chemical method. X-ray diffraction patterns confirmed that the diameters of these particles were within 7-30 nm. Magnetization measurements for various sample compositions revealed that the saturation magnetization (Ms) of 7 nm particles was maximum for the x = 0.2 sample. AC magnetic susceptibility measurements were performed for Mn0.8Zn0.2Fe2O4 (x = 0.2) samples with 13-30 nm particles. The peak of the imaginary part of the magnetic susceptibility χ″ shifted to higher temperatures as the particle size increased. An AC field was found to cause the increase in temperature, with the 18 nm particles exhibiting the highest temperature increase, as expected. In addition, in vitro experiments were carried out to study the hyperthermia effects of Mn1-xZnxFe2O4 (x = 0.2, 18 nm) particles on human cancer cells.

Development of at-wavelength metrology for x-ray optics at the ALS

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

Yashchuk, Valeriy V.; Goldberg, Kenneth A.; Yuan, Sheng

2010-07-09

The comprehensive realization of the exciting advantages of new third- and forth-generation synchrotron radiation light sources requires concomitant development of reflecting and diffractive x-ray optics capable of micro- and nano-focusing, brightness preservation, and super high resolution. The fabrication, tuning, and alignment of the optics are impossible without adequate metrology instrumentation, methods, and techniques. While the accuracy of ex situ optical metrology at the Advanced Light Source (ALS) has reached a state-of-the-art level, wavefront control on beamlines is often limited by environmental and systematic alignment factors, and inadequate in situ feedback. At ALS beamline 5.3.1, we are developing broadly applicable, high-accuracy,more » in situ, at-wavelength wavefront measurement techniques to surpass 100-nrad slope measurement accuracy for Kirkpatrick-Baez (KB) mirrors. The at-wavelength methodology we are developing relies on a series of tests with increasing accuracy and sensitivity. Geometric Hartmann tests, performed with a scanning illuminated sub-aperture determine the wavefront slope across the full mirror aperture. Shearing interferometry techniques use coherent illumination and provide higher sensitivity wavefront measurements. Combining these techniques with high precision optical metrology and experimental methods will enable us to provide in situ setting and alignment of bendable x-ray optics to realize diffraction-limited, sub 50 nm focusing at beamlines. We describe here details of the metrology beamline endstation, the x-ray beam diagnostic system, and original experimental techniques that have already allowed us to precisely set a bendable KB mirror to achieve a focused spot size of 150 nm.« less

One-dimensional nanoferroic rods; synthesis and characterization

NASA Astrophysics Data System (ADS)

Ahmed, M. A.; Seddik, U.; Okasha, N.; Imam, N. G.

2015-11-01

One-dimensional nanoferroic rods of BaTiO3 were synthesized by improved citrate auto-combustion technology using tetrabutyl titanate. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), atomic force microscopy (AFM) and Fourier transform infrared spectroscopy (FTIR) have been used to characterize the prepared sample. The results indicated that the crystal structure of BaTiO3 is tetragonal phase with an average crystallite size of 47 nm. SEM image gives a cauliflower-like morphology of the agglomerated nanorods. The stoichiometry of the chemical composition of the BaTiO3 ceramic was confirmed by EDX. TEM micrograph exhibited that BaTiO3 nanoparticles have rod-like shape with an average length of 120 nm and width of 43 nm. AFM was used to investigate the surface topography and its roughness. The topography image in 3D showed that the BaTiO3 particles have a rod shape with an average particle size of 116 nm which in agreement with 3D TEM result.

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

NASA Technical Reports Server (NTRS)

Rosemeier, R. G.

1984-01-01

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

Radiation damage free ghost diffraction with atomic resolution

DOE PAGES

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.; ...

2017-12-21

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Radiation damage free ghost diffraction with atomic resolution

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

Li, Zheng; Medvedev, Nikita; Chapman, Henry N.

The x-ray free electron lasers can enable diffractive structural determination of protein nanocrystals and single molecules that are too small and radiation-sensitive for conventional x-ray diffraction. However the electronic form factor may be modified during the ultrashort x-ray pulse due to photoionization and electron cascade caused by the intense x-ray pulse. For general x-ray imaging techniques, the minimization of the effects of radiation damage is of major concern to ensure reliable reconstruction of molecular structure. Here in this paper, we show that radiation damage free diffraction can be achieved with atomic spatial resolution by using x-ray parametric down-conversion and ghostmore » diffraction with entangled photons of x-ray and optical frequencies. We show that the formation of the diffraction patterns satisfies a condition analogous to the Bragg equation, with a resolution that can be as fine as the crystal lattice length scale of several Ångstrom. Since the samples are illuminated by low energy optical photons, they can be free of radiation damage.« less

Synchrotron Radiation X-ray Diffraction Techniques Applied to Insect Flight Muscle.

PubMed

Iwamoto, Hiroyuki

2018-06-13

X-ray fiber diffraction is a powerful tool used for investigating the molecular structure of muscle and its dynamics during contraction. This technique has been successfully applied not only to skeletal and cardiac muscles of vertebrates but also to insect flight muscle. Generally, insect flight muscle has a highly ordered structure and is often capable of high-frequency oscillations. The X-ray diffraction studies on muscle have been accelerated by the advent of 3rd-generation synchrotron radiation facilities, which can generate brilliant and highly oriented X-ray beams. This review focuses on some of the novel experiments done on insect flight muscle by using synchrotron radiation X-rays. These include diffraction recordings from single myofibrils within a flight muscle fiber by using X-ray microbeams and high-speed diffraction recordings from the flight muscle during the wing-beat of live insects. These experiments have provided information about the molecular structure and dynamic function of flight muscle in unprecedented detail. Future directions of X-ray diffraction studies on muscle are also discussed.

X-ray peak profile analysis of zinc oxide nanoparticles formed by simple precipitation method

NASA Astrophysics Data System (ADS)

Pelicano, Christian Mark; Rapadas, Nick Joaquin; Magdaluyo, Eduardo

2017-12-01

Zinc oxide (ZnO) nanoparticles were successfully synthesized by a simple precipitation method using zinc acetate and tetramethylammonium hydroxide. The synthesized ZnO nanoparticles were characterized by X-ray Diffraction analysis (XRD) and Transmission Electron Microscopy (TEM). The XRD result revealed a hexagonal wurtzite structure for the ZnO nanoparticles. The TEM image showed spherical nanoparticles with an average crystallite size of 6.70 nm. For x-ray peak analysis, Williamson-Hall (W-H) and Size-Strain Plot (SSP) methods were applied to examine the effects of crystallite size and lattice strain on the peak broadening of the ZnO nanoparticles. Based on the calculations, the estimated crystallite sizes and lattice strains obtained are in good agreement with each other.

High resolution x-ray microtomography of biological samples: Requirements and strategies for satisfying them

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

Loo, B.W. Jr.

High resolution x-ray microscopy has been made possible in recent years primarily by two new technologies: microfabricated diffractive lenses for soft x-rays with about 30-50 nm resolution, and high brightness synchrotron x-ray sources. X-ray microscopy occupies a special niche in the array of biological microscopic imaging methods. It extends the capabilities of existing techniques mainly in two areas: a previously unachievable combination of sub-visible resolution and multi-micrometer sample size, and new contrast mechanisms. Because of the soft x-ray wavelengths used in biological imaging (about 1-4 nm), XM is intermediate in resolution between visible light and electron microscopies. Similarly, the penetrationmore » depth of soft x-rays in biological materials is such that the ideal sample thickness for XM falls in the range of 0.25 - 10 {mu}m, between that of VLM and EM. XM is therefore valuable for imaging of intermediate level ultrastructure, requiring sub-visible resolutions, in intact cells and subcellular organelles, without artifacts produced by thin sectioning. Many of the contrast producing and sample preparation techniques developed for VLM and EM also work well with XM. These include, for example, molecule specific staining by antibodies with heavy metal or fluorescent labels attached, and sectioning of both frozen and plastic embedded tissue. However, there is also a contrast mechanism unique to XM that exists naturally because a number of elemental absorption edges lie in the wavelength range used. In particular, between the oxygen and carbon absorption edges (2.3 and 4.4 nm wavelength), organic molecules absorb photons much more strongly than does water, permitting element-specific imaging of cellular structure in aqueous media, with no artifically introduced contrast agents. For three-dimensional imaging applications requiring the capabilities of XM, an obvious extension of the technique would therefore be computerized x-ray microtomography (XMT).« less

Lasing and Longitudinal Cavity Modes in Photo-Pumped Deep Ultraviolet AlGaN Heterostructures

DTIC Science & Technology

2013-04-29

of the structures were intentionally doped. The AlGaN composition was determined by triple -axis high-resolution X-ray diffraction measurements. Cross...threshold can be achieved on single crystal AlN substrates. This achievement serves as a starting point towards realizing electrically pumped sub-300 nm UV

In situ hydrothermal syntheses, structures and photoluminescent properties of four novel metal-organic frameworks constructed by lanthanide (Ln=Ce(III), Pr(III), Eu(III)) and Cu(I) metals with flexible dicarboxylate acids and piperazine-based ligands

NASA Astrophysics Data System (ADS)

Ay, Burak; Karaca, Serkan; Yildiz, Emel; Lopez, Valerie; Nanao, Max H.; Zubieta, Jon

2016-01-01

Four novel metal-organic frameworks,[Cu2Cl2(pyrz)]n (1) and (H2pip)n[Ln2(pydc)4(H2O)2]n (Ln=Ce (2), Pr (3) and Eu (4), H2pzdc=2,3-pyrazinedicarboxylic acid, pyrz=pyrazine, H2pydc=2,6-pyridinedicarboxylic acid, H2pip=piperazine) have been synthesized under hydrothermal conditions and characterized by the elemental analysis, ICP, Far IR (FIR), FT-IR spectra, TGA, single crystal X-ray diffraction analysis and powder X-ray diffraction (PXRD). Compound 1 is two-dimensional containing Cl-Cu-Cl sites, while the lanthanide complexes contain one-dimensional infinite Ln-O-Ln chains. All the complexes show high thermal stability. The complexes 1-3 exhibit luminescence emission bands at 584, 598 and 614 nm at room temperature when excited at 300 nm. Complex 4 exhibits bright red solid-state phosphorescence upon exposure to UV radiation at room temperature.

Green synthesis of silver nanoparticles using marine algae Caulerpa racemosa and their antibacterial activity against some human pathogens

NASA Astrophysics Data System (ADS)

Kathiraven, T.; Sundaramanickam, A.; Shanmugam, N.; Balasubramanian, T.

2015-04-01

We present the synthesis and antibacterial activity of silver nanoparticles using Caulerpa racemosa, a marine algae. Fresh C. racemosa was collected from the Gulf of Mannar, Southeast coast of India. The seaweed extract was used for the synthesis of AgNO3 at room temperature. UV-visible spectrometry study revealed surface plasmon resonance at 413 nm. The characterization of silver nanoparticle was carried out using Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and transmission electron microscope (TEM). FT-IR measurements revealed the possible functional groups responsible for reduction and stabilization of the nanoparticles. X-ray diffraction analysis showed that the particles were crystalline in nature with face-centered cubic geometry.TEM micrograph has shown the formation of silver nanoparticles with the size in the range of 5-25 nm. The synthesized AgNPs have shown the best antibacterial activity against human pathogens such as Staphylococcus aureus and Proteus mirabilis. The above eco-friendly synthesis procedure of AgNPs could be easily scaled up in future for the industrial and therapeutic needs.

Strain relaxation of CdTe on Ge studied by medium energy ion scattering

NASA Astrophysics Data System (ADS)

Pillet, J. C.; Pierre, F.; Jalabert, D.

2016-10-01

We have used the medium energy ion scattering (MEIS) technique to assess the strain relaxation in molecular-beam epitaxial (MBE) grown CdTe (2 1 1)/Ge (2 1 1) system. A previous X-ray diffraction study, on 10 samples of the same heterostructure having thicknesses ranging from 25 nm to 10 μm has allowed the measurement of the strain relaxation on a large scale. However, the X-ray diffraction measurements cannot achieve a stress measurement in close proximity to the CdTe/Ge interface at the nanometer scale. Due to the huge lattice misfit between the CdTe and Ge, a high degree of disorder is expected at the interface. The MEIS in channeling mode is a good alternative in order to profile defects with a high depth resolution. For a 21 nm thick CdTe layer, we observed, at the interface, a high density of Cd and/or Te atoms moved from their expected crystallographic positions followed by a rapid recombination of defects. Strain relaxation mechanisms in the vicinity of the interface are discussed

Optical, Magnetic and Photocatalytic Activity Studies of Li, Mg and Sr Doped and Undoped Zinc Oxide Nanoparticles.

PubMed

Shanthi, S I; Poovaragan, S; Arularasu, M V; Nithya, S; Sundaram, R; Magdalane, C Maria; Kaviyarasu, K; Maaza, M

2018-08-01

Nanoparticles of Li, Mg and Sr doped and undoped zinc oxide was prepared by simple precipitation method. The structural, optical, and magnetic properties of the samples were investigated by the Powder X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Fourier Transform Infrared (FTIR) spectroscopy, Ultra-violet Visible spectroscopy (UV-vis) spectra, Photoluminescence (PL) and Vibrational Sample Magnetometer (VSM). The Powder X-ray diffraction data confirm the formation of hexagonal wurtzite structure of all doped and undoped ZnO. The SEM photograph reveals that the pores availability and particles size in the range of 10 nm-50 nm. FTIR and UV-Visible spectra results confirm the incorporation of the dopant into the ZnO lattice nanostructure. The UV-Visible spectra indicate that the shift of blue region (lower wavelength) due to bandgap widening. Photoluminescence intensity varies with doping due to the increase of oxygen vacancies in prepared ZnO. The pure ZnO exist paramagnetic while doped (Li, Mg and Sr) ZnO exist ferromagnetic property. The photocatalytic activity of the prepared sample also carried out in detail.

Luminescence study of ZnSe/PVA (polyvinyl alcohol) composite film

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

Lahariya, Vikas

The ZnSe nanocrystals have been prepared into poly vinyl alcohol(PVA) polymer matrix on glass using ZnCl2 and Na2SeSO3 as zinc and selenium source respectively. Poly vinyl Alcohol (PVA) used as polymer matrix cum capping agent due to their high viscosity and water solubility. It is transparent for visible region and prevents Se- ions to photo oxidation. The ZnSe/PVA composite film was deposited on glass substrate. The film was characterized by X Ray Diffraction (XRD) and UV-Visible absorption Spectroscopy and Photoluminescence. The X Ray Diffraction (XRD) study confirms the nanometer size (10 nm) particle formation within PVA matrix with cubic zinc blendmore » crystal structure. The UV-Visible Absorption spectrum of ZnSe/PVA composite film shown blue shift in absorption edge indicating increased band gap due to quantum confinement. The calculated energy band gap from the absorption edge using Tauc relation is 3.4 eV. From the Photoluminescence study a broad peak at 435 nm has been observed in violet blue region due to recombination of surface states.« less

Large exchange bias effect in NiFe2O4/CoO nanocomposites

NASA Astrophysics Data System (ADS)

Mohan, Rajendra; Prasad Ghosh, Mritunjoy; Mukherjee, Samrat

2018-03-01

In this work, we report the exchange bias effect of NiFe2O4/CoO nanocomposites, synthesized via chemical co-precipitation method. Four samples of different particle size ranging from 4 nm to 31 nm were prepared with the annealing temperature varying from 200 °C to 800 °C. X-ray diffraction analysis of all the samples confirmed the presence of cubic spinel phase of Nickel ferrite along with CoO phase without trace of any impurity. Sizes of the particles were studied from transmission electron micrographs and were found to be in agreement with those estimated from x-ray diffraction. Field cooled (FC) hysteresis loops at 5 K revealed an exchange bias (HE) of 2.2 kOe for the sample heated at 200 °C which decreased with the increase of particle size. Exchange bias expectedly vanished at 300 K due to high thermal energy (kBT) and low effective surface anisotropy. M-T curves revealed a blocking temperature of 135 K for the sample with smaller particle size.

Ultrathin Cr added Ru film as a seedless Cu diffusion barrier for advanced Cu interconnects

NASA Astrophysics Data System (ADS)

Hsu, Kuo-Chung; Perng, Dung-Ching; Yeh, Jia-Bin; Wang, Yi-Chun

2012-07-01

A 5 nm thick Cr added Ru film has been extensively investigated as a seedless Cu diffusion barrier. High-resolution transmission electron microscopy micrograph, X-ray diffraction (XRD) pattern and Fourier transform-electron diffraction pattern reveal that a Cr contained Ru (RuCr) film has a glassy microstructure and is an amorphous-like film. XRD patterns and sheet resistance data show that the RuCr film is stable up to 650 °C, which is approximately a 200 °C improvement in thermal stability as compared to that of the pure Ru film. X-ray photoelectron spectroscopy depth profiles show that the RuCr film can successfully block Cu diffusion, even after a 30-min 650 °C annealing. The leakage current of the Cu/5 nm RuCr/porous SiOCH/Si stacked structure is about two orders of magnitude lower than that of a pristine Ru sample for electric field below 1 MV/cm. The RuCr film can be a promising Cu diffusion barrier for advanced Cu metallization.

High-resolution x-ray diffraction and transmission electron microscopy of multiferroic BiFeO3 films

NASA Astrophysics Data System (ADS)

Qi, Xiaoding; Wei, Ming; Lin, Yuan; Jia, Quanxi; Zhi, Dan; Dho, Joonghoe; Blamire, Mark G.; MacManus-Driscoll, Judith L.

2005-02-01

High-resolution x-ray diffraction and transmission electron microscopy (TEM) have been used to study BiFeO3 thin films grown on the bare and SrRuO3 buffered (001) SrTiO3 substrates. Reciprocal space mapping (RSM) around (002) and (103) reflections revealed that BFO films with a thickness of about 200 nm were almost fully relaxed and had a rhombohedral structure. Cross-sectional, high-resolution TEM showed that the films started to relax at a very early stage of growth, which was consistent with the RSM results. A thin intermediate layer of about 2 nm was observed at the interface, which had a smaller lattice than the overgrown film. Twist distortions about the c axis to release the shear strain introduced by the growth of rhombic (001) BiFeO3 on cubic (001) SrTiO3 were also observed. The results indicate that a strained, coherent BiFeO3 film on (001) SrTiO3 is very difficult to maintain and (111) STO substrates are preferable.

Physicochemical and antibacterial characterization of ionocity Ag/Cu powder nanoparticles

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

Nowak, A., E-mail: ana.maria.nowak@gmail.com; Silesian Center for Education and Interdisciplinary Research, 75 Pułku Piechoty 1A, 41-500 Chorzów; Szade, J.

Metal ion in bimetallic nanoparticles has shown vast potential in a variety of applications. In this paper we show the results of physical and chemical investigations of powder Ag/Cu nanoparticles obtained by chemical synthesis. Transmission electron microscopy (TEM) experiment indicated the presence of bimetallic nanoparticles in the agglomerated form. The average size of silver and copper nanoparticles is 17.1(4) nm (Ag) and 28.9(2) nm (Cu) basing on the X-ray diffraction (XRD) data. X-ray photoelectron (XPS) and Raman spectroscopies revealed the existence of metallic silver and copper as well as Cu{sub 2}O and CuO being a part of the nanoparticles. Moreover,more » UV–Vis spectroscopy showed surface alloy of Ag and Cu while Time of Flight Secondary Ion Mass Spectroscopy (ToF-SIMS) and Energy Dispersive X-ray Spectroscopy (EDX) showed heterogeneously distributed Ag structures placed on spherical Cu nanoparticles. The tests of antibacterial activity show promising killing/inhibiting growth behaviour for Gram positive and Gram negative bacteria. - Highlights: • Ag/Cu nanoparticles were obtained in the powder form. • The average size of nanoparticles is 17.1(4) nm (Ag) and 28.9(2) nm (Cu). • Ag/Cu powder nanoparticle shows promising antibacterial properties.« less

One-pot nucleation, growth, morphogenesis, and passivation of 1.4 nm Au nanoparticles on self-assembled rosette nanotubes.

PubMed

Chhabra, Rahul; Moralez, Jesus G; Raez, Jose; Yamazaki, Takeshi; Cho, Jae-Young; Myles, Andrew J; Kovalenko, Andriy; Fenniri, Hicham

2010-01-13

A one-pot strategy for the nucleation, growth, morphogenesis, and passivation of 1.4 nm Au nanoparticles (NPs) on self-assembled rosette nanotubes (RNTs) is described. Tapping-mode atomic force microscopy, transmission electron microscopy, energy-dispersive X-ray analysis, and selected-area electron diffraction were used to establish the structure and organization of this hybrid material. Notably, we found that the Au NPs formed were nearly monodisperse clusters of Au(55) (1.4-1.5 nm) nestled in pockets on the RNT surface.

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Transverse Coherence Limited Coherent Diffraction Imaging using a Molybdenum Soft X-ray Laser Pumped at Moderate Pump Energies.

PubMed

Zürch, M; Jung, R; Späth, C; Tümmler, J; Guggenmos, A; Attwood, D; Kleineberg, U; Stiel, H; Spielmann, C

2017-07-13

Coherent diffraction imaging (CDI) in the extreme ultraviolet has become an important tool for nanoscale investigations. Laser-driven high harmonic generation (HHG) sources allow for lab scale applications such as cancer cell classification and phase-resolved surface studies. HHG sources exhibit excellent coherence but limited photon flux due poor conversion efficiency. In contrast, table-top soft X-ray lasers (SXRL) feature excellent temporal coherence and extraordinary high flux at limited transverse coherence. Here, the performance of a SXRL pumped at moderate pump energies is evaluated for CDI and compared to a HHG source. For CDI, a lower bound for the required mutual coherence factor of |μ 12 | ≥ 0.75 is found by comparing a reconstruction with fixed support to a conventional characterization using double slits. A comparison of the captured diffraction signals suggests that SXRLs have the potential for imaging micron scale objects with sub-20 nm resolution in orders of magnitude shorter integration time compared to a conventional HHG source. Here, the low transverse coherence diameter limits the resolution to approximately 180 nm. The extraordinary high photon flux per laser shot, scalability towards higher repetition rate and capability of seeding with a high harmonic source opens a route for higher performance nanoscale imaging systems based on SXRLs.

Achromatic nested Kirkpatrick–Baez mirror optics for hard X-ray nanofocusing

PubMed Central

Liu, Wenjun; Ice, Gene E.; Assoufid, Lahsen; Liu, Chian; Shi, Bing; Khachatryan, Ruben; Qian, Jun; Zschack, Paul; Tischler, Jonathan Z.; Choi, J.-Y.

2011-01-01

The first test of nanoscale-focusing Kirkpatrick–Baez (KB) mirrors in the nested (or Montel) configuration used at a hard X-ray synchrotron beamline is reported. The two mirrors are both 40 mm long and coated with Pt to produce a focal length of 60 mm at 3 mrad incident angle, and collect up to a 120 µm by 120 µm incident X-ray beam with maximum angular acceptance of 2 mrad and a broad bandwidth of energies up to 30 keV. In an initial test a focal spot of about 150 nm in both horizontal and vertical directions was achieved with either polychromatic or monochromatic beam. The nested mirror geometry, with two mirrors mounted side-by-side and perpendicular to each other, is significantly more compact and provides higher demagnification than the traditional sequential KB mirror arrangement. Ultimately, nested mirrors can focus larger divergence to improve the diffraction limit of achromatic optics. A major challenge with the fabrication of the required mirrors is the need for near-perfect mirror surfaces near the edge of at least one of the mirrors. Special polishing procedures and surface profile coating were used to preserve the mirror surface quality at the reflecting edge. Further developments aimed at achieving diffraction-limited focusing below 50 nm are underway. PMID:21685674

Synthesis and surface characterization of alumina-silica-zirconia nanocomposite ceramic fibres on aluminium at room temperature

NASA Astrophysics Data System (ADS)

Mubarak Ali, M.; Raj, V.

2010-04-01

Alumina-silica-zirconia nanocomposite (ASZNC) ceramic fibres were synthesized by conventional anodization route. Scanning Electron Microscopy (SEM), Atomic Force microscopy (AFM), X-Ray Diffraction (XRD) and Energy Dispersive X-Ray spectroscopy (EDAX) were used to characterize the morphology and crystalloid structure of ASZNC fibres. Current density (DC) is one of the important parameters to get the alumina-silica-zirconia nanocomposite (ASZNC) ceramic fibres by this route. Annealing of the films exhibited a drastic change in the properties due to improved crystallinity. The root mean square roughness of the sample observed from atomic force microscopic analysis is about 71.5 nm which is comparable to the average grain size of the coatings which is about 72 nm obtained from X-Ray diffraction. The results indicate that, the ASZNC fibres are arranged well in the nanostructure. The thickness of the coating increased with the anodizing time, but the coatings turned rougher and more porous. At the initial stage the growth of ceramic coating increases inwards to the metal substrate and outwards to the coating surface simultaneously. Subsequently, it mainly grows towards the metal substrate and the density of the ceramic coating increases gradually, which results in the decrease of the total thickness as anodizing time increases. This new approach of preparing ASZNC ceramic fibres may be important in applications ranging from gas sensors to various engineering materials.

Combining experiment and optical simulation in coherent X-ray nanobeam characterization of Si/SiGe semiconductor heterostructures

DOE PAGES

Tilka, J. A.; Park, J.; Ahn, Y.; ...

2016-07-06

Here, the highly coherent and tightly focused x-ray beams produced by hard x-ray light sources enable the nanoscale characterization of the structure of electronic materials but are accompanied by significant challenges in the interpretation of diffraction and scattering patterns. X-ray nanobeams exhibit optical coherence combined with a large angular divergence introduced by the x-ray focusing optics. The scattering of nanofocused x-ray beams from intricate semiconductor heterostructures produces a complex distribution of scattered intensity. We report here an extension of coherent xray optical simulations of convergent x-ray beam diffraction patterns to arbitrary x-ray incident angles to allow the nanobeam diffraction patternsmore » of complex heterostructures to be simulated faithfully. These methods are used to extract the misorientation of lattice planes and the strain of individual layers from synchrotron x-ray nanobeam diffraction patterns of Si/SiGe heterostructures relevant to applications in quantum electronic devices. The systematic interpretation of nanobeam diffraction patterns from semiconductor heterostructures presents a new opportunity in characterizing and ultimately designing electronic materials.« less

Depth-resolved magnetic and structural analysis of relaxing epitaxial Sr 2 CrReO 6

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

Lucy, J. M.; Hauser, A. J.; Liu, Y.

2015-03-01

Structural relaxation in a Sr2CrReO6 epitaxial film, which exhibits strong spin-orbit coupling, leads to depth-dependent magnetism. We combine two depth-resolved synchrotron x-ray techniques, two-dimensional reciprocal space mapping and x-ray magnetic circular dichroism, to quantitatively determine this effect. An 800 nm thick film of Sr2CrReO6, grown with tensile epitaxial strain on SrCr0:5Nb0:5O3(225 nm)/LSAT, relaxes away from the Sr2CrReO6/SrCr0:5Nb0:5O3 interface to its bulk lattice parameters, with much of the film being fully relaxed. Grazing incidence xray diffraction measurements of the film elucidate the in-plane strain relaxation near the film- substrate interface while depth-resolved x-ray magnetic circular dichroism at the Re L edgemore » reveals the magnetic contributions of the Re site. The smooth relaxation of the film near the interface correlates with changes in the magnetic anisotropy. This provides a systematic and powerful way to probe the depth-varying structural and magnetic properties of a complex oxide with synchrotronsource x-ray techniques.« less

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

DOE PAGES

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

2016-10-06

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

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

Soni, Abhishek Kumar; Rai, Vineet Kumar, E-mail: vineetkrrai@yahoo.co.in

Erbium ion (Er{sup 3+}) doped BaMoO{sub 4} phosphor has been synthesized via co-precipitation technique. Phase formation of the prepared phosphor has been recognized by powder X-ray diffraction analysis. The photoluminescence emission spectrum has been recorded in 400-800nm wavelength range under 380nm excitation. The observed photoluminescence peaks are explained with the help of energy level structure. The prepared phosphor seems capable to produce efficient blue colour emission which can be useful for making blue light emitting diodes (LEDs).

Facile green synthesis of fluorescent N-doped carbon dots from Actinidia deliciosa and their catalytic activity and cytotoxicity applications

NASA Astrophysics Data System (ADS)

Arul, Velusamy; Sethuraman, Mathur Gopalakrishnan

2018-04-01

Green synthesis of fluorescent nitrogen doped carbon dots (N-CDs) using Actinidia deliciosa (A. deliciosa) fruit extract as a carbon precursor and aqueous ammonia as a nitrogen dopant is reported here. The synthesized N-CDs were characterized by high resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), UV-Visible spectroscopy (UV-Vis), fluorescence spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The average size of the N-CDs was approximately 3.59 nm and the calculated inter layer distance was found to be 0.21 nm. Raman spectroscopy and SAED pattern revealed the graphitic nature of the synthesized N-CDs. The N-CDs were found to emit intense blue color at 405 nm under the excitation of 315 nm. The doping of nitrogen over the surface of the N-CDs was confirmed by EDS, FT-IR and XPS studies. The synthesized N-CDs were found to exhibit excellent catalytic activity in the reduction of Rhodamine-B using sodium borohydrate. The MTT assay was used to evaluate the cytotoxicity and biocompatibility of N-CDs towards L-929 and MCF-7 cells. From the results obtained, it was found that the N-CDs exhibit low cytotoxicity and superior biocompatibility on both L-929 and MCF-7 cells.

Structural and spectroscopic study of mechanically synthesized SnO2 nanostructures

NASA Astrophysics Data System (ADS)

Vij, Ankush; Kumar, Ravi

2016-05-01

We report the single step synthesis of SnO2 nanostructures using high energy mechanical attrition method. X-ray diffraction (XRD) pattern reveals the single phase rutile structure with appreciable broadening of diffraction peaks, which is a signature of nanostructure formation. The average crystallite size of SnO2 nanostructures has been calculated to be ~15 nm. The micro-Raman study reveals the shifting of A1g Raman mode towards lower wave number, which is correlated with the nanostructure formation.

Effect of PbO on optical properties of tellurite glass

NASA Astrophysics Data System (ADS)

Elazoumi, S. H.; Sidek, H. A. A.; Rammah, Y. S.; El-Mallawany, R.; Halimah, M. K.; Matori, K. A.; Zaid, M. H. M.

2018-03-01

Binary (1 - x)(TeO2) - x(PbO), x = 0, 0.10, 0.15, 0.20, 0.25, 0.30 mol% glass system was fabricated using melt quenching method. X-ray diffraction (XRD) technique was employed to confirm the amorphous nature. The microanalysis of the major components was performed using energy dispersive EDX and X-ray spectrometry. Both the molar volume and the density were measured. FTIR and UV spectra were recorded at 400-4000 cm-1 and 220-800 nm, respectively. The optical band gap (Eopt), Urbach's energy (Eu), index of refraction (n) were calculated using absorption spectrum fitting (ASF) and derivation of absorption spectrum fitting (DASF) methods. Molar refraction Rm and molecular polarizability αm have been calculated according to (ASF) method.

Investigations on surface chemical analysis using X-ray photoelectron spectroscopy and optical properties of Dy3+-doped LiNa3P2O7 phosphor

NASA Astrophysics Data System (ADS)

Munirathnam, K.; Dillip, G. R.; Chaurasia, Shivanand; Joo, S. W.; Deva Prasad Raju, B.; John Sushma, N.

2016-08-01

Near white-light emitting LiNa3P2O7:Dy3+ phosphors were prepared by a conventional solid-state reaction method. The orthorhombic crystal structure of the phosphors was confirmed using X-ray diffraction (XRD), and the valence states of the surface elements were determined from the binding energies of Li 1s, O 1s, Na 1s, P 2p, and Dy 3d by X-ray photoelectron spectroscopy (XPS). Attenuated total reflectance (ATR) - Fourier transform infrared (FT-IR) spectroscopy was employed to identify the pyrophosphate groups in the phosphors. Diffuse reflectance spectra (DRS) show the absorption bands of the Dy3+ ions in the host material. Intense blue (481 nm) and yellow (575 nm) emissions were obtained at an excitation wavelength of 351 nm and are attributed to the 4F9/2 → 6H15/2 and 4F9/2 → 6H13/2 transitions of Dy3+ ions, respectively. The combination of these two intense bands generates light emission in the near-white region of the chromaticity diagram.

Dynamical scattering in coherent hard x-ray nanobeam Bragg diffraction

NASA Astrophysics Data System (ADS)

Pateras, A.; Park, J.; Ahn, Y.; Tilka, J. A.; Holt, M. V.; Kim, H.; Mawst, L. J.; Evans, P. G.

2018-06-01

Unique intensity features arising from dynamical diffraction arise in coherent x-ray nanobeam diffraction patterns of crystals having thicknesses larger than the x-ray extinction depth or exhibiting combinations of nanoscale and mesoscale features. We demonstrate that dynamical scattering effects can be accurately predicted using an optical model combined with the Darwin theory of dynamical x-ray diffraction. The model includes the highly divergent coherent x-ray nanobeams produced by Fresnel zone plate focusing optics and accounts for primary extinction, multiple scattering, and absorption. The simulation accurately reproduces the dynamical scattering features of experimental diffraction patterns acquired from a GaAs/AlGaAs epitaxial heterostructure on a GaAs (001) substrate.

Focal Spot and Wavefront Sensing of an X-Ray Free Electron laser using Ronchi shearing interferometry

DOE PAGES

Nagler, Bob; Aquila, Andrew; Boutet, Sebastien; ...

2017-10-20

The Linac Coherent Light Source (LCLS) is an X-ray source of unmatched brilliance, that is advancing many scientific fields at a rapid pace. The highest peak intensities that are routinely produced at LCLS take place at the Coherent X-ray Imaging (CXI) instrument, which can produce spotsize at the order of 100 nm, and such spotsizes and intensities are crucial for experiments ranging from coherent diffractive imaging, non-linear x-ray optics and high field physics, and single molecule imaging. Nevertheless, a full characterisation of this beam has up to now not been performed. In this paper we for the first time characterisemore » this nanofocused beam in both phase and intensity using a Ronchi Shearing Interferometric technique. The method is fast, in-situ, uses a straightforward optimization algoritm, and is insensitive to spatial jitter.« less

Synthesis of gold nanochains via photoactivation technique and their catalytic applications.

PubMed

Sinha, Arun Kumar; Basu, Mrinmoyee; Sarkar, Sougata; Pradhan, Mukul; Pal, Tarasankar

2013-05-15

The article reports a simple photoactivation technique for the synthesis of chain like assembly of spherical Au nanocrystals using a nontoxic biochemical, β-cyclodextrin under ~365 nm UV-light irradiation. Under UV irradiation, β-cyclodextrin acts as a reducing as well as capping agent and eventually becomes a stabilizing linker for Au nanoparticles. The UV-visible spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), X-ray diffraction (XRD), and X-ray photoelectron spectroscopic techniques are employed to systematically characterize the Au nanochains. Additionally, it is shown that the Au nanocrystals act as an effective catalyst for the reduction in nitrobenzene to aniline and methylene blue to leuco methylene blue in presence of suitable reducing agent. The catalytic reduction reactions and kinetic parameters are evaluated from UV-visible spectroscopy. Copyright © 2013 Elsevier Inc. All rights reserved.

A chemical reduction approach to the synthesis of copper nanoparticles

NASA Astrophysics Data System (ADS)

Khan, Ayesha; Rashid, Audil; Younas, Rafia; Chong, Ren

2016-11-01

Development of improved methods for the synthesis of copper nanoparticles is of high priority for the advancement of material science and technology. Herein, starch-protected zero-valent copper (Cu) nanoparticles have been successfully synthesized by a novel facile route. The method is based on the chemical reduction in aqueous copper salt using ascorbic acid as reducing agent at low temperature (80 °C). X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray spectroscopy measurements were taken to investigate the size, structure and composition of synthesized Cu nanocrystals, respectively. Average crystallite size of Cu nanocrystals calculated from the major diffraction peaks using the Scherrer formula is about 28.73 nm. It is expected that the outcomes of the study take us a step closer toward designing rational strategies for the synthesis of nascent Cu nanoparticles without inert gas protection.

Synthesis of ZnO nanoparticles by a green process and the investigation of their physical properties

NASA Astrophysics Data System (ADS)

Nethavhanani, T.; Diallo, A.; Madjoe, R.; Kotsedi, L.; Maaza, M.

2018-05-01

This contribution reports on the synthesis and the physical properties of ZnO nanoparticles prepared using a green chemistry process. Aspalathus Linearis's extract was used as an effective chelating agent. The whole reaction process for the ZnO nanoparticle was conducted at room temperature. The microstructural properties of ZnO was investigated using X-ray diffraction, furthermore Electron Dispersive X-rays Spectroscopy was employed as quantitative elemental analysis. From the Transmission Electron Microscopy results, the ZnO nanoparticles were found to be highly crystalline with an average diameter of 23.7 nm.

DynAMITe: a prototype large area CMOS APS for breast cancer diagnosis using x-ray diffraction measurements

NASA Astrophysics Data System (ADS)

Konstantinidis, A.; Anaxagoras, T.; Esposito, M.; Allinson, N.; Speller, R.

2012-03-01

X-ray diffraction studies are used to identify specific materials. Several laboratory-based x-ray diffraction studies were made for breast cancer diagnosis. Ideally a large area, low noise, linear and wide dynamic range digital x-ray detector is required to perform x-ray diffraction measurements. Recently, digital detectors based on Complementary Metal-Oxide- Semiconductor (CMOS) Active Pixel Sensor (APS) technology have been used in x-ray diffraction studies. Two APS detectors, namely Vanilla and Large Area Sensor (LAS), were developed by the Multidimensional Integrated Intelligent Imaging (MI-3) consortium to cover a range of scientific applications including x-ray diffraction. The MI-3 Plus consortium developed a novel large area APS, named as Dynamically Adjustable Medical Imaging Technology (DynAMITe), to combine the key characteristics of Vanilla and LAS with a number of extra features. The active area (12.8 × 13.1 cm2) of DynaMITe offers the ability of angle dispersive x-ray diffraction (ADXRD). The current study demonstrates the feasibility of using DynaMITe for breast cancer diagnosis by identifying six breast-equivalent plastics. Further work will be done to optimize the system in order to perform ADXRD for identification of suspicious areas of breast tissue following a conventional mammogram taken with the same sensor.

In Situ Ramp Anneal X-ray Diffraction Study of Atomic Layer Deposited Ultrathin TaN and Ta 1-x Al x N y Films for Cu Diffusion Barrier Applications

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

Consiglio, S.; Dey, S.; Yu, K.

2016-01-01

Ultrathin TaN and Ta 1-xAl xN y films with x = 0.21 to 0.88 were deposited by atomic layer deposition (ALD) and evaluated for Cu diffusion barrier effectiveness compared to physical vapor deposition (PVD) grown TaN. Cu diffusion barrier effectiveness was investigated using in-situ ramp anneal synchrotron X-ray diffraction (XRD) on Cu/1.8 nm barrier/Si stacks. A Kissinger-like analysis was used to assess the kinetics of Cu 3Si formation and determine the effective activation energy (E a) for Cu silicidation. Compared to the stack with a PVD TaN barrier, the stacks with the ALD films exhibited a higher crystallization temperature (Tmore » c) for Cu silicidation. The Ea values of Cu 3Si formation for stacks with the ALD films were close to the reported value for grain boundary diffusion of Cu whereas the Ea of Cu 3Si formation for the stack with PVD TaN is closer to the reported value for lattice diffusion. For 3 nm films, grazing incidence in-plane XRD showed evidence of nanocrystallites in an amorphous matrix with broad peaks corresponding to high density cubic phase for the ALD grown films and lower density hexagonal phase for the PVD grown film further elucidating the difference in initial failure mechanisms due to differences in barrier crystallinity and associated phase.« less

Resolution enhancement in coherent x-ray diffraction imaging by overcoming instrumental noise.

PubMed

Kim, Chan; Kim, Yoonhee; Song, Changyong; Kim, Sang Soo; Kim, Sunam; Kang, Hyon Chol; Hwu, Yeukuang; Tsuei, Ku-Ding; Liang, Keng San; Noh, Do Young

2014-11-17

We report that reference objects, strong scatterers neighboring weak phase objects, enhance the phase retrieval and spatial resolution in coherent x-ray diffraction imaging (CDI). A CDI experiment with Au nano-particles exhibited that the reference objects amplified the signal-to-noise ratio in the diffraction intensity at large diffraction angles, which significantly enhanced the image resolution. The interference between the diffracted x-ray from reference objects and a specimen also improved the retrieval of the phase of the diffraction signal. The enhancement was applied to image NiO nano-particles and a mitochondrion and confirmed in a simulation with a bacteria phantom. We expect that the proposed method will be of great help in imaging weakly scattering soft matters using coherent x-ray sources including x-ray free electron lasers.

Substrate impact on the low-temperature growth of GaN thin films by plasma-assisted atomic layer deposition

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

Kizir, Seda; Haider, Ali; Biyikli, Necmi, E-mail: biyikli@unam.bilkent.edu.tr

2016-07-15

Gallium nitride (GaN) thin films were grown on Si (100), Si (111), and c-plane sapphire substrates at 200 °C via hollow-cathode plasma-assisted atomic layer deposition (HCPA-ALD) using GaEt{sub 3} and N{sub 2}/H{sub 2} plasma as group-III and V precursors, respectively. The main aim of the study was to investigate the impact of substrate on the material properties of low-temperature ALD-grown GaN layers. Structural, chemical, and optical characterizations were carried out in order to evaluate and compare film quality of GaN on different substrates. X-ray reflectivity measurements showed film density values of 5.70, 5.74, and 5.54 g/cm{sup 3} for GaN grown on Simore » (100), Si (111), and sapphire, respectively. Grazing incidence x-ray diffraction measurements exhibited hexagonal wurtzite structure in all HCPA-ALD grown GaN samples. However, dominant diffraction peak for GaN films grown on Si and sapphire substrates were detected differently as (002) and (103), respectively. X-ray diffraction gonio scans measured from GaN grown on c-plane sapphire primarily showed (002) orientation. All samples exhibited similar refractive index values (∼2.17 at 632 nm) with 2–3 at. % of oxygen impurity existing within the bulk of the films. The grain size was calculated as ∼9–10 nm for GaN grown on Si (100) and Si (111) samples while it was ∼5 nm for GaN/sapphire sample. Root-mean-square surface roughness values found as 0.68, 0.76, and 1.83 nm for GaN deposited on Si (100), Si (111), and sapphire, respectively. Another significant difference observed between the samples was the film growth per cycle: GaN/sapphire sample showed a considerable higher thickness value when compared with GaN/Si samples, which might be attributed to a possibly more-efficient nitridation and faster nucleation of sapphire surface.« less

Synthesis of gold and silver nanoparticles using leaf extract of Perilla frutescens--a biogenic approach.

PubMed

Basavegowda, Nagaraj; Lee, Yong Rok

2014-06-01

The present investigation demonstrates a rapid biogenic approach for the synthesis of gold and silver nanoparticles using biologically active and medicinal important Perilla frutescens leaf extract as a reducing and stabilizing agent under ambient conditions. Gold and silver nanoparticles were first synthesized from Perilla frutescens leaf extract which was used as a vegetable and in traditional medicines for a long time in Korea, Japan, and China. The nanoparticles obtained were characterized by UV-vis spectroscopy, transmission electron microscopy, X-ray diffraction, and Fourier transform infrared spectroscopy. Surface plasmon resonance spectra of gold and silver nanoparticles were obtained at 540 and 430 nm and triangular and spherical shape respectively. TEM studies showed that the particle sizes of gold and silver nanoparticles ranges -50 nm and -40 nm respectively. X-ray diffraction studies confirm that the biosynthesized nanoparticles were crystalline gold and silver. Fourier transform infra-red spectroscopy revealed that biomolecules were involved in the synthesis and capping of the nanoparticles produced. XRD and EDX confirmed the formation of gold and silver nanoparticles. This is a simple, efficient and rapid method to synthesize gold and silver nanoparticles at room temperature without use of toxic chemicals. Obtained gold and silver nanoparticles can be used in various biomedical and biotechnological applications.

ZnS, CdS and HgS nanoparticles via alkyl-phenyl dithiocarbamate complexes as single source precursors.

PubMed

Onwudiwe, Damian C; Ajibade, Peter A

2011-01-01

The synthesis of II-VI semiconductor nanoparticles obtained by the thermolysis of certain group 12 metal complexes as precursors is reported. Thermogravimetric analysis of the single source precursors showed sharp decomposition leading to their respective metal sulfides. The structural and optical properties of the prepared nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) UV-Vis and photoluminescence spectroscopy. The X-ray diffraction pattern showed that the prepared ZnS nanoparticles have a cubic sphalerite structure; the CdS indicates a hexagonal phase and the HgS show the presence of metacinnabar phase. The TEM image demonstrates that the ZnS nanoparticles are dot-shaped, the CdS and the HgS clearly showed a rice and spherical morphology respectively. The UV-Vis spectra exhibited a blue-shift with respect to that of the bulk samples which is attributed to the quantum size effect. The band gap of the samples have been calculated from absorption spectra and werefound to be about 4.33 eV (286 nm), 2.91 eV (426 nm) and 4.27 eV (290 nm) for the ZnS, CdS and HgS samples respectively.

ZnS, CdS and HgS Nanoparticles via Alkyl-Phenyl Dithiocarbamate Complexes as Single Source Precursors

PubMed Central

Onwudiwe, Damian C.; Ajibade, Peter A.

2011-01-01

The synthesis of II-VI semiconductor nanoparticles obtained by the thermolysis of certain group 12 metal complexes as precursors is reported. Thermogravimetric analysis of the single source precursors showed sharp decomposition leading to their respective metal sulfides. The structural and optical properties of the prepared nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) UV-Vis and photoluminescence spectroscopy. The X-ray diffraction pattern showed that the prepared ZnS nanoparticles have a cubic sphalerite structure; the CdS indicates a hexagonal phase and the HgS show the presence of metacinnabar phase. The TEM image demonstrates that the ZnS nanoparticles are dot-shaped, the CdS and the HgS clearly showed a rice and spherical morphology respectively. The UV-Vis spectra exhibited a blue-shift with respect to that of the bulk samples which is attributed to the quantum size effect. The band gap of the samples have been calculated from absorption spectra and werefound to be about 4.33 eV (286 nm), 2.91 eV (426 nm) and 4.27 eV (290 nm) for the ZnS, CdS and HgS samples respectively. PMID:22016607

Effects of high temperature and film thicknesses on the texture evolution in Ag thin films

NASA Astrophysics Data System (ADS)

Eshaghi, F.; Zolanvari, A.

2017-04-01

In situ high-temperature X-ray diffraction techniques were used to study the effect of high temperatures (up to 600°C) on the texture evolution in silver thin films. Ag thin films with different thicknesses of 40, 80, 120 and 160nm were sputtered on the Si(100) substrates at room temperature. Then, microstructure of thin films was determined using X-ray diffraction. To investigate the influence of temperature on the texture development in the Ag thin films with different thicknesses, (111), (200) and (220) pole figures were evaluated and orientation distribution functions were calculated. Minimizing the total energy of the system which is affected by competition between surface and elastic strain energy was a key factor in the as-deposited and post annealed thin films. Since sputtering depositions was performed at room temperature and at the same thermodynamic conditions, the competition growth caused the formation of the {122} < uvw \\rangle weak fiber texture in as-deposited Ag thin films. It was significantly observed that the post annealed Ag thin films showed {111} < uvw \\rangle orientations as their preferred orientations, but their preferred fiber texture varied with the thickness of thin films. Increasing thin film thickness from 40nm to 160nm led to decreasing the intensity of the {111} < uvw \\rangle fiber texture.

Effect of film thickness on structural and mechanical properties of AlCrN nanocompoite thin films deposited by reactive DC magnetron sputtering

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

Prakash, Ravi; Kaur, Davinder, E-mail: dkaurfph@iitr.ac.in

2016-05-06

In this study, the influence of film thickness on the structural, surface morphology and mechanical properties of Aluminum chromium nitride (AlCrN) thin films has been successfully investigated. The AlCrN thin films were deposited on silicon (100) substrate using dc magnetron reactive co-sputtering at substrate temperature 400° C. The structural, surface morphology and mechanical properties were studied using X-ray diffraction, field-emission scanning electron microscopy and nanoindentation techniques respectively. The thickness of these thin films was controlled by varying the deposition time therefore increase in deposition time led to increase in film thickness. X-ray diffraction pattern of AlCrN thin films with differentmore » deposition time shows the presence of (100) and (200) orientations. The crystallite size varies in the range from 12.5 nm to 36.3 nm with the film thickness due to surface energy minimization with the higher film thickness. The hardness pattern of these AlCrN thin films follows Hall-Petch relation. The highest hardness 23.08 Gpa and young modulus 215.31 Gpa were achieved at lowest grain size of 12.5 nm.« less

Low-temperature synthesis of homogeneous solid solutions of scheelite-structured Ca 1-xSr xWO 4 and Sr 1-xBa xWO 4 nanocrystals

DOE PAGES

Culver, Sean P.; Greaney, Matthew J.; Tinoco, Antonio; ...

2015-07-24

Here, a series of compositionally complex scheelite-structured nanocrystals of the formula A 1-xA’ xWO 4 (A = Ca, Sr, Ba) have been prepared under benign synthesis conditions using the vapor diffusion sol–gel method. Discrete nanocrystals with sub-20 nm mean diameters were obtained after kinetically controlled hydro- lysis and polycondensation at room temperature, followed by composition-dependent thermal aging at or below 60 °C. Rietveld analysis of X-ray diffraction data and Raman spectroscopy verified the synthesis of continuous and phase-pure nanocrystal solid solutions across the entire composition space for A 1-xA’ xWO 4, where 0 ≤ x ≤ 1. Elemental analysis bymore » X-ray photoelectron and inductively coupled plasma- atomic emission spectroscopies demonstrated excellent agreement between the nominal and experi- mentally determined elemental stoichiometries, while energy dispersive X-ray spectroscopy illustrated good spatial elemental homogeneity within these nanocrystals synthesized under benign conditions.« less

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

Gelles, D. S.; Browning, James Frederick; Snow, Clark Sheldon

Er(D,T){sub 2-x} {sup 3}He{sub x}, erbium di-tritide, films of thicknesses 500 nm, 400 nm, 300 nm, 200 nm, and 100 nm were grown and analyzed by Transmission Electron Microscopy, X-Ray Diffraction, and Ion Beam Analysis to determine variations in film microstructure as a function of film thickness and age, due to the time-dependent build-up of {sup 3}He in the film from the radioactive decay of tritium. Several interesting features were observed: One, the amount of helium released as a function of film thickness is relatively constant. This suggests that the helium is being released only from the near surface regionmore » and that the helium is not diffusing to the surface from the bulk of the film. Two, lenticular helium bubbles are observed as a result of the radioactive decay of tritium into {sup 3}He. These bubbles grow along the [111] crystallographic direction. Three, a helium bubble free zone, or 'denuded zone' is observed near the surface. The size of this region is independent of film thickness. Four, an analysis of secondary diffraction spots in the Transmission Electron Microscopy study indicate that small erbium oxide precipitates, 5-10 nm in size, exist throughout the film. Further, all of the films had large erbium oxide inclusions, in many cases these inclusions span the depth of the film.« less

In situ growth of capping-free magnetic iron oxide nanoparticles on liquid-phase exfoliated graphene

NASA Astrophysics Data System (ADS)

Tsoufis, T.; Syrgiannis, Z.; Akhtar, N.; Prato, M.; Katsaros, F.; Sideratou, Z.; Kouloumpis, A.; Gournis, D.; Rudolf, P.

2015-05-01

We report a facile approach for the in situ synthesis of very small iron oxide nanoparticles on the surface of high-quality graphene sheets. Our synthetic strategy involved the direct, liquid-phase exfoliation of highly crystalline graphite (avoiding any oxidation treatment) and the subsequent chemical functionalization of the graphene sheets via the well-established 1,3-dipolar cycloaddition reaction. The resulting graphene derivatives were employed for the immobilization of the nanoparticle precursor (Fe cations) at the introduced organic groups by a modified wet-impregnation method, followed by interaction with acetic acid vapours. The final graphene-iron oxide hybrid material was achieved by heating (calcination) in an inert atmosphere. Characterization by X-ray diffraction, transmission electron and atomic force microscopy, Raman and X-ray photoelectron spectroscopy gave evidence for the formation of rather small (<12 nm), spherical, magnetite-rich nanoparticles which were evenly distributed on the surface of few-layer (<1.2 nm thick) graphene. Due to the presence of the iron oxide nanoparticles, the hybrid material showed a superparamagnetic behaviour at room temperature.We report a facile approach for the in situ synthesis of very small iron oxide nanoparticles on the surface of high-quality graphene sheets. Our synthetic strategy involved the direct, liquid-phase exfoliation of highly crystalline graphite (avoiding any oxidation treatment) and the subsequent chemical functionalization of the graphene sheets via the well-established 1,3-dipolar cycloaddition reaction. The resulting graphene derivatives were employed for the immobilization of the nanoparticle precursor (Fe cations) at the introduced organic groups by a modified wet-impregnation method, followed by interaction with acetic acid vapours. The final graphene-iron oxide hybrid material was achieved by heating (calcination) in an inert atmosphere. Characterization by X-ray diffraction, transmission electron and atomic force microscopy, Raman and X-ray photoelectron spectroscopy gave evidence for the formation of rather small (<12 nm), spherical, magnetite-rich nanoparticles which were evenly distributed on the surface of few-layer (<1.2 nm thick) graphene. Due to the presence of the iron oxide nanoparticles, the hybrid material showed a superparamagnetic behaviour at room temperature. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr00765h

Simple route to (NH4)xWO3 nanorods for near infrared absorption

NASA Astrophysics Data System (ADS)

Guo, Chongshen; Yin, Shu; Dong, Qiang; Sato, Tsugio

2012-05-01

Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows.Described here is how to synthesize one-dimensional ammonium tungsten bronze ((NH4)xWO3) by a facile solvothermal approach in which ethylene glycol and acetic acid were employed as solvents and ammonium paratungstate was used as a starting material, as well as how to develop the near infrared absorption properties of (NH4)xWO3 nanorods for application as a solar light control filter. The as-obtained product was characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetry (TG), atomic force microscope (AFM) and UV-Vis-NIR spectra. The SEM and TEM images clearly revealed that the obtained sample possessed rod/fiber-like morphologies with diameters around 120 nm. As determined by UV-Vis-NIR optical measurement, the thin film consisted of (NH4)xWO3 nanoparticles, which can selectively transmit most visible lights, but strongly absorb the near-infrared (NIR) lights and ultraviolet rays. These interesting optical properties make the (NH4)xWO3 nanorods suitable for the solar control windows. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr30612c

Ag nanodots decorated SiO2 coated ZnO core-shell nanostructure with enhanced luminescence property as potential imaging agent

NASA Astrophysics Data System (ADS)

Gupta, Jagriti; Barick, K. C.; Hassan, P. A.; Bahadur, Dhirendra

2018-04-01

Ag decorated silica coated ZnO nanocomposite (Ag@SiO2@ZnO NCs) has been synthesized by soft chemical approach. The physico-chemical properties of Ag@SiO2@ZnO NCs are investigated by various sophisticated characterization techniques such as X-ray diffraction, Transmission electron microscopy, X-ray photoelectron spectroscopy, UV-visible absorption and photoluminescent spectroscopy. X-ray diffraction confirms the phase formation of ZnO and Ag in nanocomposite. TEM micrograph clearly shows that Ag nanodots are well decorated over silica coated ZnO NCs. The photoluminescent study reveals the enhancement in the photoluminance property when the Ag nanodots are decorated over silica coated ZnO nanocomposite due to an electromagnetic coupling between excitons and plasmons. Furthermore, the photoluminescent property is an important tool for bio-imaging application, reveal that NCs give green and red emission after excitation with 488 and 535 nm. Therefore, low cytotoxicity and excellent fluorescence stability in vitro makes it a more suitable material for both cellular imaging and therapy for biomedical applications.

Synthesis and characterization of Ce, Cu co-doped ZnS nanoparticles

NASA Astrophysics Data System (ADS)

Harish, G. S.; Sreedhara Reddy, P.

2015-09-01

Ce, Cu co-doped ZnS nanoparticles were prepared at room temperature using a chemical co-precipitation method. The prepared nanoparticles were characterized by X- ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive analysis of X-rays (EDAX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) and high resolution Raman spectroscopic techniques. Transmission electron microscopy (TEM) and X-ray diffraction studies showed that the diameter of the particles was around 2-3 nm. Broadened XRD peaks revealed the formation of nanoparticles with a face centered cubic (fcc) structure. DRS studies confirmed that the band gap increased with an increase in the dopant concentration. The Raman spectra of undoped and Ce, Cu ions co-doped ZnS nanoparticles showed longitudinal optical mode and transverse optical mode. Compared with the Raman modes (276 and 351 cm-1) of undoped ZnS nanoparticles, the Raman modes of Ce, Cu co- doped ZnS nanoparticles were slightly shifted towards lower frequency. PL spectra of the samples showed remarkable enhancement in the intensity upon doping.

Impurity precipitation in atomized particles evidenced by nano x-ray diffraction computed tomography

NASA Astrophysics Data System (ADS)

Bonnin, Anne; Wright, Jonathan P.; Tucoulou, Rémi; Palancher, Hervé

2014-08-01

Performances and physical properties of high technology materials are influenced or even determined by their initial microstructure and by the behavior of impurity phases. Characterizing these impurities and their relations with the surrounding matrix is therefore of primary importance but it unfortunately often requires a destructive approach, with the risk of misinterpreting the observations. The improvement we have done in high resolution X-ray diffraction computed tomography combined with the use of an X-ray nanoprobe allows non-destructive crystallographic description of materials with microscopic heterogeneous microstructure (with a grain size between 10 nm and 10 μm). In this study, the grain localization in a 2D slice of a 20 μm solidified atomized γU-Mo particle is shown and a minority U(C,O) phase (1 wt. %) with sub-micrometer sized grains was characterized inside. Evidence is presented showing that the onset of U(C,O) grain crystallization can be described by a precipitation mechanism since one single U-Mo grain has direct orientation relationship with more than one surrounding U(C,O) grains.

Structural, optical and enhanced power filtering application of PEG capped Zn1-xCoxS quantum dots

NASA Astrophysics Data System (ADS)

Vineeshkumar, T. V.; Prasanth, S.; Pragash, R.; Unnikrishnan, N. V.; Sudarsanakumar, C.

2018-04-01

Zn1-xCoxS (x= 0.05, 0.1, 0.15 and 0.2) quantum dots were synthesized successfully using co precipitation technique in polyethylene glycol (PEG) matrix. The PEG acted as a capping agent as well as a reducing agent. The structural and optical properties of the samples were studied by x-ray diffraction (XRD), TEM analysis and UV-Visible absorption. Nonlinear optical properties were measured using open aperture z-scan technique, employing frequency doubled (532 nm) pumping sources.

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

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

Sinsheimer, John; Bouet, Nathalie; Ghose, Sanjit

2016-10-06

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

Local terahertz field enhancement for time-resolved x-ray diffraction

DOE PAGES

Kozina, M.; Pancaldi, M.; Bernhard, C.; ...

2017-02-20

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Local terahertz field enhancement for time-resolved x-ray diffraction

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

Kozina, M.; Pancaldi, M.; Bernhard, C.

We report local field strength enhancement of single-cycle terahertz (THz) pulses in an ultrafast time-resolved x-ray diffraction experiment. We show that patterning the sample with gold microstructures increases the THz field without changing the THz pulse shape or drastically affecting the quality of the x-ray diffraction pattern. Lastly, we find a five-fold increase in THz-induced x-ray diffraction intensity change in the presence of microstructures on a SrTiO 3 thin-film sample.

Structural analysis and martensitic transformation in equiatomic HfPd alloy

NASA Astrophysics Data System (ADS)

Hisada, S.; Matsuda, M.; Takashima, K.; Yamabe-Mitarai, Y.

2018-02-01

We investigated the crystal structure and the martensitic transformation in equiatomic HfPd alloy. The analysis of the crystal structure by electron diffraction and Rietveld refinement using X-ray diffraction data indicates that the space group of the martensitic phase is Cmcm, and the lattice parameters are a = 0.329 nm, b = 1.021 nm, and c = 0.438 nm. Martensitic variants are composed of the plate-like morphology of several hundred nm, and the boundaries between the variants have (021)Cmcm twin relations. This (021)Cmcm twin boundary seems to be sharp without ledge and steps. Differential scanning calorimetry measurement indicates that each martensitic transformation temperature is determined to be Ms = 819 K, Mf = 794 K, As = 928 K, and Af = 954 K. Based on the dimension change using a thermo-mechanical analyzer, the expansion and shrinkage of the sample occurred with the forward and reverse martensitic transformation, respectively.

Thermal x-ray diffraction and near-field phase contrast imaging

NASA Astrophysics Data System (ADS)

Li, Zheng; Classen, Anton; Peng, Tao; Medvedev, Nikita; Wang, Fenglin; Chapman, Henry N.; Shih, Yanhua

2017-10-01

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. In this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Thermal x-ray diffraction and near-field phase contrast imaging

DOE PAGES

Li, Zheng; Classen, Anton; Peng, Tao; ...

2017-12-27

Using higher-order coherence of thermal light sources, the resolution power of standard x-ray imaging techniques can be enhanced. Here in this work, we applied the higher-order measurement to far-field x-ray diffraction and near-field phase contrast imaging (PCI), in order to achieve superresolution in x-ray diffraction and obtain enhanced intensity contrast in PCI. The cost of implementing such schemes is minimal compared to the methods that achieve similar effects by using entangled x-ray photon pairs.

Nanometres-resolution Kikuchi patterns from materials science specimens with transmission electron forward scatter diffraction in the scanning electron microscope.

PubMed

Brodusch, N; Demers, H; Gauvin, R

2013-04-01

A charge-coupled device camera of an electron backscattered diffraction system in a scanning electron microscope was positioned below a thin specimen and transmission Kikuchi patterns were collected. Contrary to electron backscattered diffraction, transmission electron forward scatter diffraction provides phase identification and orientation mapping at the nanoscale. The minimum Pd particle size for which a Kikuchi diffraction pattern was detected and indexed reliably was 5.6 nm. An orientation mapping resolution of 5 nm was measured at 30 kV. The resolution obtained with transmission electron forward scatter diffraction was of the same order of magnitude than that reported in electron nanodiffraction in the transmission electron microscope. An energy dispersive spectrometer X-ray map and a transmission electron forward scatter diffraction orientation map were acquired simultaneously. The high-resolution chemical, phase and orientation maps provided at once information on the chemical form, orientation and coherency of precipitates in an aluminium-lithium 2099 alloy. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

An image focusing means by using an opaque object to diffract x-rays

DOEpatents

Sommargren, Gary E.; Weaver, H. Joseph

1991-01-01

The invention provides a method and apparatus for focusing and imaging x-rays. An opaque sphere is used as a diffractive imaging element to diffract x-rays from an object so that the divergent x-ray wavefronts are transformed into convergent wavefronts and are brought to focus to form an image of the object with a large depth of field.

Porous Ni-Mn oxide nanosheets in situ formed on nickel foam as 3D hierarchical monolith de-NOx catalysts

NASA Astrophysics Data System (ADS)

Cai, Sixiang; Zhang, Dengsong; Shi, Liyi; Xu, Jing; Zhang, Lei; Huang, Lei; Li, Hongrui; Zhang, Jianping

2014-06-01

In this work, we successfully in situ decorated nickel foam with porous Ni-Mn oxide nanosheets (3DH-NM/NF) as 3D hierarchical monolith de-NOx catalysts via a simple hydrothermal reaction and calcination process. The catalysts were carefully examined by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, elemental mapping, X-ray photoelectron spectroscopy, H2 temperature-programmed reduction and NH3 temperature-programmed desorption measurements. The results indicated that the nanosheets are composed of a Ni6Mn1O8 spinel and the metal species are uniformly dispersed in bi-metal oxides. As a result, the strong synergistic effects between the Mn and Ni species have been observed. The active oxygen species, reducible species and acidity are enhanced by the in situ formation of the nanosheets on the surface of nickel foam. These desirable features of 3DH-NM/NF catalysts bring about the excellent de-NOx performance. Moreover, the 3DH-NM/NF catalysts also present good stability and H2O resistance. Based on these favorable properties, 3DH-NM/NF could be considered as a promising candidate for the monolith de-NOx catalysts.In this work, we successfully in situ decorated nickel foam with porous Ni-Mn oxide nanosheets (3DH-NM/NF) as 3D hierarchical monolith de-NOx catalysts via a simple hydrothermal reaction and calcination process. The catalysts were carefully examined by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, elemental mapping, X-ray photoelectron spectroscopy, H2 temperature-programmed reduction and NH3 temperature-programmed desorption measurements. The results indicated that the nanosheets are composed of a Ni6Mn1O8 spinel and the metal species are uniformly dispersed in bi-metal oxides. As a result, the strong synergistic effects between the Mn and Ni species have been observed. The active oxygen species, reducible species and acidity are enhanced by the in situ formation of the nanosheets on the surface of nickel foam. These desirable features of 3DH-NM/NF catalysts bring about the excellent de-NOx performance. Moreover, the 3DH-NM/NF catalysts also present good stability and H2O resistance. Based on these favorable properties, 3DH-NM/NF could be considered as a promising candidate for the monolith de-NOx catalysts. Electronic supplementary information (ESI) available: Experimental details and catalytic performance of the NM/cordierite catalysts, SEM image and EDX analysis of the NF and 3DH-N/NF catalysts, N2 selectivity and catalytic performance under different gas hourly space velocities of the 3DH-NM/NF catalysts. See DOI: 10.1039/c4nr00475b

Green synthesis of gold nanoparticles using Citrus fruits (Citrus limon, Citrus reticulata and Citrus sinensis) aqueous extract and its characterization.

PubMed

Sujitha, Mohanan V; Kannan, Soundarapandian

2013-02-01

This study reports the biological synthesis of gold nanoparticles by the reduction of HAuCl(4) by using citrus fruits (Citrus limon, Citrus reticulata and Citrus sinensis) juice extract as the reducing and stabilizing agent. A various shape and size of gold nanoparticles were formed when the ratio of the reactants were altered with respect to 1.0mM chloroauric acid solution. The gold nanoparticles obtained were characterized by UV-visible spectra, transmission electron microscopy (TEM) and X-ray diffraction (XRD). TEM studies showed the particles to be of various shapes and sizes and particle size ranges from 15 to 80 nm. Selected-area electron diffraction (SAED) pattern confirmed fcc phase and crystallinity of the particles. The X-ray diffraction analysis revealed the distinctive facets (111, 200, 220 and 222 planes) of gold nanoparticles. Dynamic light scattering (DLS) studies revealed that the average size for colloid gp(3) of C. limon, C. reticulata and C. sinensis are 32.2 nm, 43.4 nm and 56.7 nm respectively. The DLS graph showed that the particles size was larger and more polydispersed compared to the one observed by TEM due to the fact that the measured size also includes the bio-organic compounds enveloping the core of the Au NPs. Zeta potential value for gold nanoparticles obtained from colloid gp(3) of C. limon, C. reticulata and C. sinensis are -45.9, -37.9 and -31.4 respectively indicating the stability of the synthesized nanoparticles. Herein we propose a novel, previously unexploited method for the biological syntheses of polymorphic gold nanoparticles with potent biological applications. Copyright © 2012 Elsevier B.V. All rights reserved.

Size dependence of magnetorheological properties of cobalt ferrite ferrofluid

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

Radhika, B.; Sahoo, Rasmita; Srinath, S., E-mail: srinath@uohyd.ac.in

2015-06-24

Cobalt Ferrite nanoparticles were synthesized using co-precipitation method at reaction temperatures of 40°C and 80°C. X-Ray diffraction studies confirm cubic phase formation. The average crystallite sizes were found to be ∼30nm and ∼48nm for 40°C sample and 80°C sample respectively. Magnetic properties measured using vibrating sample magnetometer show higher coercivety and magnetization for sample prepared at 80°C. Magnetorheological properties of CoFe2O4 ferrofluids were measured and studied.

Nanometer-scale ablation using focused, coherent extreme ultraviolet/soft x-ray light

DOEpatents

Menoni, Carmen S [Fort Collins, CO; Rocca, Jorge J [Fort Collins, CO; Vaschenko, Georgiy [San Diego, CA; Bloom, Scott [Encinitas, CA; Anderson, Erik H [El Cerrito, CA; Chao, Weilun [El Cerrito, CA; Hemberg, Oscar [Stockholm, SE

2011-04-26

Ablation of holes having diameters as small as 82 nm and having clean walls was obtained in a poly(methyl methacrylate) on a silicon substrate by focusing pulses from a Ne-like Ar, 46.9 nm wavelength, capillary-discharge laser using a freestanding Fresnel zone plate diffracting into third order is described. Spectroscopic analysis of light from the ablation has also been performed. These results demonstrate the use of focused coherent EUV/SXR light for the direct nanoscale patterning of materials.

Imaging single cells in a beam of live cyanobacteria with an X-ray laser (CXIDB ID 27)

DOE Data Explorer

Schot, Gijs, vander

2015-02-10

Diffraction pattern of a micron-sized S. elongatus cell at 1,100 eV photon energy (1.13 nm wavelength) with ~10^11 photons per square micron on the sample in ~70 fs. The signal to noise ratio at 4 nm resolution is 3.7 with 0.24 photons per Nyquist pixel. The cell was alive at the time of the exposure. The central region of the pattern (dark red) is saturated and this prevented reliable image reconstruction.

New frontiers in water purification: highly stable amphopolycarboxyglycinate-stabilized Ag-AgCl nanocomposite and its newly discovered potential

NASA Astrophysics Data System (ADS)

Krutyakov, Yurii A.; Zherebin, Pavel M.; Kudrinskiy, Alexey A.; Zubavichus, Yan V.; Presniakov, Mikhail Yu; Yapryntsev, Alexey D.; Karabtseva, Anastasia V.; Mikhaylov, Dmitry M.; Lisichkin, Georgii V.

2016-09-01

A simple synthetic procedure for high-stable dispersions of porous composite Ag/AgCl nanoparticles stabilized with amphoteric surfactant sodium tallow amphopolycarboxyglycinate has been proposed for the first time. The prepared samples were characterized by UV-vis spectroscopy, x-ray powder diffraction (XRD), x-ray photoelectron spectroscopy, small area electron diffraction (SAED), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and electron probe micro-analysis. In addition, measurements (carried out at the Kurchatov synchrotron radiation source stations) of the Ag K-edge extended x-ray absorption fine structure (EXAFS) and x-ray absorption near edge structure (XANES) spectra and XRD of the prepared nanoparticles have been performed. The obtained results suggest that small-sized Ag clusters are homogeneously distributed in the mass of the AgCl nanoparticle (~80 nm) formed during the synthesis. The Ag/AgCl dispersion demonstrates photocatalytic activity (with respect to methyl orange) and high bactericidal activity against E. coli. This activity is superior to the activity of both Ag and AgCl nanoparticles stabilized by the same surfactant. Thus, porous composite Ag/AgCl nanoparticles can be used as a multifunctional agent that is able to remove both pollutants and bacterium from water.

53 W average power few-cycle fiber laser system generating soft x rays up to the water window.

PubMed

Rothhardt, Jan; Hädrich, Steffen; Klenke, Arno; Demmler, Stefan; Hoffmann, Armin; Gotschall, Thomas; Eidam, Tino; Krebs, Manuel; Limpert, Jens; Tünnermann, Andreas

2014-09-01

We report on a few-cycle laser system delivering sub-8-fs pulses with 353 μJ pulse energy and 25 GW of peak power at up to 150 kHz repetition rate. The corresponding average output power is as high as 53 W, which represents the highest average power obtained from any few-cycle laser architecture so far. The combination of both high average and high peak power provides unique opportunities for applications. We demonstrate high harmonic generation up to the water window and record-high photon flux in the soft x-ray spectral region. This tabletop source of high-photon flux soft x rays will, for example, enable coherent diffractive imaging with sub-10-nm resolution in the near future.

Thermoluminescence (TL) properties and x-ray diffraction (XRD) analysis of high purity CaSO4:Dy TL material

NASA Astrophysics Data System (ADS)

Kamarudin, Nadira; Abdullah, Wan Saffiey Wan; Hamid, Muhammad Azmi Abdul; Dollah, Mohd Taufik

2014-09-01

This paper presents the characterization and TL properties of dysprosium (Dy) doped calcium sulfate (CaSO4) TL material produced by co-precipitation technique with 0.5mol% concentration of dopant. The morphology of the produced TL material was studied using scanning electron microscope (SEM) and the micrograph shows that rectangular parallelepiped shaped crystal with the average of 150 μm in length were produced. The crystallinity of the produced powder was studied using x-ray powder diffraction (XRD). The XRD spectra show that the TL material produced is high purity anhydrite CaSO4 with average crystallite size of 74 nm with orthorhombic crystal system. The TL behavior of produced CaSO4:Dy was studied using a TLD reader after exposure to gamma ray by Co60 source with the doses of 1,5 and 10 Gy. The glow curve shows linear response with glow peak around 230°C which is desired development in the field of radiation dosimetry.

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

NASA Astrophysics Data System (ADS)

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

2013-03-01

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

Rietveld analysis using powder diffraction data with anomalous scattering effect obtained by focused beam flat sample method

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

Tanaka, Masahiko, E-mail: masahiko@spring8.or.jp; Katsuya, Yoshio, E-mail: katsuya@spring8.or.jp; Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp

2016-07-27

Focused-beam flat-sample method (FFM) is a new trial for synchrotron powder diffraction method, which is a combination of beam focusing optics, flat shape powder sample and area detectors. The method has advantages for X-ray diffraction experiments applying anomalous scattering effect (anomalous diffraction), because of 1. Absorption correction without approximation, 2. High intensity X-rays of focused incident beams and high signal noise ratio of diffracted X-rays 3. Rapid data collection with area detectors. We applied the FFM to anomalous diffraction experiments and collected synchrotron X-ray powder diffraction data of CoFe{sub 2}O{sub 4} (inverse spinel structure) using X-rays near Fe K absorptionmore » edge, which can distinguish Co and Fe by anomalous scattering effect. We conducted Rietveld analyses with the obtained powder diffraction data and successfully determined the distribution of Co and Fe ions in CoFe{sub 2}O{sub 4} crystal structure.« less

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

NASA Astrophysics Data System (ADS)

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

2016-09-01

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

Irradiation induced formation of VN in CrN thin films

NASA Astrophysics Data System (ADS)

Novaković, M.; Popović, M.; Zhang, K.; Mitrić, M.; Bibić, N.

2015-09-01

Reactively sputtered CrN layer, deposited on Si(1 0 0) wafer, was implanted at room temperature with 80-keV V+ ions to the fluence of 2 × 1017 ions/cm2. After implantation the sample was annealed in a vacuum, for 2 h at 700 °C. The microstructure and chemical composition of CrN films was investigated using Rutherford backscattering spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction and cross-sectional transmission electron microscopy (conventional and high-resolution), together with fast Fourier transformation analyses. It was found that vanadium atoms are distributed in the sub-surface region of CrN layer, with the maximum concentration at ∼20 nm. After annealing the formation of VN nanoparticles was observed. The nanoparticles are spherical shaped with a size of 8-20 nm in diameter.

[Characterization of microstructure of ibuprofen-hydroxypropyl-beta-cyclodextrin and ibuprofen-beta-cyclodextrin by atomic force microscope].

PubMed

Wang, Li-juan; Zhu, Zhao-jing; Che, Ke-ke; Ju, Feng-ge

2008-09-01

The microstructures of ibuprofen-hydroxypropyl-bets-cyclodextrin (IBU-HP-beta-CyD) and ibuprofen-beta-cyclodextrin (IBU-beta-CyD) were observed by atomic force microscope (AFM). The high resolving capability of AFM has the tungsten filament probe with the spring constant of 0.06 N x m(-1). Samples were observed in a small scale scanning area of 10.5 nm x 10.5 nm and 800 x 800 pixels. The original scanning images were gained by tapping mode at room temperature. Their three-dimensional reconstruction of microstructure was performed by G3DR software. The outer diameters of HP-beta-CyD and beta-CyD are 1.53 nm. The benzene diameter of IBU is 0.62 nm, fitting to the inner diameters of HP-beta-CyD and beta-CyD. The benzene and hydrophobic chain of IBU enter into the hole of cyclodextrin at 1:1 ratio. The results were evidenced by IR, X-ray diffraction and the phase solubility.

Electrical, structural and optical properties of tellurium thin films on silicon substrate

NASA Astrophysics Data System (ADS)

Arora, Swati; Vijay, Y. K.

2018-05-01

Tellurium (Te) thin films of various thicknesses (200nm, 275nm, 350nm & 500nm) were prepared on Silicon (Si) using thermal evaporation at vacuum of 10-5 torr. It is observed that the resistivity decreases exponentially with the Increases Temperature. A direct band gap between 0.368 eV to 0.395 eV is obtained at different temperatures with Four Probe Method which shows that when we increase the thickness of material the band gap will exponentially decreases. Samples were analysed through X-ray diffraction and atomic force microscopy to attain complete and reliable micro structural in order.

A general route for the rapid synthesis of one-dimensional nanostructured single-crystal Te, Se and Se Te alloys directly from Te or/and Se powders

NASA Astrophysics Data System (ADS)

Zhou, Bo; Zhu, Jun-Jie

2006-03-01

A general and template-free 'disproportionation and reversal' route was developed to synthesize one-dimensional (1D) nanostructures of Te, Se and Se-Te alloys directly from Te or/and Se powders. The products were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and scanning electron microscopy (SEM). Te nanorods and nanowires with a width varying from about 40 nm to about 300 nm, Se nanowires with a width of 60-100 nm and a length of 4-6 µm, and SexTe100-x alloy nanorods with x in a wide range, and with a width of 30-70 nm and an aspect ratio of three to five, were prepared. The mechanism of formation of the nanorods and nanowires and the effects of the experimental conditions, such as solution concentration, cooling rate, solvent nature and heating process, on the morphology and size of the products have been discussed. We believe that this general route and some other proper reversible processes between solid state and solution state can be extended to the transformations from various bulk materials into nanosized materials with various morphologies.

Preparation and structural characterization of vulcanized natural rubber nanocomposites containing nickel-zinc ferrite nanopowders.

PubMed

Bellucci, F S; Salmazo, L O; Budemberg, E R; da Silva, M R; Rodríguez-Pérez, M A; Nobre, M A L; Job, A E

2012-03-01

Single-phase polycrystalline mixed nickel-zinc ferrites belonging to Ni0.5Zn0.5Fe2O4 were prepared on a nanometric scale (mean crystallite size equal to 14.7 nm) by chemical synthesis named the modified poliol method. Ferrite nanopowder was then incorporated into a natural rubber matrix producing nanocomposites. The samples were investigated by means of infrared spectroscopy, X-ray diffraction, scanning electron microscopy and magnetic measurements. The obtained results suggest that the base concentration of nickel-zinc ferrite nanoparticles inside the polymer matrix volume greatly influences the magnetic properties of nanocomposites. A small quantity of nanoparticles, less than 10 phr, in the nanocomposite is sufficient to produce a small alteration in the semi-crystallinity of nanocomposites observed by X-ray diffraction analysis and it produces a flexible magnetic composite material with a saturation magnetization, a coercivity field and an initial magnetic permeability equal to 3.08 emu/g, 99.22 Oe and 9.42 x 10(-5) respectively.

Rapid crystallization of WS2 films assisted by a thin nickel layer: An in situ energy-dispersive X-ray diffraction study

NASA Astrophysics Data System (ADS)

Ellmer, K.; Seeger, S.; Mientus, R.

2006-08-01

By rapid thermal crystallization of an amorphous WS3+x film, deposited by reactive magnetron sputtering at temperatures below 150 °C, layer-type semiconducting tungsten disulfide films (WS2) were grown. The rapid crystallization was monitored in real-time by in situ energy-dispersive X-ray diffraction. The films crystallize very fast (>40 nm/s), provided that a thin nickel film acts as nucleation seeds. Experiments on different substrates and the onset of the crystallization only at a temperature between 600 and 700 °C points to the decisive role of seeds for the textured growth of WS2, most probably liquid NiSx drops. The rapidly crystallized WS2 films exhibit a pronounced (001) texture with the van der Waals planes oriented parallel to the surface, leading to photoactive layers with a high hole mobility of about 80 cm2/Vs making such films suitable as absorbers for thin film solar cells.

Analyse de l'état mécanique et microstructural de films minces supraconducteurs YBa_2 Cu_3O_7 par diffraction des rayons X

NASA Astrophysics Data System (ADS)

Auzary, S.; Badawi, K. F.; Bimbault, L.; Rabier, J.; Gaboriaud, R. J.; Goudeau, Ph.

1997-01-01

Mechanical and microstructural analysis in a 100nm thin film is presented in this study. Using X-ray diffraction with a tensorial approach, we have determined stresses, strains, stress-free lattice parameters, microdistorsions and diffracting coherent domains size. Stress-free lattice parameters are higher than the bulk values. A high value of stresses is explained as a combination of coherent stresses, thermal stresses and intrinsic ones. Diffraction peaks line profiles analysis suggests grain boundaries presence as well as high lattice elastic microdistorsions. Cette étude présente une analyse de l'état mécanique et microstructurale dans un film mince de 100nm d'épaisseur d'YBCO déposé sur un substrat de MgO. En utilisant la diffraction des rayons X couplée à une approche tensorielle, nous avons déterminé les déformations, les contraintes, les paramètres libres de contraintes, les microdistorsions élastiques ainsi que la taille des domaines cohérents de diffraction. Les paramètres libres de contrainte sont supérieurs à ceux du massif. Une valeur élevée des contraintes est expliquée à partir des contraintes de cohérence, des contraintes thermiques et intrinsèques. L'analyse des profils des pics de diffraction suggère la présence de sous-joints et de distorsions élastiques élevées au niveau des mailles cristallographiques.

Dynamical effects in Bragg coherent x-ray diffraction imaging of finite crystals

NASA Astrophysics Data System (ADS)

Shabalin, A. G.; Yefanov, O. M.; Nosik, V. L.; Bushuev, V. A.; Vartanyants, I. A.

2017-08-01

We present simulations of Bragg coherent x-ray diffractive imaging (CXDI) data from finite crystals in the frame of the dynamical theory of x-ray diffraction. The developed approach is based on a numerical solution of modified Takagi-Taupin equations and can be applied for modeling of a broad range of x-ray diffraction experiments with finite three-dimensional crystals of arbitrary shape also in the presence of strain. We performed simulations for nanocrystals of a cubic and hemispherical shape of different sizes and provided a detailed analysis of artifacts in the Bragg CXDI reconstructions introduced by the dynamical diffraction. Based on our theoretical analysis we developed an analytical procedure to treat effects of refraction and absorption in the reconstruction. Our results elucidate limitations for the kinematical approach in the Bragg CXDI and suggest a natural criterion to distinguish between kinematical and dynamical cases in coherent x-ray diffraction on a finite crystal.

Facile one-pot synthesis of hexagons of NaSrB5O9:Tb3+ phosphor for solid-state lighting

NASA Astrophysics Data System (ADS)

Ramesh, B.; Dillip, G. R.; Deva Prasad Raju, B.; Somasundaram, K.; Prasad Peddi, Siva; de Carvalho dos Anjos, Virgilio; Joo, S. W.

2017-04-01

NaSrB5O9:Tb3+ hexagons were synthesized by a facile solid-state reaction method. The synthesized powders were structurally examined by x-ray diffraction analysis (XRD), and Rietveld refinement was performed using the XRD data and Fullprof software. Hexagon-like morphology was observed using field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The elemental composition of the phosphors was investigated qualitatively by energy dispersive x-ray analysis (EDS) and quantitatively by x-ray photoelectron spectroscopy (XPS). The phosphor has a strong green emission at 545 nm under excitation of 379 nm, which is due to the 5{{\\text{D}}4}{{\\to}7}{{\\text{F}}5} transition of the Tb3+ ion. A lifetime of 3.48 ms was obtained for the phosphor. The important parameters of the light source were determined, such as the thermal quenching, critical distance, the nature of the dopant ion interaction, color coordinates, and quantum yield values. Other reported properties include the site occupancy of the dopant, surface properties, morphological properties, and optical properties.

Comparative study of structural and magnetic properties of nano-crystalline Li 0.5Fe 2.5O 4 prepared by various methods

NASA Astrophysics Data System (ADS)

Verma, Vivek; Pandey, Vibhav; Singh, Sukhveer; Aloysius, R. P.; Annapoorni, S.; Kotanala, R. K.

2009-08-01

Lithium ferrite has been considered as one of the highly strategic magnetic material. Nano-crystalline Li 0.5Fe 2.5O 4 was prepared by four different techniques and characterized by X-ray diffraction, vibrating sample magnetometer (VSM), transmission electron microscope (TEM) and Fourier transform infrareds (FTIR). The effect of annealing temperature (700, 900 and 1050 °C) on microstructure has been correlated to the magnetic properties. From X-ray diffraction patterns, it is confirmed that the pure phase of lithium ferrite began to form at 900 °C annealing. The particle size of as-prepared lithium ferrite was observed around 40, 31, 22 and 93 nm prepared by flash combustion, sol-gel, citrate precursor and standard ceramic technique, respectively. Lithium ferrite prepared by citrate precursor method shows a maximum saturation magnetization 67.6 emu/g at 5 KOe.

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

NASA Astrophysics Data System (ADS)

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

2003-10-01

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

Determination of the size and phase composition of silver nanoparticles in a gel film of bacterial cellulose by small-angle X-ray scattering, electron diffraction, and electron microscopy

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

Volkov, V. V.; Klechkovskaya, V. V., E-mail: klechvv@ns.crys.ras.ru; Shtykova, E. V.

2009-03-15

The nanoscale structural features in a composite (gel film of Acetobacter Xylinum cellulose with adsorbed silver nanoparticles, stabilized by N-polyvinylpyrrolidone) have been investigated by small-angle X-ray scattering. The size distributions of inhomogeneities in the porous structure of the cellulose matrix and the size distributions of silver nanoparticles in the composite have been determined. It is shown that the sizes of synthesized nanoparticles correlate with the sizes of inhomogeneities in the gel film. Particles of larger size (with radii up to 100 nm) have also been found. Electron microscopy of thin cross sections of a dried composite layer showed that largemore » particles are located on the cellulose layer surface. Electron diffraction revealed a crystal structure of silver nanoparticles in the composite.« less

Conducting linear chains of sulphur inside carbon nanotubes

PubMed Central

Fujimori, Toshihiko; Morelos-Gómez, Aarón; Zhu, Zhen; Muramatsu, Hiroyuki; Futamura, Ryusuke; Urita, Koki; Terrones, Mauricio; Hayashi, Takuya; Endo, Morinobu; Young Hong, Sang; Chul Choi, Young; Tománek, David; Kaneko, Katsumi

2013-01-01

Despite extensive research for more than 200 years, the experimental isolation of monatomic sulphur chains, which are believed to exhibit a conducting character, has eluded scientists. Here we report the synthesis of a previously unobserved composite material of elemental sulphur, consisting of monatomic chains stabilized in the constraining volume of a carbon nanotube. This one-dimensional phase is confirmed by high-resolution transmission electron microscopy and synchrotron X-ray diffraction. Interestingly, these one-dimensional sulphur chains exhibit long domain sizes of up to 160 nm and high thermal stability (~800 K). Synchrotron X-ray diffraction shows a sharp structural transition of the one-dimensional sulphur occurring at ~450–650 K. Our observations, and corresponding electronic structure and quantum transport calculations, indicate the conducting character of the one-dimensional sulphur chains under ambient pressure. This is in stark contrast to bulk sulphur that needs ultrahigh pressures exceeding ~90 GPa to become metallic. PMID:23851903

Enhancement in surface area and magnetization of CoFe2O4 nanoparticles for targeted drug delivery application

NASA Astrophysics Data System (ADS)

Kale, Swati B.; Somvanshi, Sandeep B.; Sarnaik, M. N.; More, S. D.; Shukla, S. J.; Jadhav, K. M.

2018-05-01

This paper reports facile synthesis, characterizations by X-ray diffraction and scanning electron microscopy and magnetic behaviour of cobalt ferrite nanoparticles. Cobalt ferrite nanoparticles were prepared by sol-gel auto combustion technique using glycine as a fuel. Phase purity and nanocrystalline nature of the prepared sample was confirmed through X-ray diffraction technique. No extra peak other than cubic spinel structure was observed in the XRD pattern. The crystallite size calculated by using Scherrer's formula is of the order of 21.6 nm indicating the nanocrystalline nature of the prepared cobalt ferrite sample. The surface morphological studies were carried out using scanning electron microscope (SEM). SEM image shows homogeneous, agglomerated particles with sponge-like form. The saturation magnetization, coercivity and remenance magnetization obtained by hysteresis curve clearly gives the evidence of excellent and enhanced magnetic behaviour.

Green synthesis of silver nanoparticles from Moringa oleifera leaf extracts and its antimicrobial potential

NASA Astrophysics Data System (ADS)

Moodley, Jerushka S.; Babu Naidu Krishna, Suresh; Pillay, Karen; Sershen; Govender, Patrick

2018-03-01

In this study we report on the synthesis of silver nanoparticles (AgNPs) from the leaf extracts of Moringa oleifera using sunlight irradiation as primary source of energy, and its antimicrobial potential. Silver nanoparticle formation was confirmed by surface plasmon resonance at 450 nm and 440 nm, respectively for both fresh and freeze-dried leaf samples. Crystanality of AgNPs was confirmed by transmission electron microscopy, scanning electron microscopy with energy dispersive x-ray spectroscopy and Fourier transform infrared (FTIR) spectroscopy analysis. FTIR spectroscopic analysis suggested that flavones, terpenoids and polysaccharides predominate and are primarily responsible for the reduction and subsequent capping of AgNPs. X-ray diffraction analysis also demonstrated that the size range of AgNPs from both samples exhibited average diameters of 9 and 11 nm, respectively. Silver nanoparticles showed antimicrobial activity on both bacterial and fungal strains. The biosynthesised nanoparticle preparations from M. oleifera leaf extracts exhibit potential for application as broad-spectrum antimicrobial agents.

Exploring the Nature of Cellulose Microfibrils

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

Su, Ying; Burger, Christian; Ma, Hongyang

2015-03-20

Ultrathin cellulose microfibril fractions were extracted from spruce wood powder using combined delignification, TEMPO-catalyzed oxidation, and sonication processes. Small-angle X-ray scattering of these microfibril fractions in a “dilute” aqueous suspension (concentration 0.077 wt %) revealed that their shape was in the form of nanostrip with 4 nm width and only about 0.5 nm thicknesses. We found that these dimensions were further confirmed by TEM and AFM measurements. The 0.5 nm thickness implied that the nanostrip could contain only a single layer of cellulose chains. At a higher concentration (0.15 wt %), SAXS analysis indicated that these nanostrips aggregated into amore » layered structure. The X-ray diffraction of samples collected at different preparation stages suggested that microfibrils were delaminated along the (110) planes from the Iβ cellulose crystals. Moreover, the degree of oxidation and solid-state 13C NMR characterizations indicated that, in addition to the surface molecules, some inner molecules of microfibrils were also oxidized, facilitating the delamination into cellulose nanostrips.« less

Exploring the nature of cellulose microfibrils.

PubMed

Su, Ying; Burger, Christian; Ma, Hongyang; Chu, Benjamin; Hsiao, Benjamin S

2015-04-13

Ultrathin cellulose microfibril fractions were extracted from spruce wood powder using combined delignification, TEMPO-catalyzed oxidation, and sonication processes. Small-angle X-ray scattering of these microfibril fractions in a "dilute" aqueous suspension (concentration 0.077 wt %) revealed that their shape was in the form of nanostrip with 4 nm width and only about 0.5 nm thicknesses. These dimensions were further confirmed by TEM and AFM measurements. The 0.5 nm thickness implied that the nanostrip could contain only a single layer of cellulose chains. At a higher concentration (0.15 wt %), SAXS analysis indicated that these nanostrips aggregated into a layered structure. The X-ray diffraction of samples collected at different preparation stages suggested that microfibrils were delaminated along the (11̅0) planes from the Iβ cellulose crystals. The degree of oxidation and solid-state (13)C NMR characterizations indicated that, in addition to the surface molecules, some inner molecules of microfibrils were also oxidized, facilitating the delamination into cellulose nanostrips.

Gold nanoparticles supported on magnesium oxide for CO oxidation

NASA Astrophysics Data System (ADS)

Carabineiro, Sónia Ac; Bogdanchikova, Nina; Pestryakov, Alexey; Tavares, Pedro B.; Fernandes, Lisete Sg; Figueiredo, José L.

2011-06-01

Au was loaded (1 wt%) on a commercial MgO support by three different methods: double impregnation, liquid-phase reductive deposition and ultrasonication. Samples were characterised by adsorption of N2 at -96°C, temperature-programmed reduction, high-resolution transmission electron microscopy, energy-dispersive X-ray spectroscopy and X-ray diffraction. Upon loading with Au, MgO changed into Mg(OH)2 (the hydroxide was most likely formed by reaction with water, in which the gold precursor was dissolved). The size range for gold nanoparticles was 2-12 nm for the DIM method and 3-15 nm for LPRD and US. The average size of gold particles was 5.4 nm for DIM and larger than 6.5 for the other methods. CO oxidation was used as a test reaction to compare the catalytic activity. The best results were obtained with the DIM method, followed by LPRD and US. This can be explained in terms of the nanoparticle size, well known to determine the catalytic activity of gold catalysts.

Critical layer thickness in In/sub 0. 2/Ga/sub 0. 8/As/GaAs single strained quantum well structures

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

Fritz, I.J.; Gourley, P.L.; Dawson, L.R.

1987-09-28

We report accurate determination of the critical layer thickness (CLT) for single strained-layer epitaxy in the InGaAs/GaAs system. Our samples were molecular beam epitaxially grown, selectively doped, single quantum well structures comprising a strained In/sub 0.2/Ga/sub 0.8/As layer imbedded in GaAs. We determined the CLT by two sensitive techniques: Hall-effect measurements at 77 K and photoluminescence microscopy. Both techniques indicate a CLT of about 20 nm. This value is close to that determined previously (--15 nm) for comparable strained-layer superlattices, but considerably less than the value of --45 nm suggested by recent x-ray rocking-curve measurements. We show by a simplemore » calculation that photoluminescence microscopy is more than two orders of magnitude more sensitive to dislocations than x-ray diffraction. Our results re-emphasize the necessity of using high-sensitivity techniques for accurate determination of critical layer thicknesses.« less

Acceptor-modulated optical enhancements and band-gap narrowing in ZnO thin films

NASA Astrophysics Data System (ADS)

Hassan, Ali; Jin, Yuhua; Irfan, Muhammad; Jiang, Yijian

2018-03-01

Fermi-Dirac distribution for doped semiconductors and Burstein-Moss effect have been correlated first time to figure out the conductivity type of ZnO. Hall Effect in the Van der Pauw configuration has been applied to reconcile our theoretical estimations which evince our assumption. Band-gap narrowing has been found in all p-type samples, whereas blue Burstein-Moss shift has been recorded in the n-type films. Atomic Force Microscopic (AFM) analysis shows that both p-type and n-type films have almost same granular-like structure with minor change in average grain size (˜ 6 nm to 10 nm) and surface roughness rms value 3 nm for thickness ˜315 nm which points that grain size and surface roughness did not play any significant role in order to modulate the conductivity type of ZnO. X-ray diffraction (XRD), Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Photoelectron Spectroscopy (XPS) have been employed to perform the structural, chemical and elemental analysis. Hexagonal wurtzite structure has been observed in all samples. The introduction of nitrogen reduces the crystallinity of host lattice. 97% transmittance in the visible range with 1.4 × 107 Ω-1cm-1 optical conductivity have been detected. High absorption value in the ultra-violet (UV) region reveals that NZOs thin films can be used to fabricate next-generation high-performance UV detectors.

Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

NASA Technical Reports Server (NTRS)

Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

2010-01-01

An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

Nanometer-scale characterization of laser-driven plasmas, compression, shocks and phase transitions, by coherent small angle x-ray scattering

NASA Astrophysics Data System (ADS)

Kluge, Thomas

2015-11-01

Combining ultra-intense short-pulse and high-energy long-pulse lasers, with brilliant coherent hard X-ray FELs, such as the Helmholtz International Beamline for Extreme Fields (HIBEF) under construction at the HED Instrument of European XFEL, or MEC at LCLS, holds the promise to revolutionize our understanding of many High Energy Density Physics phenomena. Examples include the relativistic electron generation, transport, and bulk plasma response, and ionization dynamics and heating in relativistic laser-matter interactions, or the dynamics of laser-driven shocks, quasi-isentropic compression, and the kinetics of phase transitions at high pressure. A particularly promising new technique is the use of coherent X-ray diffraction to characterize electron density correlations, and by resonant scattering to characterize the distribution of specific charge-state ions, either on the ultrafast time scale of the laser interaction, or associated with hydrodynamic motion. As well one can image slight density changes arising from phase transitions inside of shock-compressed high pressure matter. The feasibility of coherent diffraction techniques in laser-driven matter will be discussed. including recent results from demonstration experiments at MEC. Among other things, very sharp density changes from laser-driven compression are observed, having an effective step width of 10 nm or smaller. This compares to a resolution of several hundred nm achievedpreviously with phase contrast imaging. and on behalf of HIBEF User Consortium, for the Helmholtz International Beamline for Extreme Fields at the European XFEL.

Rapid extra-/intracellular biosynthesis of gold nanoparticles by the fungus Penicillium sp.

NASA Astrophysics Data System (ADS)

Du, Liangwei; Xian, Liang; Feng, Jia-Xun

2011-03-01

In this work, the fungus Penicillium was used for rapid extra-/intracellular biosynthesis of gold nanoparticles. AuCl4 - ions reacted with the cell filtrate of Penicillium sp. resulting in extracellular biosynthesis of gold nanoparticles within 1 min. Intracellular biosynthesis of gold nanoparticles was obtained by incubating AuCl4 - solution with fungal biomass for 8 h. The gold nanoparticles were characterized by means of visual observation, UV-Vis absorption spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). The extracellular nanoparticles exhibited maximum absorbance at 545 nm in UV-Vis spectroscopy. The XRD spectrum showed Bragg reflections corresponding to the gold nanocrystals. TEM exhibited the formed spherical gold nanoparticles in the size range from 30 to 50 nm with an average size of 45 nm. SEM and TEM revealed that the intracellular gold nanoparticles were well dispersed on the cell wall and within the cell, and they are mostly spherical in shape with an average diameter of 50 nm. The presence of gold was confirmed by EDX analysis.

Synthesis, self-assembly, and properties of Mn doped ZnO nanoparticles.

PubMed

Barick, K C; Bahadur, D

2007-06-01

We report here a novel process to prepare Mn doped ZnO nanoparticles by a soft chemical route at low temperature. The synthesis process is based on the hydrolysis of zinc acetate dihydrate and manganese acetate tetrahydrate heated under reflux to 160-175 degrees C using diethylene glycol as a solvent. X-ray diffraction analysis reveals that the Mn doped ZnO crystallizes in a wurtzite structure with crystal size of 15-25 nm. These nano size crystallites of Mn doped ZnO self-organize into polydisperse spheres in size ranging from 100-400 nm. Transmission Electron Microscopy image also shows that each sphere is made up of numerous nanocrystals of average diameter 15-25 nm. By means of X-ray photoelectron spectroscopy and electron spin resonance spectroscopy, we determined the valence state of Mn ions as 2+. These nanoparticles were found to be ferromagnetic at room temperature. Monodisperse porous spheres (approximately 250 nm) were obtained by size selective separation technique and then self-assembled in a closed pack periodic array through sedimentation with slow solvent evaporation, which gives strong opalescence in visible region.

Influence of deposition temperature on WTiN coatings tribological performance

NASA Astrophysics Data System (ADS)

Londoño-Menjura, R. F.; Ospina, R.; Escobar, D.; Quintero, J. H.; Olaya, J. J.; Mello, A.; Restrepo-Parra, E.

2018-01-01

WTiN films were grown on silicon and stainless-steel substrates using the DC magnetron sputtering technique. The substrate temperature was varied taking values of 100 °C, 200 °C, 300 °C, and 400 °C. X-ray diffraction analysis allowed us to identify a rock salt-type face centered cubic (FCC) structure, with a lattice parameter of approximately 4.2 nm, a relatively low microstrain (deformations at microscopy level, between 4.7% and 6.7%), and a crystallite size of a few nanometers (11.6 nm-31.5 nm). The C1s, N1s, O1s, Ti2p, W4s, W4p, W4d and W4f narrow spectra were obtained using X-ray photoelectron spectroscopy (XPS) and depending on the substrate temperature, the deconvoluted spectra presented different binding energies. Grain sizes and roughness (approximately 4 nm) of films were determined using atomic force microscopy. Scratch and pin on disc tests were conducted, showing better performance of the film grown at 200 °C. This sample exhibited a lower roughness, coefficient of friction, and wear rate.

Crystal Growth and Luminescence Properties of Yb-doped Gd3Al2Ga3O12 Infra-red Scintillator

NASA Astrophysics Data System (ADS)

Suzuki, Akira; Kurosawa, Shunsuke; Nagata, Shinji; Yamamura, Tomoo; Pejchal, Jan; Yamaji, Akihiro; Yokota, Yuui; Shirasaki, Kenji; Homma, Yoshiya; Aoki, Dai; Shikama, Tatsuo; Yoshikawa, Akira

2014-07-01

1-mol%-Yb-doped Gd3Al2Ga3O12 infra-red scintillator crystal has been studied as a novel implantable radiation monitor in radiation therapy. Powder X-ray diffraction measurement and chemical analysis with a field emission scanning microscope and wavelength dispersive spectrometer determined its garnet structure and average chemical composition of Yb0.03±0.01Gd2.99±0.07Al2.21±0.08Ga2.64±0.09O12.10±0.09. Transmittance measurements reached high values of approximately 70% in the human body transparency region between 650 to 1200 nm. Photoluminescence peaks were detected around 970 and 1030 nm under the 940 nm excitation with a Xe lamp. Infra-red scintillation emissions were clearly observed around 970 and 1030 nm due to Yb3+ 4f-4f transitions under X-ray excitation. Therefore, these results suggest that Yb-doped Gd3Al2Ga3O12 might be used as an infra-red scintillator material.

Philip A. Parilla | NREL

Science.gov Websites

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

Erratum to: Psammoma bodies in two types of human ovarian tumours: a mineralogical study

NASA Astrophysics Data System (ADS)

Meng, Fanlu; Wang, Changqiu; Li, Yan; Lu, Anhuai; Mei, Fang; Liu, Jianying; Du, Jingyun; Zhang, Yan

2015-06-01

Psammoma body (PB) is a common form of calcification in pathological diagnosis and closely relevant to tumours. This paper focuses on the mineralogical characteristics of PBs in ovarian serous cancer and teratoma by using polarization microscope (POM), environmental scanning electron microscope (ESEM), micro-Fourier transform infrared spectroscopy (micro-FT-IR), transmission electron microscope (TEM), micro-area synchrotron radiation X-ray powder diffraction (μ-SRXRD) and fluorescence (μ-SRXRF). Both the PBs in tissues and separated from eight typical cases were investigated. POM and ESEM observation revealed the inside-out growth pattern of PBs. μ-SRXRD and micro-FT-IR results demonstrated the dominant mineral phase of PBs in ovarian serous cancer and teratoma was AB-type carbonate hydroxyapatite (Ca10[(PO4)6-x-y(CO3)x(HPO4)y][(OH)2-u(CO3)u] with 0 ≤ x,y,u ≤ 2). As observed by ESEM and TEM, the layer-rich PBs in teratoma were up to 70 μm and mainly consisted of 5 nm-wide, 5-12 nm-long columnar crystals; the PBs in ovarian serous cancer with a maximum diameter of 35 μm were composed of slightly longer columnar crystals and granulates with 20-100 nm in diameter. The selected area electron diffraction patterns showed dispersed polycrystalline diffraction rings with arching behavior of (002) diffraction, indicating the aggregated nanocrystals grew in the preferred orientation of (002) face. The EDX and μ-SRXRF results together indicated the existence of Na, Mg, Zn and Sr in PBs. These detailed mineralogical characteristics may help uncover the nature of the pathological PBs in ovary.

Psammoma bodies in two types of human ovarian tumours: a mineralogical study

NASA Astrophysics Data System (ADS)

Fanlu, Meng; Changqiu, Wang; Yan, Li; Anhuai, Lu; Fang, Mei; Jianying, Liu; Jingyun, Du; Yan, Zhang

2015-06-01

Psammoma body (PB) is a common form of calcification in pathological diagnosis and closely relevant to tumours. This paper focuses on the mineralogical characteristics of PBs in ovarian serous cancer and teratoma by using polarization microscope (POM), environmental scanning electron microscope (ESEM), micro-Fourier transform infrared spectroscopy (micro-FT-IR), transmission electron microscope (TEM), micro-area synchrotron radiation X-ray powder diffraction (μ-SRXRD) and fluorescence (μ-SRXRF). Both the PBs in tissues and separated from eight typical cases were investigated. POM and ESEM observation revealed the inside-out growth pattern of PBs. μ-SRXRD and micro-FT-IR results demonstrated the dominant mineral phase of PBs in ovarian serous cancer and teratoma was AB-type carbonate hydroxyapatite (Ca10[(PO4)6-x-y(CO3)x(HPO4 2-)y][(OH)2-u(CO3)u] with 0 ≤ x,y,u ≤ 2). As observed by ESEM and TEM, the layer-rich PBs in teratoma were up to 70 μm and mainly consisted of 5 nm-wide, 5-12 nm-long columnar crystals; the PBs in ovarian serous cancer with a maximum diameter of 35 μm were composed of slightly longer columnar crystals and granulates with 20-100 nm in diameter. The selected area electron diffraction patterns showed dispersed polycrystalline diffraction rings with arching behavior of (002) diffraction, indicating the aggregated nanocrystals grew in the preferred orientation of (002) face. The EDX and μ-SRXRF results together indicated the existence of Na, Mg, Zn and Sr in PBs. These detailed mineralogical characteristics may help uncover the nature of the pathological PBs in ovary.

Cadmium effect on structural properties of Cu{sub 2}Zn{sub 1-x}Cd{sub x}SnS{sub 4} quinternary alloys nanostructures

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

Ibraheam, A. S.; Al-Douri, Y., E-mail: yaldouri@yahoo.com; Hashim, U.

The study report novel sensing plat of extended quinternart materials, Cu{sub 2}Zn{sub 1-x}d{sub x}SnS{sub 4} quinternary alloy nanostructures were fabricated onto oxidized silicon substrate by sol-gel method and characterized were synthesized by X-ray diffraction (XRD). The XRD peaks were shifted towered the lower angle side with increasing cadmium content. The practical size average of the Cu{sub 2}Zn{sub 1-x}d{sub x}SnS{sub 4} quinternary alloy nanostructures between 34.55 to 63.30 nm.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources.

PubMed

Tang, M X; Zhang, Y Y; E, J C; Luo, S N

2018-05-01

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic-plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of the diffraction patterns is discussed.

Simulations of X-ray diffraction of shock-compressed single-crystal tantalum with synchrotron undulator sources

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

Tang, M. X.; Zhang, Y. Y.; E, J. C.

Polychromatic synchrotron undulator X-ray sources are useful for ultrafast single-crystal diffraction under shock compression. Here, simulations of X-ray diffraction of shock-compressed single-crystal tantalum with realistic undulator sources are reported, based on large-scale molecular dynamics simulations. Purely elastic deformation, elastic–plastic two-wave structure, and severe plastic deformation under different impact velocities are explored, as well as an edge release case. Transmission-mode diffraction simulations consider crystallographic orientation, loading direction, incident beam direction, X-ray spectrum bandwidth and realistic detector size. Diffraction patterns and reciprocal space nodes are obtained from atomic configurations for different loading (elastic and plastic) and detection conditions, and interpretation of themore » diffraction patterns is discussed.« less

Rationale for the crystallization of titania polymorphs in solution

NASA Astrophysics Data System (ADS)

Kränzlin, N.; Staniuk, M.; Heiligtag, F. J.; Luo, L.; Emerich, H.; van Beek, W.; Niederberger, M.; Koziej, D.

2014-11-01

We use in situ X-ray absorption and diffraction studies to directly monitor the crystallization of different titania polymorphs in one and the same solution. We find that, despite the commonly accepted polymorphic-crossover from anatase to rutile triggered by the critical size of nanoparticles, in the solution their respective nucleation and growth are independent processes. Moreover, we find that 5.9 nm rutile nanoparticles are formed prior to the formation of 8.4 nm anatase nanoparticles. Our results suggest that the origins of this crystallization mechanism lie in the formation of an intermediate non-crystalline phase and in time-dependent changes in the chemical environment.We use in situ X-ray absorption and diffraction studies to directly monitor the crystallization of different titania polymorphs in one and the same solution. We find that, despite the commonly accepted polymorphic-crossover from anatase to rutile triggered by the critical size of nanoparticles, in the solution their respective nucleation and growth are independent processes. Moreover, we find that 5.9 nm rutile nanoparticles are formed prior to the formation of 8.4 nm anatase nanoparticles. Our results suggest that the origins of this crystallization mechanism lie in the formation of an intermediate non-crystalline phase and in time-dependent changes in the chemical environment. Electronic supplementary information (ESI) available: Detailed instructions on the experimental part including set-up, recorded XAS and PXRD raw data and their details. See DOI: 10.1039/c4nr04346d

Structural and spectroscopic study of mechanically synthesized SnO{sub 2} nanostructures

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

Vij, Ankush, E-mail: vij-anx@yahoo.com; Kumar, Ravi; Presently at Beant College of Engineering and Technology, Gurdaspur-143521

2016-05-23

We report the single step synthesis of SnO{sub 2} nanostructures using high energy mechanical attrition method. X-ray diffraction (XRD) pattern reveals the single phase rutile structure with appreciable broadening of diffraction peaks, which is a signature of nanostructure formation. The average crystallite size of SnO{sub 2} nanostructures has been calculated to be ~15 nm. The micro-Raman study reveals the shifting of A{sub 1g} Raman mode towards lower wave number, which is correlated with the nanostructure formation.

Astigmatism correction in x-ray scanning photoemission microscope with use of elliptical zone plate

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

Ade, H.; Ko, C.; Anderson, E.

1992-03-02

We report the impact of an elliptical, high resolution zone plate on the performance of an initially astigmatic soft x-ray scanning photoemission microscope. A zone plate with carefully calibrated eccentricity has been used to eliminate astigmatism arising from transport optics, and an improvement of about a factor of 3 in spatial resolution was achieved. The resolution is still dominated by the source size and chromatic aberrations rather than by diffraction and coma, and a further gain of about a factor of 2 in resolution is possible. Sub 100 nm photoemission microscopy with primary photoelectrons is now within reach.

Hydrothermal synthesis of uniform WO{sub 3} submicrospheres using thiourea as an assistant agent

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

Su, X.T.; Xiao, F.; Lin, J.L.

2010-08-15

Nearly monodisperse tungsten trioxide submicrospheres have been synthesized with tungsten acid and HCl as the starting materials and thiourea as a structure-directing agent through a facile hydrothermal method. The obtained products were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy and energy dispersive X-ray, respectively. The results show that the WO{sub 3} submicrospheres are monodisperse with a diameter of about 800-1000 nm. The morphology of the products gradually evolutes from rods to spheres with increase of the reaction time. The formation mechanism of the WO{sub 3} submicrospheres is primarily discussed.

A High-Precision Instrument for Mapping of Rotational Errors in Rotary Stages

DOE PAGES

Xu, W.; Lauer, K.; Chu, Y.; ...

2014-11-02

A rotational stage is a key component of every X-ray instrument capable of providing tomographic or diffraction measurements. To perform accurate three-dimensional reconstructions, runout errors due to imperfect rotation (e.g. circle of confusion) must be quantified and corrected. A dedicated instrument capable of full characterization and circle of confusion mapping in rotary stages down to the sub-10 nm level has been developed. A high-stability design, with an array of five capacitive sensors, allows simultaneous measurements of wobble, radial and axial displacements. The developed instrument has been used for characterization of two mechanical stages which are part of an X-ray microscope.

In situ X-ray ptychography imaging of high-temperature CO2 acceptor particle agglomerates

NASA Astrophysics Data System (ADS)

Høydalsvik, Kristin; Bø Fløystad, Jostein; Zhao, Tiejun; Esmaeili, Morteza; Diaz, Ana; Andreasen, Jens W.; Mathiesen, Ragnvald H.; Rønning, Magnus; Breiby, Dag W.

2014-06-01

Imaging nanoparticles under relevant reaction conditions of high temperature and gas pressure is difficult because conventional imaging techniques, like transmission electron microscopy, cannot be used. Here we demonstrate that the coherent diffractive imaging technique of X-ray ptychography can be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO2 capture material, was studied at a pressure of one atmosphere in air and in CO2, at temperatures exceeding 600 °C. Images with a spatial resolution better than 200 nm were retrieved, and possibilities for improving the experiment are described.

Coherent X-ray diffraction imaging of nanoengineered polymeric capsules

NASA Astrophysics Data System (ADS)

Erokhina, S.; Pastorino, L.; Di Lisa, D.; Kiiamov, A. G.; Faizullina, A. R.; Tayurskii, D. A.; Iannotta, S.; Erokhin, V.

2017-10-01

For the first time, nanoengineered polymeric capsules and their architecture have been studied with coherent X-ray diffraction imaging technique. The use of coherent X-ray diffraction imaging technique allowed us to analyze the samples immersed in a liquid. We report about the significant difference between polymeric capsule architectures under dry and liquid conditions.

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Johns Hopkins University School of Medicine, Baltimore, MD 21205; Lyubimov, Artem Y.

A highly X-ray-transparent, silicon nitride-based device has been designed and fabricated to harvest protein microcrystals for high-resolution X-ray diffraction data collection using microfocus beamlines and XFELs. Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming themore » challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

Rapid prototyping of Fresnel zone plates via direct Ga(+) ion beam lithography for high-resolution X-ray imaging.

PubMed

Keskinbora, Kahraman; Grévent, Corinne; Eigenthaler, Ulrike; Weigand, Markus; Schütz, Gisela

2013-11-26

A significant challenge to the wide utilization of X-ray microscopy lies in the difficulty in fabricating adequate high-resolution optics. To date, electron beam lithography has been the dominant technique for the fabrication of diffractive focusing optics called Fresnel zone plates (FZP), even though this preparation method is usually very complicated and is composed of many fabrication steps. In this work, we demonstrate an alternative method that allows the direct, simple, and fast fabrication of FZPs using focused Ga(+) beam lithography practically, in a single step. This method enabled us to prepare a high-resolution FZP in less than 13 min. The performance of the FZP was evaluated in a scanning transmission soft X-ray microscope where nanostructures as small as sub-29 nm in width were clearly resolved, with an ultimate cutoff resolution of 24.25 nm, demonstrating the highest first-order resolution for any FZP fabricated by the ion beam lithography technique. This rapid and simple fabrication scheme illustrates the capabilities and the potential of direct ion beam lithography (IBL) and is expected to increase the accessibility of high-resolution optics to a wider community of researchers working on soft X-ray and extreme ultraviolet microscopy using synchrotron radiation and advanced laboratory sources.

Influence of preliminary deformation on the hardening effect upon aging of Al-Cu-Li alloys

NASA Astrophysics Data System (ADS)

Betsofen, S. Ya.; Ashmarin, A. A.; Knyazev, M. I.; Dolgova, M. I.

2016-09-01

The influence of preliminary deformation upon rolling of wedge specimens on the mechanical properties and the structural phase state of Al-Cu-Li alloys are studied by X-ray diffraction and hardness measurements. Strong dependence of the hardening effect upon aging on the reduction upon rolling has been revealed. Deformation weakly influences the hardness and significantly increases the hardening upon aging. Herewith, the hardening effect is nearly absent at the minimum deformation ratio of 1% and increases with its increase. It is demonstrated that the content of T1 phase increases from 2 to 4% in the range of a preliminary deformation ratio of 6-10% and the content of δ' phase is 17% at a deformation ratio in the range 1‒6% and increases to 18-19% at a deformation ratio of 6-10%. The δ' phase in an alloy contains <20% nanocrystalline particles with 6-20 nm in size, and the remaining part consists of amorphous particles (as detected by X-ray diffraction) <5 nm in size, which precipitate coherently from the matrix and have the same orientation as the nanocrystalline particles and the solid solution.

Characterisation and sintering of nanophase hydroxyapatite synthesised by a species of Serratia

NASA Astrophysics Data System (ADS)

LSammons, R.; Thackray, A. C.; Medina Ledo, H.; Marquis, P. M.; Jones, I. P.; Yong, P.; Macaskie, L. E.

2007-12-01

The bacterium Serratia sp. NCIMB40259, which grows as a biofilm on polymeric, glass and metal substrates, produces extracellular crystals of hydroxyapatite (HA) by enzymatic cleavage of β-glycerophosphate in the presence of calcium chloride. Following growth on polyurethane foam, biomineralisation and subsequent sintering, an HA scaffold is formed whose three-dimensional architecture replicates that of the foam and the biofilm. Serratia HA was characterised using X-ray diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The nascent, unsintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61+/- 0.06 and crystal size (TEM) of 50 +/- 10nm length. ED of unsintered crystals and crystals sintered at 600° C showed resolvable ring (unsintered) or dot (600° C) patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. Material sintered at 1200° C consisted of needle-like crystals of length range 54-111nm (XRD) with lattice parameters of a = 9.441 Å and c = 6.875 Å, consistent with HA.

Langmuir-Blodgett and X-ray diffraction studies of isolated photosystem II reaction centers in monolayers and multilayers: physical dimensions of the complex.

PubMed

Uphaus, R A; Fang, J Y; Picorel, R; Chumanov, G; Wang, J Y; Cotton, T M; Seibert, M

1997-04-01

The photosystem II (PSII) reaction center (RC) is a hydrophobic intrinsic protein complex that drives the water-oxidation process of photosynthesis. Unlike the bacterial RC complex, an X-ray crystal structure of the PSII RC is not available. In order to determine the physical dimensions of the isolated PSII RC complex, we applied Langmuir techniques to determine the cross-sectional area of an isolated RC in a condensed monolayer film. Low-angle X-ray diffraction results obtained by examining Langmuir-Blodgett multilayer films of alternating PSII RC/Cd stearate monolayers were used to determine the length (or height; z-direction, perpendicular to the plane of the original membrane) of the complex. The values obtained for a PSII RC monomer were 26 nm2 and 4.8 nm, respectively, and the structural integrity of the RC in the multilayer film was confirmed by several approaches. Assuming a cylindrical-type RC structure, the above dimensions lead to a predicted volume of about 125 nm3. This value is very close to the expected volume of 118 nm3, calculated from the known molecular weight and partial specific volume of the PSII RC proteins. This same type of comparison was also made with the Rhodobacter sphaeroides RC based on published data, and we conclude that the PSII RC is much shorter in length and has a more regular solid geometric structure than the bacterial RC. Furthermore, the above dimensions of the PSII RC and those of PSII core (RC plus proximal antenna) proteins protruding outside the plane of the PSII membrane into the lumenal space as imaged by scanning tunneling microscopy (Seibert, Aust. J. Pl. Physiol. 22, 161-166, 1995) fit easily into the known dimensions of the PSII core complex visualized by others as electron-density projection maps. From this we conclude that the in situ PSII core complex is a dimeric structure containing two copies of the PSII RC.

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

PubMed Central

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

2010-01-01

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

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

DOE PAGES

Huang, Xiaojing; Miao, Huijie; Nelson, Johanna; ...

2011-05-01

Cryogenic microscopy allows one to view frozen hydrated biological and soft matter specimens with good structural preservation and a high degree of stability against radiation damage. We describe a liquid nitrogen-cooled anti-contamination device for cryogenic X-ray diffraction microscopy. The anti-contaminator greatly reduces the buildup of ice layers on the specimen due to condensation of residual water vapor in the experimental vacuum chamber. We show by coherent X-ray diffraction measurements that this leads to fivefold reduction of background scattering, which is important for far-field X-ray diffraction microscopy of biological specimens.

Lu{sub 2}O{sub 3}:Eu{sup 3+} glass ceramic films: Synthesis, structural and spectroscopic studies

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

Carrera Jota, M.L.; García Murillo, A., E-mail: angarciam@ipn.mx; Carrillo Romo, F.

2014-03-01

Graphical abstract: - Highlights: • Lu{sub 2}O{sub 3}:Eu{sup 3+}@SiO{sub 2} films were synthesized by sol–gel and by dip-coating technique. • Effects of incorporating PVP on structural properties were studied. • Effects of incorporating silica (SiO{sub 2}) luminescence characteristics were analyzed. • X-ray diffraction results showed that Lu{sub 2}O{sub 3}:Eu{sup 3+}@SiO{sub 2} crystallizes at 700 °C. • The 611 nm emission for the Lu:Si = 8:1 system presented an improvement. - Abstract: For the first time, transparent and crack free europium-doped lutetia silica sol–gel films were synthesized using the dip-coating technique on silica quartz substrates. In this study, we examined themore » effects of incorporating polyvinylpyrrolidone (PVP) and silica (SiO{sub 2}) into different precursor solutions for different Lu–Si molar ratios: 4:1, 6:1, 8:1 and 10:1. Different systems, such as Lu{sub 2}O{sub 3}:Eu{sup 3+}@SiO{sub 2} (using the above Lu:Si molar ratios), were synthesized by sol–gel and by dip-coating technique, employing acetylacetonate lutetium and tetraethylorthosilicate as Lu and Si precursors, in order to produce Lu{sub 2}O{sub 3}:Eu{sup 3+} (5 mol%)@SiO{sub 2} glass–ceramic films. The film microstructure was studied by microRaman spectroscopy (MRS) and X-ray diffraction (XRD) for different Lu:Si molar ratios on films annealed at 700 °C. X-ray diffraction results showed that the lutetium oxide cubic phase crystallizes in the silica matrix at 700 °C, and the crystallite size of Lu{sub 2}O{sub 3}:Eu{sup 3+}@SiO{sub 2} films varies from 5 nm to 17 nm according to the respective Lu:Si molar ratios. Opto-geometrical parameters determined by m-lines spectroscopy using a 632.5 nm He–Ne laser showed that the Eu{sup 3+} doped films heat-treated at 700 °C presented a thickness and density of 1.7 μm (8.8 g cm{sup −3}), 970 nm (9.2 g cm{sup −3}), 1 μm (9.3 g cm{sup −3}) and 1.3 μm (9.25 g cm{sup −3}) for the Lu:Si = 4:1, 6:1, 8:1 and 10:1 molar ratio systems, respectively. The Lu:Si = 8:1 system 611 nm emission presented an improvement. These results were provided by photoluminescent spectroscopy.« less

Observation of electromigration in a Cu thin line by in situ coherent x-ray diffraction microscopy

NASA Astrophysics Data System (ADS)

Takahashi, Yukio; Nishino, Yoshinori; Furukawa, Hayato; Kubo, Hideto; Yamauchi, Kazuto; Ishikawa, Tetsuya; Matsubara, Eiichiro

2009-06-01

Electromigration (EM) in a 1-μm-thick Cu thin line was investigated by in situ coherent x-ray diffraction microscopy (CXDM). Characteristic x-ray speckle patterns due to both EM-induced voids and thermal deformation in the thin line were observed in the coherent x-ray diffraction patterns. Both parts of the voids and the deformation were successfully visualized in the images reconstructed from the diffraction patterns. This result not only represents the first demonstration of the visualization of structural changes in metallic materials by in situ CXDM but is also an important step toward studying the structural dynamics of nanomaterials using x-ray free-electron lasers in the near future.

Crystal structure and phase transformations of calcium yttrium orthophosphate, Ca 3Y(PO 4) 3

NASA Astrophysics Data System (ADS)

Fukuda, Koichiro; Iwata, Tomoyuki; Niwa, Takahiro

2006-11-01

Crystal structure and phase transformations of calcium yttrium orthophosphate Ca 3Y(PO 4) 3 were investigated by X-ray powder diffraction, selected-area electron diffraction, transmission electron microscopy and optical microscopy. The high-temperature phase is isostructural with eulytite, cubic (space group I4¯3d) with a=0.983320(5) nm, V=0.950790(8) nm 3, Z=4 and D x=3.45 Mg m -3. The crystal structure was refined with a split-atom model, in which the oxygen atoms are distributed over two partially occupied sites. Below the stable temperature range of eulytite, the crystal underwent a martensitic transformation, which is accompanied by the formation of platelike surface reliefs. The inverted crystal is triclinic (space group P1) with a=1.5726(1) nm, b=0.84267(9) nm, c=0.81244(8) nm, α=109.739(4)°, β=90.119(5)°, γ=89.908(7)°, V=1.0134(1) nm 3, Z=4 and D x=3.24 Mg m -3. The crystal grains were composed of pseudo-merohedral twins. The adjacent twin domains were related by the pseudo-symmetry mirror planes parallel to {101¯} with the composition surface {101¯}. When the eulytite was cooled relatively slowly from the stable temperature range, the decomposition reaction of Ca 3Y(PO 4) 3→ β-Ca 3(PO 4) 2+YPO 4 occurred.

Synthesis and Characterization of Nd(3+)-Doped CaF2 Nanoparticles.

PubMed

Yuan, Dan; Li, Weiwei; Mei, Bingchu; Song, Jinghong

2015-12-01

The Ca(1-x)F(2+x):Nd(x) nanoparticles were synthesized by chemical direct precipitation method. X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Image analyzer, absorption spectrum and transmittance were taken to characterization the phases, morphologies, sizes, size distribution and optical properties of the samples. The results indicate that the Ca(1-x)F(2+x):Nd(x) samples can be rationally modified in size and morphology by altering the Nd3+ ions doping concentration. With increasing concentration of Nd3+ ions, the particle size decreased from 24 to 14 nm, the intensity of the diffraction peaks decreased, the Ca(1-x)F(2+x):Nd(x) particles aggregated ion of the formed clusters which should have an effect on both speed and orientation of the particles growth. The transmittance of ceramics with a thickness of 2 mm showed that the transmittance can reach 90% when the doping concentration was 5%, which should be profitable for LD pumping.

Agglomeration dynamics of germanium islands on a silicon oxide substrate: A grazing incidence small-angle x-ray scattering study

NASA Astrophysics Data System (ADS)

Cheynis, F.; Leroy, F.; Passanante, T.; Müller, P.

2013-04-01

Grazing-incidence small-angle X-ray scattering (GISAXS) and grazing-incidence X-ray diffraction techniques are used to characterise the thermally induced solid-state dewetting of Ge(001) thin films leading to the formation of 3D Ge islands. A quantitative analysis based on the Kolmogorov-Johnson-Mehl-Avrami model is derived. The main physical parameters controlling the dewetting (activation energy and kinetic pre-factors) are determined. Assuming that the dewetting is driven by surface/interface minimisation and limited by surface diffusion, the Ge surface self-diffusion reads as Ds ,0c0 e-Ea/(kBT) ˜3×1018 e-2.6±0.3eV/(kBT) nm2/s. GISAXS technique enables to reconstruct the mean Ge-island shape, including facets.

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

PubMed

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

2014-04-01

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

Photoluminescence properties of white light emitting La2O3:Dy3+ nanocrystals

NASA Astrophysics Data System (ADS)

Reenabati Devi, Konsam; Dorendrajit Singh, Shougaijam; David Singh, Th.

2018-06-01

White light emitting nanocrystalline La2O3:Dy3+ phosphors with different concentration (0.5-2 at.%) were synthesized by simple precipitation method. X-ray diffraction (XRD) pattern indicates all the samples crystallizes in the hexagonal phase. Average crystallite sizes of the samples calculated from XRD data were found to be in the range of 20-55 nm. Transmission electron microscopy, selected area electron diffraction, energy dispersive analysis of X-ray and photoluminescence (PL) of the samples are also reported. Strong PL excitation peak due to charge transfer band was observed at 230 nm. Photoluminescence emission peaks observed at 486 and 575 nm were probably attributed to 4F9/2-6H15/2 and 4F9/2-6H13/2 of Dy3+ ions respectively. Optimum luminescence intensity is found at 1 at.% Dy3+ doped La2O3 sample. Further, Commission Internationale de l'é clairage (CIE, 1931) co-ordinates and correlated color temperature (CCT) of the doped sample were calculated to investigate the phosphors' performance and technical applicability of the emitted light respectively. CCT of the 0.5 and 1 at.% samples is 5894 K (white light), within the range of vertical daylight, which makes the synthesised samples promising nanophosphor and may find application in simulating vertical daylight of the Sun.

Photoluminescence properties of white light emitting La2O3:Dy3+ nanocrystals

NASA Astrophysics Data System (ADS)

Reenabati Devi, Konsam; Dorendrajit Singh, Shougaijam; David Singh, Th.

2018-01-01

White light emitting nanocrystalline La2O3:Dy3+ phosphors with different concentration (0.5-2 at.%) were synthesized by simple precipitation method. X-ray diffraction (XRD) pattern indicates all the samples crystallizes in the hexagonal phase. Average crystallite sizes of the samples calculated from XRD data were found to be in the range of 20-55 nm. Transmission electron microscopy, selected area electron diffraction, energy dispersive analysis of X-ray and photoluminescence (PL) of the samples are also reported. Strong PL excitation peak due to charge transfer band was observed at 230 nm. Photoluminescence emission peaks observed at 486 and 575 nm were probably attributed to 4F9/2-6H15/2 and 4F9/2-6H13/2 of Dy3+ ions respectively. Optimum luminescence intensity is found at 1 at.% Dy3+ doped La2O3 sample. Further, Commission Internationale de l'é clairage (CIE, 1931) co-ordinates and correlated color temperature (CCT) of the doped sample were calculated to investigate the phosphors' performance and technical applicability of the emitted light respectively. CCT of the 0.5 and 1 at.% samples is 5894 K (white light), within the range of vertical daylight, which makes the synthesised samples promising nanophosphor and may find application in simulating vertical daylight of the Sun.

The effect of TiO2 thin film thickness on self-cleaning glass properties

NASA Astrophysics Data System (ADS)

Mufti, Nandang; Laila, Ifa K. R.; Hartatiek; Fuad, Abdulloh

2017-05-01

TiO2 is one of semiconductor materials which are widely used as photocatalyst in the form of a thin film. The TiO2 thin film is prepared by using the spin coating sol-gel method. The researcher prepared TiO2 thin film with 3 coating variations and X-Ray Diffraction characterization, UV-Vis Spectrophotometer, Electron Microscopy Scanning, and examined its hydrophilic and anti-fogging properties. The result of X-Ray Diffraction showed that the phase formed is the anatase on 101crystal field. The Electron Microscopy Scanning images showed that TiO2 thin films had a homogeneous surface with the particle sizes as big as 235 nm, 179 nm, and 137 nm. The thickness of each thin film was 2.06μm, 3.33μm, and 5.20μm. The characterization of UV-Vis Spectrophotometer showed that the greatest absorption to the wavelength of visible light was in the thin film’s thickness of 3 coatings with the band-gap determined by using 3.30 eV, 3.33 eV, and 3.33 eV Plot Tuoc. These results indicated that the rate of absorption would be increased by increasing the thickness of film. The increasing thickness of the thin film makes the film hydrophilic able to be used as an anti-fogging substance.

Effect of fluorine doping on highly transparent conductive spray deposited nanocrystalline tin oxide thin films

NASA Astrophysics Data System (ADS)

Moholkar, A. V.; Pawar, S. M.; Rajpure, K. Y.; Bhosale, C. H.; Kim, J. H.

2009-09-01

The undoped and fluorine doped thin films are synthesized by using cost-effective spray pyrolysis technique. The dependence of optical, structural and electrical properties of SnO 2 films, on the concentration of fluorine is reported. Optical absorption, X-ray diffraction, scanning electron microscope (SEM) and Hall effect studies have been performed on SnO 2:F (FTO) films coated on glass substrates. The film thickness varies from 800 to 1572 nm. X-ray diffraction pattern reveals the presence of cassiterite structure with (2 0 0) preferential orientation for FTO films. The crystallite size varies from 35 to 66 nm. SEM and AFM study reveals the surface of FTO to be made of nanocrystalline particles. The electrical study reveals that the films are degenerate and exhibit n-type electrical conductivity. The 20 wt% F doped film has a minimum resistivity of 3.8 × 10 -4 Ω cm, carrier density of 24.9 × 10 20 cm -3 and mobility of 6.59 cm 2 V -1 s -1. The sprayed FTO film having minimum resistance of 3.42 Ω/cm 2, highest figure of merit of 6.18 × 10 -2 Ω -1 at 550 nm and 96% IR reflectivity suggest, these films are useful as conducting layers in electrochromic and photovoltaic devices and also as the passive counter electrode.

Oxygen vacancy effect on photoluminescence of KNb3O8 nanosheets

NASA Astrophysics Data System (ADS)

Li, Rui; Liu, Liying; Ming, Bangming; Ji, Yuhang; Wang, Ruzhi

2018-05-01

Fungus-like potassium niobate (KNb3O8) nanosheets have been synthesized on indium-doped tin oxide (ITO) glass substrates by a simple and environmental friendly two-step hydrothermal process. The prepared samples have been characterized by using X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), High Resolution Transmission Electron Microscope (HRTEM), Fourier Transform Infra-Red Spectroscopy (FTIR), Raman Spectroscopy and X-ray Photoelectron Spectroscopy (XPS). Furthermore, the photoluminescence (PL) of KNb3O8 nanosheets have been systematically studied. The results showed that the PL spectrum is between 300 and 645 nm with a 325 nm light excitation, which is divided into some sub-peaks. It is different from the perfect KNb3O8 nanosheets whose PL emission peaks located at near 433 nm. It should be originated from the effect of the oxygen (O) vacancies in the KNb3O8 nanosheets, which the PLs peaks can be found at about 490 nm and 530 nm by different position of O vacancy. The experimental results are in accordance with the first-principles calculations. Our results may present a feasible clue to estimate the defect position in KNb3O8 by the shape analysis of its spectrum of PLs.

Growth and characterization of MnAu2 films

NASA Astrophysics Data System (ADS)

Cheng, S. F.; Bussmann, K. M.

2017-01-01

MnAu2 films ranging from 60 to 200 nm thickness are deposited by co-sputtering from elemental targets. X-ray diffraction confirmed these films to be nearly single phase with tetragonal lattice parameters of a=0.336 nm and c=0.872 nm that compare well to the bulk values of a=0.336 nm and c=0.876 nm. The density of the films is analyzed using x-ray reflectivity to be 14.95 g/cm3 and within experimental error of previously determined value of 15.00 g/cm3. The films grown on c-plane sapphire, (100)MgO and (100)MgF2 are randomly oriented polycrystalline, while the films grown on a-plane sapphire, (111)MgO and (111)Si/(0001)AlN showed that the (110) plane is parallel to the film plane and there are three sets of domains in equal amount differing by 60° in-plane rotation. Magnetic order is found to become paramagnetic near 360 K which is in close proximity to the bulk value. There are deviations in the slope of hysteresis loops observed at 10 K around 10 kOe that indicate complex magnetic switching.

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

NASA Technical Reports Server (NTRS)

Park, Yoonjoon; Choi, Sang Hyouk; King, Glen C.; Elliott, James R.; Dimarcantonio, Albert L.

2010-01-01

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Crystal structure and europium luminescence of NaMgH3-xFx

NASA Astrophysics Data System (ADS)

Pflug, Christian; Franz, Alexandra; Kohlmann, Holger

2018-02-01

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

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source

NASA Astrophysics Data System (ADS)

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source.

PubMed

Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

2017-04-01

As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

Gas gun shock experiments with single-pulse x-ray phase contrast imaging and diffraction at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Luo, S. N.; Jensen, B. J.; Hooks, D. E.; Fezzaa, K.; Ramos, K. J.; Yeager, J. D.; Kwiatkowski, K.; Shimada, T.

2012-07-01

The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for in situ, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal (<100 ps) and spatial (˜2 μm) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.

Investigations on synthesis, growth and physicochemical properties of semi-organic NLO crystal bis(thiourea) ammonium nitrate for nonlinear frequency conversion

NASA Astrophysics Data System (ADS)

Anbarasi, A.; Ravi Kumar, S. M.; Sundar, G. J. Shanmuga; Mosses, M. Allen; Raj, M. Packiya; Prabhakaran, M.; Ravisankar, R.; Gunaseelan, R.

2017-10-01

Bis(thiourea) ammonium nitrate (BTAN), a new nonlinear optical crystal was grown successfully by slow evaporation technique using water as solvent at room temperature. The grown crystals were optically good quality with dimensions upto 10 × 6 × 3 mm3. Single crystal X-Ray diffraction analysis reveals that the crystal lattice is orthorhombic. From Powder X-ray diffraction analysis the diffraction planes have been indexed. The presence of the various functional groups of BTAN was identified through FTIR spectroscopic analysis. UV cut-off wavelength was observed from optical absorbance spectrum and it was found to be 240 nm. Second harmonic efficiency was determined using Kurtz powder method in comparison with KDP to confirm the nonlinearity of the material. Thermal analysis confirmed that grown crystal is thermally stable upto 184 °C. Microhardness studies show that hardness number (Hv) increases with load. Conductivity measurements such as dielectric, ac and photoconductivity were studied. Growth mechanism and surface features of the as grown single crystal was analysed by chemical etching analysis.

Sol–gel synthesized zinc oxide nanorods and their structural and optical investigation for optoelectronic application

PubMed Central

2014-01-01

Nanostructured zinc oxide (ZnO) nanorods (NRs) with hexagonal wurtzite structures were synthesized using an easy and low-cost bottom-up hydrothermal growth technique. ZnO thin films were prepared with the use of four different solvents, namely, methanol, ethanol, isopropanol, and 2-methoxyethanol, and then used as seed layer templates for the subsequent growth of the ZnO NRs. The influences of the different solvents on the structural and optical properties were investigated through scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, ultraviolet–visible spectroscopy, and photoluminescence. The obtained X-ray diffraction patterns showed that the synthesized ZnO NRs were single crystals and exhibited a preferred orientation along the (002) plane. In addition, the calculated results from the specific models of the refractive index are consistent with the experimental data. The ZnO NRs that grew from the 2-methoxyethanol seeded layer exhibited the smallest grain size (39.18 nm), largest diffracted intensities on the (002) plane, and highest bandgap (3.21 eV). PMID:25221458

Femtosecond Optical and X-Ray Measurement of the Semiconductor-to-Metal Transition in VO2

NASA Astrophysics Data System (ADS)

Cavalleri, Andrea; Toth, Csaba; Squier, Jeff; Siders, Craig; Raksi, Ferenc; Forget, Patrick; Kieffer, Jean-Claude

2001-03-01

While the use of ultrashort visible pulses allows access to ultrafast changes in the optical properties during phase transitions, measurement of the correlation between atomic movement and electronic rearrangement has proven more elusive. Here, we report on the conjunct measurement of ultrafast electronic and structural dynamics during a semiconductor-to-metal phase transition in VO2. Rearrangement of the unit cell from monoclinic to rutile (measured by ultrafast x-ray diffraction) is accompanied by a sharp increase in the electrical conductivity and perturbation of the optical properties (measured with ultrafast visible spectroscopy). Ultrafast x-ray diffraction experiments were performed using femtosecond bursts of Cu-Ka from a laser generated plasma source. A clear rise of the diffraction signal originating from the impulsively generated metallic phase was observable on the sub-picosecond timescale. Optical experiments were performed using time-resolved microscopy, providing temporally and spatially resolved measurements of the optical reflectivity at 800 nm. The data indicate that the reflectivity of the low-temperature semiconducting solid is driven to that of the equilibrium, high-temperature metallic phase within 400 fs after irradiation with a 50-fs laser pulse at fluences in excess of 10 mJ/cm2. In conclusion, the data presented in this contribution suggest that the semiconductor-to-metal transition in VO2 occurs within 500 fs after laser-irradiation. A nonthermal physical mechanism governs the re-arrangement.

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

NASA Astrophysics Data System (ADS)

Kyriacou, Andreas

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

X-ray and neutron diffraction studies of crystallinity in hydroxyapatite coatings.

PubMed

Girardin, E; Millet, P; Lodini, A

2000-02-01

To standardize industrial implant production and make comparisons between different experimental results, we have to be able to quantify the crystallinity of hydroxyapatite. Methods of measuring crystallinity ratio were developed for various HA samples before and after plasma spraying. The first series of methods uses X-ray diffraction. The advantage of these methods is that X-ray diffraction equipment is used widely in science and industry. In the second series, a neutron diffraction method is developed and the results recorded are similar to those obtained by the modified X-ray diffraction methods. The advantage of neutron diffraction is the ability to obtain measurements deep inside a component. It is a nondestructive method, owing to the very low absorption of neutrons in most materials. Copyright 2000 John Wiley & Sons, Inc.

X-ray Diffraction Gratings for Astrophysics

NASA Astrophysics Data System (ADS)

Paerels, Frits

2010-12-01

Over the past year, we have celebrated the tenth anniversary of the Chandra and XMM-Newton X-ray observatories. Both carry powerful, novel diffraction grating spectrometers, which have opened true X-ray spectroscopy for astrophysics. I will describe the design and operation of these instruments, as the background to some of the beautiful results they have produced. But these designs do not exhaust the versatility and essential simplicity of diffraction grating spectrometers, and I will discuss applications for the International X-ray Observatory IXO.

Coating and functionalization of high density ion track structures by atomic layer deposition

NASA Astrophysics Data System (ADS)

Mättö, Laura; Szilágyi, Imre M.; Laitinen, Mikko; Ritala, Mikko; Leskelä, Markku; Sajavaara, Timo

2016-10-01

In this study flexible TiO2 coated porous Kapton membranes are presented having electron multiplication properties. 800 nm crossing pores were fabricated into 50 μm thick Kapton membranes using ion track technology and chemical etching. Consecutively, 50 nm TiO2 films were deposited into the pores of the Kapton membranes by atomic layer deposition using Ti(iOPr)4 and water as precursors at 250 °C. The TiO2 films and coated membranes were studied by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray reflectometry (XRR). Au metal electrode fabrication onto both sides of the coated foils was achieved by electron beam evaporation. The electron multipliers were obtained by joining two coated membranes separated by a conductive spacer. The results show that electron multiplication can be achieved using ALD-coated flexible ion track polymer foils.

Synthesis and characterization of blue fluorescent surface modified nano-graphene oxide flakes as a pH-sensitive drug delivery system

NASA Astrophysics Data System (ADS)

Hashemi, Hamed; Namazi, Hassan

2018-07-01

A new blue fluorescent surface modified graphene oxide (GO) by 6-(5-bromothiophen-2-yl) benzo[c][1,2,5]selenadiazole-5-carboxylic acid (TB) denoted as (GO-TB) was synthesized. The obtained hybrid was characterized by Scanning Electron Microscope (SEM/EDS); Brunauer-Emmett-Teller (BET); X-Ray Diffraction Spectroscopy (XRD); X-Ray Photoelectron Spectroscopy (XPS); UV-Vis Absorption Spectroscopy, and Fourier Transformed Infrared Spectroscopy (FTIR). The synthesized TB moiety displayed orange emission around 590 nm, while GO-TB exhibited a blue photoluminescence around 431 and 159 nm blue shift of photoluminescence. Doxorubicin immobilized on the hybrid surface up to 93%, and the release behavior in three different pHs was investigated. The release profile indicated a pH-dependent liberation with Fickian diffusion mechanism. The cytotoxicity of the hybrid was studied and the IC50 value for the hybrid was 5.16 µg/ml.

Investigation of tin oxide nanofibers synthesized via bio-template technique

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

Kundu, Virender Singh, E-mail: vskundu-kuk@rediffmail.com; Dhiman, Jonny; Kumar, Suresh

In the present paper tin oxide nanofibers have been by synthesized using cotton as bio-template via sol-gel route. This is comparatively a new synthesis technique. The structure and morphology of the obtained SnO{sub 2} nanofibers were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDX). The optical properties of the same have been studied by using UV-Vis spectroscopy. The observed XRD pattern showed that peaks are very narrow and sharp which indicates crystalline nature of samples. SEM images gave an idea about the sample morphology and confirm that the obtained sample were nanofibers. The optical absorbancemore » spectrum of the sample under study was recorded in UV-visible region (200nm- 800nm). The band gap of the sample was found to be 3.95 eV which is higher than their bulk counterpart.« less

One-pot template-free synthesis of uniform-sized fullerene-like magnetite hollow spheres

NASA Astrophysics Data System (ADS)

Zhu, Qing; Zhang, Yue; Liu, Zheng; Zhou, Xinrui; Zhang, Xinmei; Zeng, Lintao

2015-11-01

Uniform-sized Fe3O4 hollow spheres with average diameter of 250 nm and shell thickness of ∼50 nm have been successfully synthesized through a simple hydrothermal route with the presence of di-n-propylamine (DPA) as a weak-base. The reaction time and DPA amount play important roles in the formation of the magnetite hollow spheres. The structures of the products were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectra, scanning electron microscopy, transmission electron microscopy, and high-resolution transmission electron microscopy. The results show that the single-crystalline Fe3O4 hollow spheres are composed of well-aligned magnetite nanoparticles (NPs). The magnetic property investigation shows that these hollow spheres have a higher saturation magnetization (Ms) than the solid spheres. Furthermore, a possible mechanism for the formation of magnetite hollow spheres is proposed based on the experimental observations.

Amorphous boron gasket in diamond anvil cell research

NASA Astrophysics Data System (ADS)

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

2003-11-01

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

Extending X-Ray Crystallography to Allow the Imaging of Noncrystalline Materials, Cells, and Single Protein Complexes

NASA Astrophysics Data System (ADS)

Miao, Jianwei; Ishikawa, Tetsuya; Shen, Qun; Earnest, Thomas

2008-05-01

In 1999, researchers extended X-ray crystallography to allow the imaging of noncrystalline specimens by measuring the X-ray diffraction pattern of a noncrystalline specimen and then directly phasing it using the oversampling method with iterative algorithms. Since then, the field has evolved moving in three important directions. The first is the 3D structural determination of noncrystalline materials, which includes the localization of the defects and strain field inside nanocrystals, and quantitative 3D imaging of disordered materials such as nanoparticles and biomaterials. The second is the 3D imaging of frozen-hydrated whole cells at a resolution of 10 nm or better. A main thrust is to localize specific multiprotein complexes inside cells. The third is the potential of imaging single large protein complexes using extremely intense and ultrashort X-ray pulses. In this article, we review the principles of this methodology, summarize recent developments in each of the three directions, and illustrate a few examples.

Nano-structuring of multi-layer material by single x-ray vortex pulse with femtosecond duration

NASA Astrophysics Data System (ADS)

Kohmura, Yoshiki; Zhakhovsky, Vasily; Takei, Dai; Suzuki, Yoshio; Takeuchi, Akihisa; Inoue, Ichiro; Inubushi, Yuichi; Inogamov, Nail; Ishikawa, Tetsuya; Yabashi, Makina

2018-03-01

A narrow zero-intensity spot arising from an x-ray vortex has huge potential for future applications such as nanoscopy and nanofabrication. We here present an X-ray Free Electron Laser (XFEL) experiment with a focused vortex wavefront which generated high aspect ratio nanoneedles on a Cr/Au multi-layer (ML) specimen. A sharp needle with a typical width and height of 310 and 600 nm was formed with a high occurrence rate at the center of a 7.71 keV x-ray vortex on this ML specimen, respectively. The observed width exceeds the diffraction limit, and the smallest structures ever reported using an intense-XFEL ablation were fabricated. We found that the elemental composition of the nanoneedles shows a significant difference from that of the unaffected area of Cr/Au ML. All these results are well explained by the molecular dynamics simulations, leading to the elucidation of the needle formation mechanism on an ultra-fast timescale.

X-Ray Sum Frequency Diffraction for Direct Imaging of Ultrafast Electron Dynamics

NASA Astrophysics Data System (ADS)

Rouxel, Jérémy R.; Kowalewski, Markus; Bennett, Kochise; Mukamel, Shaul

2018-06-01

X-ray diffraction from molecules in the ground state produces an image of their charge density, and time-resolved x-ray diffraction can thus monitor the motion of the nuclei. However, the density change of excited valence electrons upon optical excitation can barely be monitored with regular diffraction techniques due to the overwhelming background contribution of the core electrons. We present a nonlinear x-ray technique made possible by novel free electron laser sources, which provides a spatial electron density image of valence electron excitations. The technique, sum frequency generation carried out with a visible pump and a broadband x-ray diffraction pulse, yields snapshots of the transition charge densities, which represent the electron density variations upon optical excitation. The technique is illustrated by ab initio simulations of transition charge density imaging for the optically induced electronic dynamics in a donor or acceptor substituted stilbene.

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

Pathak, S.; Li, N.; Maeder, X.

We investigated the mechanical response of physical vapor deposited Cu–TiN nanolayered composites of varying layer thicknesses from 5 nm to 200 nm. Both the Cu and TiN layers were found to consist of single phase nanometer sized grains. The grain sizes in the Cu and TiN layers, measured using transmission electron microscopy and X-ray diffraction, were found to be comparable to or smaller than their respective layer thicknesses. Indentation hardness testing revealed that the hardness of such nanolayered composites exhibits a weak dependence on the layer thickness but is more correlated to their grain size.

Preparation of CuO nanoparticles by laser ablation in liquid

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

Abdulateef, Sinan A., E-mail: sinan1974@yahoo.com; MatJafri, M. Z.; Omar, A. F., E-mail: thinker-academy@yahoo.com

2016-07-06

Colloidal Cu nanoparticles (NPs) were synthesized by pulsed Nd:YAG laser ablation in acetone. Cu NPs were converted into CuO. The size and optical properties of these NPs were characterized using an UV/Vis spectrophotometer, transmission electron microscopy, and X-ray diffraction. Cu NPs were spherical, and their mean diameter in acetone was 8 nm–10 nm. Optical extinction immediately after the ablation showed surface Plasmon resonance peaks at 602 nm. The color of Cu NPs in acetone was green and stable even after a long time.

Structural, morphological and optical properties of chromium oxide nanoparticles

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

Babukutty, Blessy; Parakkal, Fasalurahman; Nair, Swapna S., E-mail: swapna.s.nair@gmail.com

2015-06-24

Chromium oxide nanoparticles are synthesized by reduction route from chloride precursors with surfactant, trioctylphosphine oxide (TOPO). Structural and morphological characterization are analyzed using X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM). Transmission Electron micrographs show that the average grain size lies in the range 5nm to 10nm. Optical characterization has been done by UV-VIS spectrophotometer. Distinct optical absorptions of Cr{sup 3+} ions show hinting towards the presence of Cr{sub 2}O{sub 3}. Presence of oxygen is also confirmed from Electron Energy Loss Spectroscopy (EELS) studies.

Interaction between U/UO2 bilayers and hydrogen studied by in-situ X-ray diffraction

NASA Astrophysics Data System (ADS)

Darnbrough, J. E.; Harker, R. M.; Griffiths, I.; Wermeille, D.; Lander, G. H.; Springell, R.

2018-04-01

This paper reports experiments investigating the reaction of H2 with uranium metal-oxide bilayers. The bilayers consist of ≤ 100 nm of epitaxial α-U (grown on a Nb buffer deposited on sapphire) with a UO2 overlayer of thicknesses of between 20 and 80 nm. The oxides were made either by depositing via reactive magnetron sputtering, or allowing the uranium metal to oxidise in air at room temperature. The bilayers were exposed to hydrogen, with sample temperatures between 80 and 200 C, and monitored via in-situ x-ray diffraction and complimentary experiments conducted using Scanning Transmission Electron Microscopy - Electron Energy Loss Spectroscopy (STEM-EELS). Small partial pressures of H2 caused rapid consumption of the U metal and lead to changes in the intensity and position of the diffraction peaks from both the UO2 overlayers and the U metal. There is an orientational dependence in the rate of U consumption. From changes in the lattice parameter we deduce that hydrogen enters both the oxide and metal layers, contracting the oxide and expanding the metal. The air-grown oxide overlayers appear to hinder the H2-reaction up to a threshold dose, but then on heating from 80 to 140 C the consumption is more rapid than for the as-deposited overlayers. STEM-EELS establishes that the U-hydride layer lies at the oxide-metal interface, and that the initial formation is at defects or grain boundaries, and involves the formation of amorphous and/or nanocrystalline UH3. This explains why no diffraction peaks from UH3 are observed.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens.

PubMed

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10(-2) Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Development of an adaptable coherent x-ray diffraction microscope with the emphasis on imaging hydrated specimens

NASA Astrophysics Data System (ADS)

Nam, Daewoong; Park, Jaehyun; Gallagher-Jones, Marcus; Shimada, Hiroki; Kim, Sangsoo; Kim, Sunam; Kohmura, Yoshiki; Ishikawa, Tetsuya; Song, Changyong

2013-11-01

This paper describes the development of a versatile coherent x-ray diffraction microscope capable of imaging biological specimens in solution. The microscope is a flexible platform accommodating various conditions, from low vacuum (10-2 Pa) to helium gas filled ambient pressure. This flexibility greatly expands the application area, from in situ materials science to biology systems in their native state, by significantly relaxing restrictions to the sample environment. The coherent diffraction microscope has been used successfully to image a yeast cell immersed in buffer solution. We believe that the design of this coherent diffraction microscope can be directly adapted to various platforms such as table top soft x-ray laser, synchrotron x-ray sources, and x-ray free electron laser with minor relevant adjustments.

Thin Film Research. Volume 1

DTIC Science & Technology

1985-05-30

Order (FECO) ......... 23 3. X -Ray Diffraction ............................... 26 4. Transmission Electron Microscopy (TEM) ............... 26 5...remained amorphous after bombardment, as evidenced by X - ray diffraction, and showed no other changes. 0 (2) For Sb203, the crystallite size was reduced...main effect on MgF2 was the reduction in crystallite size. The films were too thir. for meaningful x - ray diffraction analysis. Durability and

X-Ray Diffraction and the Discovery of the Structure of DNA

ERIC Educational Resources Information Center

Crouse, David T.

2007-01-01

A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

2000-01-01

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

Hard X-ray polarizer to enable simultaneous three-dimensional nanoscale imaging of magnetic structure and lattice strain

DOE PAGES

Logan, Jonathan; Harder, Ross; Li, Luxi; ...

2016-01-01

Recent progress in the development of dichroic Bragg coherent diffractive imaging, a new technique for simultaneous three-dimensional imaging of strain and magnetization at the nanoscale, is reported. This progress includes the installation of a diamond X-ray phase retarder at beamline 34-ID-C of the Advanced Photon Source. Here, the performance of the phase retarder for tuning X-ray polarization is demonstrated with temperature-dependent X-ray magnetic circular dichroism measurements on a gadolinium foil in transmission and on a Gd 5Si 2Ge 2crystal in diffraction geometry with a partially coherent, focused X-ray beam. Feasibility tests for dichroic Bragg coherent diffractive imaging are presented. Thesemore » tests include (1) using conventional Bragg coherent diffractive imaging to determine whether the phase retarder introduces aberrations using a nonmagnetic gold nanocrystal as a control sample, and (2) collecting coherent diffraction patterns of a magnetic Gd 5Si 2Ge 2nanocrystal with left- and right-circularly polarized X-rays. Future applications of dichroic Bragg coherent diffractive imaging for the correlation of strain and lattice defects with magnetic ordering and inhomogeneities are considered.« less

Photoluminescence properties of LiF bismuth silicate glass

NASA Astrophysics Data System (ADS)

Krishnan, M. Laya; Kumar, V. V. Ravi Kanth

2018-04-01

The sample (60-X) Bi2O3-30SiO2-XLiF where X=10, 15, 25 were prepared by conventional melt quenching method. X-ray diffraction pattern conformed the amorphous nature of the prepared sample and a broad peak at 2θ=30°. The Raman spectra confirmed that the Bi can exist both network former (BiO3 pyramidal) and network modifier (BiO6 octahedral)in the glass matrix. The samples showing broad absorption at 470nm is due to the presence of Bi2+ ions, because of increasing optical basicity the absorption edge of the sample is blue shifted. The photoluminescence spectra of the glass under 350nm excitation are showing two main peaks at 430nm and 630 nm due to Bi3+ and Bi2+ respectively and 25 LBS glass showing yellow, 15LBS showing near bluish white and 10LBS showing blue luminescence. The color purity and correlated color temperature are also calculated.

Pt-B System Revisited: Pt2B, a New Structure Type of Binary Borides. Ternary WAl12-Type Derivative Borides.

PubMed

Sologub, Oksana; Salamakha, Leonid; Rogl, Peter; Stöger, Berthold; Bauer, Ernst; Bernardi, Johannes; Giester, Gerald; Waas, Monika; Svagera, Robert

2015-11-16

On the basis of a detailed study applying X-ray single-crystal and powder diffraction, differential scanning calorimetry, and scanning electron microscopy analysis, it was possible to resolve existing uncertainties in the Pt-rich section (≥65 atom % Pt) of the binary Pt-B phase diagram above 600 °C. The formation of a unique structure has been observed for Pt2B [X-ray single-crystal data: space group C2/m, a = 1.62717(11) nm, b = 0.32788(2) nm, c = 0.44200(3) nm, β = 104.401(4)°, RF2 = 0.030]. Within the homogeneity range of "Pt3B", X-ray powder diffraction phase analysis prompted two structural modifications as a function of temperature. The crystal structure of "hT-Pt3B" complies with the hitherto reported structure of anti-MoS2 [space group P63/mmc, a = 0.279377(2) nm, c = 1.04895(1) nm, RF = 0.075, RI = 0.090]. The structure of the new "[Formula: see text]T-Pt3B" is still unknown. The formation of previously reported Pt∼4B has not been confirmed from binary samples. Exploration of the Pt-rich section of the Pt-Cu-B system at 600 °C revealed a new ternary compound, Pt12CuB6-y [X-ray single-crystal data: space group Im3̅, a = 0.75790(2) nm, y = 3, RF2 = 0.0129], which exhibits the filled WAl12-type structure accommodating boron in the interstitial trigonal-prismatic site 12e. The isotypic platinum-aluminum-boride was synthesized and studied. The solubility of copper in binary platinum borides has been found to attain ∼7 atom % Cu for Pt2B but to be insignificant for "[Formula: see text]T-Pt3B". The architecture of the new Pt2B structure combines puckered layers of boron-filled and empty [Pt6] octahedra (anti-CaCl2-type fragment) alternating along the x axis with a double layer of boron-semifilled [Pt6] trigonal prisms interbedded with a layer of empty tetrahedra and tetragonal pyramids (B-deficient α-T[Formula: see text]I fragment). Assuming boron vacancies ordering (space group R3), the Pt12CuB6-y structure exhibits serpentine-like columns of edge-connected boron-filled [Pt6] trigonal prisms running infinitely along the z axis and embedding the icosahedrally coordinated Cu atom. Pt2B, (Pt1-yCuy)2B (y = 0.045), and Pt12CuB6-y (y = 3) behave metallically, as revealed by temperature-dependent electrical resistivity measurements.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

DOE PAGES

Cha, W.; Ulvestad, A.; Allain, M.; ...

2016-11-23

Here, we present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We also demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Furthermore, variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Synchrotron X-Ray Diffraction Analysis of Meteorites in Thin Section: Preliminary Results

NASA Technical Reports Server (NTRS)

Treiman, A. H.; Lanzirotti, A.; Xirouchakis, D.

2004-01-01

X-ray diffraction is the pre-eminent technique for mineral identification and structure determination, but is difficult to apply to grains in thin section, the standard meteorite preparation. Bright focused X-ray beams from synchrotrons have been used extensively in mineralogy and have been applied to extraterrestrial particles. The intensity and small spot size achievable in synchrotron X-ray beams makes them useful for study of materials in thin sections. Here, we describe Synchrotron X-ray Diffraction (SXRD) in thin section as done at the National Synchrotron Light Source, and cite examples of its value for studies of meteorites in thin section.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging

NASA Astrophysics Data System (ADS)

Cha, W.; Ulvestad, A.; Allain, M.; Chamard, V.; Harder, R.; Leake, S. J.; Maser, J.; Fuoss, P. H.; Hruszkewycz, S. O.

2016-11-01

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Three Dimensional Variable-Wavelength X-Ray Bragg Coherent Diffraction Imaging.

PubMed

Cha, W; Ulvestad, A; Allain, M; Chamard, V; Harder, R; Leake, S J; Maser, J; Fuoss, P H; Hruszkewycz, S O

2016-11-25

We present and demonstrate a formalism by which three-dimensional (3D) Bragg x-ray coherent diffraction imaging (BCDI) can be implemented without moving the sample by scanning the energy of the incident x-ray beam. This capability is made possible by introducing a 3D Fourier transform that accounts for x-ray wavelength variability. We demonstrate the approach by inverting coherent Bragg diffraction patterns from a gold nanocrystal measured with an x-ray energy scan. Variable-wavelength BCDI will expand the breadth of feasible in situ 3D strain imaging experiments towards more diverse materials environments, especially where sample manipulation is difficult.

Mössbauer study of Cu1-xZnxFe2O4 catalytic materials

NASA Astrophysics Data System (ADS)

Koleva, K.; Velinov, N.; Tsoncheva, T.; Mitov, I.

2014-04-01

Copper zinc ferrites (Cu1-xZnxFe2O4) with different composition (x = 1; 0.2; 0.5; 0.8) were prepared by conventional thermal method. Formation of well crystallized ferrite phase with cubic structure and crystallites size of about 19.08-24.39 nm was observed by Powder X-ray diffraction and Mössbauer spectroscopy. The ferrite materials were tested as catalysts in methanol decomposition to CO and H2. A strong dependence of the catalytic behaviour of Cu1-xZnxFe2O4 ferrites of their composition and the phase transformations which occurred under the reaction medium was established.

In-situ X-ray diffraction system using sources and detectors at fixed angular positions

DOEpatents

Gibson, David M [Voorheesville, NY; Gibson, Walter M [Voorheesville, NY; Huang, Huapeng [Latham, NY

2007-06-26

An x-ray diffraction technique for measuring a known characteristic of a sample of a material in an in-situ state. The technique includes using an x-ray source for emitting substantially divergent x-ray radiation--with a collimating optic disposed with respect to the fixed source for producing a substantially parallel beam of x-ray radiation by receiving and redirecting the divergent paths of the divergent x-ray radiation. A first x-ray detector collects radiation diffracted from the sample; wherein the source and detector are fixed, during operation thereof, in position relative to each other and in at least one dimension relative to the sample according to a-priori knowledge about the known characteristic of the sample. A second x-ray detector may be fixed relative to the first x-ray detector according to the a-priori knowledge about the known characteristic of the sample, especially in a phase monitoring embodiment of the present invention.

Catalytic Biomineralization of Fluorescent Calcite by the Thermophilic Bacterium Geobacillus thermoglucosidasius▿

PubMed Central

Yoshida, Naoto; Higashimura, Eiji; Saeki, Yuichi

2010-01-01

The thermophilic Geobacillus bacterium catalyzed the formation of 100-μm hexagonal crystals at 60°C in a hydrogel containing sodium acetate, calcium chloride, and magnesium sulfate. Under fluorescence microscopy, crystals fluoresced upon excitation at 365 ± 5, 480 ± 20, or 545 ± 15 nm. X-ray diffraction indicated that the crystals were magnesium-calcite in calcite-type calcium carbonate. PMID:20851984

Response of Gd 2 Ti 2 O 7 and La 2 Ti 2 O 7 to swift-heavy ion irradiation and annealing

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

Park, Sulgiye; Lang, Maik; Tracy, Cameron L.

2015-07-01

Swift heavy ion (2 GeV 181Ta) irradiation-induced amorphization and temperature-induced recrystallization of cubic pyrochlore Gd2Ti2O7 (Fd3¯m) are compared with the response of a compositionally-similar material with a monoclinic-layered perovskite-type structure, La2Ti2O7 (P21). The averaged electronic energy loss, dE/dx, was 37 keV/nm and 35 keV/nm in Gd2Ti2O7 and La2Ti2O7, respectively. Systematic analysis of the structural modifications was completed using transmission electron microscopy, synchrotron X-ray diffraction, Raman spectroscopy, and small-angle X-ray scattering. Increasing ion-induced amorphization with increasing ion fluence was evident in the X-ray diffraction patterns of both compositions by a reduction in the intensity of the diffraction maxima concurrent with themore » growth in intensity of a broad diffuse scattering halo. Transmission electron microscopy analysis showed complete amorphization within ion tracks (diameter: ~10 nm) for the perovskite-type material; whereas a concentric, core–shell morphology was evident in the ion tracks of the pyrochlore, with an outer shell of disordered yet still crystalline material with the fluorite structure surrounding an amorphous track core (diameter: ~9 nm). The radiation response of both titanate oxides with the same stoichiometry can be understood in terms of differences in their structures and compositions. While the radiation damage susceptibility of pyrochlore A2B2O7 materials decreases as a function of the cation radius ratio rA/rB, the current study correlates this behavior with the stability field of monoclinic structures, where rLa/rTi > rGd/rTi. Isochronal annealing experiments of the irradiated materials showed complete recrystallization of La2Ti2O7 at 775 °C and of Gd2Ti2O7 at 850 °C. The annealing behavior is discussed in terms of enhanced damage recovery in La2Ti2O7, compared to the pyrochlore compounds Gd2Ti2O7. The difference in the recrystallization behavior may be related to structural constraints, i.e., reconstructing a low symmetry versus a high symmetry phase.« less

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

NASA Astrophysics Data System (ADS)

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

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

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions

NASA Astrophysics Data System (ADS)

Hruszkewycz, S. O.; Harder, R.; Xiao, X.; Fuoss, P. H.

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

The effect of exit beam phase aberrations on parallel beam coherent x-ray reconstructions.

PubMed

Hruszkewycz, S O; Harder, R; Xiao, X; Fuoss, P H

2010-12-01

Diffraction artifacts from imperfect x-ray windows near the sample are an important consideration in the design of coherent x-ray diffraction measurements. In this study, we used simulated and experimental diffraction patterns in two and three dimensions to explore the effect of phase imperfections in a beryllium window (such as a void or inclusion) on the convergence behavior of phasing algorithms and on the ultimate reconstruction. A predictive relationship between beam wavelength, sample size, and window position was derived to explain the dependence of reconstruction quality on beryllium defect size. Defects corresponding to this prediction cause the most damage to the sample exit wave and induce signature error oscillations during phasing that can be used as a fingerprint of experimental x-ray window artifacts. The relationship between x-ray window imperfection size and coherent x-ray diffractive imaging reconstruction quality explored in this work can play an important role in designing high-resolution in situ coherent imaging instrumentation and will help interpret the phasing behavior of coherent diffraction measured in these in situ environments.

Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals

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

Frank, Matthias; Carlson, David B.; Hunter, Mark

2014-02-28

Here we present femtosecond x-ray diffraction patterns from two-dimensional (2-D) protein crystals using an x-ray free electron laser (XFEL). To date it has not been possible to acquire x-ray diffraction from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permits a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy methodology at the Linac Coherent Light Source, we observed Bragg diffraction to better than 8.5 Å resolution for two different 2-D protein crystal samples that were maintained at room temperature. These proof-of-principle results show promisemore » for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.« less

Alternating current magnetic susceptibility and heat dissipation by Mn{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} nanoparticles for hyperthermia treatment

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

Kondo, T.; Mori, K.; Hachisu, M.

2015-05-07

Mn-Zn ferrite, Mn{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} nanoparticles encapsulated in amorphous SiO{sub 2} were prepared using our original wet chemical method. X-ray diffraction patterns confirmed that the diameters of these particles were within 7–30 nm. Magnetization measurements for various sample compositions revealed that the saturation magnetization (M{sub s}) of 7 nm particles was maximum for the x = 0.2 sample. AC magnetic susceptibility measurements were performed for Mn{sub 0.8}Zn{sub 0.2}Fe{sub 2}O{sub 4} (x = 0.2) samples with 13–30 nm particles. The peak of the imaginary part of the magnetic susceptibility χ″ shifted to higher temperatures as the particle size increased. An AC field was found to causemore » the increase in temperature, with the 18 nm particles exhibiting the highest temperature increase, as expected. In addition, in vitro experiments were carried out to study the hyperthermia effects of Mn{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (x = 0.2, 18 nm) particles on human cancer cells.« less

Influence of gamma ray irradiation on stoichiometry of hydrothermally synthesized bismuth telluride nanoparticles

NASA Astrophysics Data System (ADS)

Abishek, N. S.; Naik, K. Gopalakrishna

2018-05-01

Bismuth telluride (Bi2Te3) nanoparticles were synthesized by the hydrothermal method at 200 °C for 24 h. The synthesized Bi2Te3 nanoparticles were irradiated with gamma rays at doses of 50 kGy and 100 kGy. The structural characterization of the pre-irradiated and post-irradiated samples was carried out by X-ray diffraction technique and was found to have rhombohedral phase having R3 ¯m (166) space group. The X-ray diffraction peaks were found to shift towards lower diffraction angle with gamma ray irradiation. The morphologies and compositions of the grown Bi2Te3 nanoparticles were studied using Field Emission Scanning Electron Microscope and X-ray energy dispersive analysis, respectively. The possible cause for the shift in the X-ray diffraction peaks with gamma ray irradiation has been discussed in the present work.

High Power Optical Coatings by Atomic Layer Deposition and Signatures of Laser-Induced Damage

DTIC Science & Technology

2012-08-28

diffraction angle 0 into crystal lattice spacing d by the Bragg condition, mX = 2d sin 0. Here X is the x - ray wavelength... angle x - ray diffraction (GAXRD) measurements, which were made at a fixed shallow incidence angle of 0.5°. Detector scans were done to measure the...was finished with 200 hafnia cycles m the fmal half period rather than 400. Crystallinity was measured by x - ray diffraction (XRD) with

Materials identification using a small-scale pixellated x-ray diffraction system

NASA Astrophysics Data System (ADS)

O'Flynn, D.; Crews, C.; Drakos, I.; Christodoulou, C.; Wilson, M. D.; Veale, M. C.; Seller, P.; Speller, R. D.

2016-05-01

A transmission x-ray diffraction system has been developed using a pixellated, energy-resolving detector (HEXITEC) and a small-scale, mains operated x-ray source (Amptek Mini-X). HEXITEC enables diffraction to be measured without the requirement of incident spectrum filtration, or collimation of the scatter from the sample, preserving a large proportion of the useful signal compared with other diffraction techniques. Due to this efficiency, sufficient molecular information for material identification can be obtained within 5 s despite the relatively low x-ray source power. Diffraction data are presented from caffeine, hexamine, paracetamol, plastic explosives and narcotics. The capability to determine molecular information from aspirin tablets inside their packaging is demonstrated. Material selectivity and the potential for a sample classification model is shown with principal component analysis, through which each different material can be clearly resolved.

Dynamic X-ray diffraction sampling for protein crystal positioning

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

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE PAGES

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; ...

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

PubMed Central

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; Kissick, David J.; Zhang, Shijie; Newman, Justin A.; Sheedlo, Michael J.; Chowdhury, Azhad U.; Fischetti, Robert F.; Das, Chittaranjan; Buzzard, Gregery T.; Bouman, Charles A.; Simpson, Garth J.

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations. PMID:28009558

Dynamic X-ray diffraction sampling for protein crystal positioning.

PubMed

Scarborough, Nicole M; Godaliyadda, G M Dilshan P; Ye, Dong Hye; Kissick, David J; Zhang, Shijie; Newman, Justin A; Sheedlo, Michael J; Chowdhury, Azhad U; Fischetti, Robert F; Das, Chittaranjan; Buzzard, Gregery T; Bouman, Charles A; Simpson, Garth J

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.

Magnetic topology of Co-based inverse opal-like structures

NASA Astrophysics Data System (ADS)

Grigoryeva, N. A.; Mistonov, A. A.; Napolskii, K. S.; Sapoletova, N. A.; Eliseev, A. A.; Bouwman, W.; Byelov, D. V.; Petukhov, A. V.; Chernyshov, D. Yu.; Eckerlebe, H.; Vasilieva, A. V.; Grigoriev, S. V.

2011-08-01

The magnetic and structural properties of a cobalt inverse opal-like crystal have been studied by a combination of complementary techniques ranging from polarized neutron scattering and superconducting quantum interference device (SQUID) magnetometry to x-ray diffraction. Microradian small-angle x-ray diffraction shows that the inverse opal-like structure (OLS) synthesized by the electrochemical method fully duplicates the three-dimensional net of voids of the template artificial opal. The inverse OLS has a face-centered cubic (fcc) structure with a lattice constant of 640±10 nm and with a clear tendency to a random hexagonal close-packed structure along the [111] axes. Wide-angle x-ray powder diffraction shows that the atomic cobalt structure is described by coexistence of 95% hexagonal close-packed and 5% fcc phases. The SQUID measurements demonstrate that the inverse OLS film possesses easy-plane magnetization geometry with a coercive field of 14.0 ± 0.5 mT at room temperature. The detailed picture of the transformation of the magnetic structure under an in-plane applied field was detected with the help of small-angle diffraction of polarized neutrons. In the demagnetized state the magnetic system consists of randomly oriented magnetic domains. A complex magnetic structure appears upon application of the magnetic field, with nonhomogeneous distribution of magnetization density within the unit element of the OLS. This distribution is determined by the combined effect of the easy-plane geometry of the film and the crystallographic geometry of the opal-like structure with respect to the applied field direction.

Ba2Mg(BO3)2:Bi3+ - A new phosphor with ultraviolet light emission

NASA Astrophysics Data System (ADS)

Lakshminarasimhan, N.; Jayakiruba, S.; Prabhavathi, K.

2017-10-01

Ultraviolet light emission was observed in a new Ba2Mg(BO3)2:Bi3+ phosphor. Bi3+ substitution for Ba2+ in the lattice was supplemented with K+ to maintain the charge neutrality. The samples of the formula Ba2-2xBixKxMg(BO3)2 [x = 0, 0.001, 0.01, 0.02, and 0.05] synthesized by solid state reaction were characterized using powder X-ray diffraction for their phase formation. Raman and diffuse reflectance UV-Vis spectroscopic techniques were used to obtain information on the vibrational modes and optical properties, respectively. The room temperature photoluminescence measurements revealed an ultraviolet emission at 370 nm when excited using 304 nm wavelength and the Stokes shift is 5868 cm-1.

Fixture for supporting and aligning a sample to be analyzed in an x-ray diffraction apparatus

DOEpatents

Green, L.A.; Heck, J.L. Jr.

1985-04-23

A fixture is provided for supporting and aligning small samples of material on a goniometer for x-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the x-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an x-ray diffraction apparatus previously limited to the analysis of much larger samples.

Fixture for supporting and aligning a sample to be analyzed in an X-ray diffraction apparatus

DOEpatents

Green, Lanny A.; Heck, Jr., Joaquim L.

1987-01-01

A fixture is provided for supporting and aligning small samples of material on a goniometer for X-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the X-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an X-ray diffraction apparatus previously limited to the analysis of much larger samples.

Size-controlled synthesis of ZnO quantum dots in microreactors

NASA Astrophysics Data System (ADS)

Schejn, Aleksandra; Frégnaux, Mathieu; Commenge, Jean-Marc; Balan, Lavinia; Falk, Laurent; Schneider, Raphaël

2014-04-01

In this paper, we report on a continuous-flow microreactor process to prepare ZnO quantum dots (QDs) with widely tunable particle size and photoluminescence emission wavelengths. X-ray diffraction, electron diffraction, UV-vis, photoluminescence and transmission electron microscopy measurements were used to characterize the synthesized ZnO QDs. By varying operating conditions (temperature, flow rate) or the capping ligand, ZnO QDs with diameters ranging from 3.6 to 5.2 nm and fluorescence maxima from 500 to 560 nm were prepared. Results obtained show that low reaction temperatures (20 or 35 °C), high flow rates and the use of propionic acid as a stabilizing agent are favorable for the production of ZnO QDs with high photoluminescence quantum yields (up to 30%).

Fabrication of 200 nanometer period centimeter area hard x-ray absorption gratings by multilayer deposition

PubMed Central

Lynch, S K; Liu, C; Morgan, N Y; Xiao, X; Gomella, A A; Mazilu, D; Bennett, E E; Assoufid, L; de Carlo, F; Wen, H

2012-01-01

We describe the design and fabrication trials of x-ray absorption gratings of 200 nm period and up to 100:1 depth-to-period ratios for full-field hard x-ray imaging applications. Hard x-ray phase-contrast imaging relies on gratings of ultra-small periods and sufficient depth to achieve high sensitivity. Current grating designs utilize lithographic processes to produce periodic vertical structures, where grating periods below 2.0 μm are difficult due to the extreme aspect ratios of the structures. In our design, multiple bilayers of x-ray transparent and opaque materials are deposited on a staircase substrate, and mostly on the floor surfaces of the steps only. When illuminated by an x-ray beam horizontally, the multilayer stack on each step functions as a micro-grating whose grating period is the thickness of a bilayer. The array of micro-gratings over the length of the staircase works as a single grating over a large area when continuity conditions are met. Since the layers can be nanometers thick and many microns wide, this design allows sub-micron grating periods and sufficient grating depth to modulate hard x-rays. We present the details of the fabrication process and diffraction profiles and contact radiography images showing successful intensity modulation of a 25 keV x-ray beam. PMID:23066175

Structural and magnetic properties of chromium doped zinc ferrite

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

Sebastian, Rintu Mary; Thankachan, Smitha; Xavier, Sheena

2014-01-28

Zinc chromium ferrites with chemical formula ZnCr{sub x}Fe{sub 2−x}O{sub 4} (x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.0) were prepared by Sol - Gel technique. The structural as well as magnetic properties of the synthesized samples have been studied and reported here. The structural characterizations of the samples were analyzed by using X – Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscope (SEM), and Transmission Electron Microscope (TEM). The single phase spinel cubic structure of all the prepared samples was tested by XRD and FTIR. The particle size was observed to decrease from 18.636 nm to 6.125more » nm by chromium doping and induced a tensile strain in all the zinc chromium mixed ferrites. The magnetic properties of few samples (x = 0.0, 0.4, 1.0) were investigated using Vibrating Sample Magnetometer (VSM)« less

Thermoluminescence (TL) properties and x-ray diffraction (XRD) analysis of high purity CaSO{sub 4}:Dy TL material

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

Kamarudin, Nadira; Abdullah, Wan Saffiey Wan; Dollah, Mohd Taufik

2014-09-03

This paper presents the characterization and TL properties of dysprosium (Dy) doped calcium sulfate (CaSO{sub 4}) TL material produced by co-precipitation technique with 0.5mol% concentration of dopant. The morphology of the produced TL material was studied using scanning electron microscope (SEM) and the micrograph shows that rectangular parallelepiped shaped crystal with the average of 150 μm in length were produced. The crystallinity of the produced powder was studied using x-ray powder diffraction (XRD). The XRD spectra show that the TL material produced is high purity anhydrite CaSO{sub 4} with average crystallite size of 74 nm with orthorhombic crystal system. Themore » TL behavior of produced CaSO{sub 4}:Dy was studied using a TLD reader after exposure to gamma ray by Co{sup 60} source with the doses of 1,5 and 10 Gy. The glow curve shows linear response with glow peak around 230°C which is desired development in the field of radiation dosimetry.« less

JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

Treesearch

Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

2006-01-01

X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

DOE PAGES

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; ...

2015-08-11

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessarymore » to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. In addition, the features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

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

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called `fixed-target' sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary tomore » fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15µm) loaded into the chips yielded a complete, high-resolution (<1.6Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs.« less

A high-transparency, micro-patternable chip for X-ray diffraction analysis of microcrystals under native growth conditions

PubMed Central

Murray, Thomas D.; Lyubimov, Artem Y.; Ogata, Craig M.; Vo, Huy; Uervirojnangkoorn, Monarin; Brunger, Axel T.; Berger, James M.

2015-01-01

Microcrystals present a significant impediment to the determination of macromolecular structures by X-ray diffraction methods. Although microfocus synchrotron beamlines and X-ray free-electron lasers (XFELs) can enable the collection of interpretable diffraction data from microcrystals, there is a need for efficient methods of harvesting small volumes (<2 µl) of microcrystals grown under common laboratory formats and delivering them to an X-ray beam source under native growth conditions. One approach that shows promise in overcoming the challenges intrinsic to microcrystal analysis is to pair so-called ‘fixed-target’ sample-delivery devices with microbeam-based X-ray diffraction methods. However, to record weak diffraction patterns it is necessary to fabricate devices from X-ray-transparent materials that minimize background scattering. Presented here is the design of a new micro-diffraction device consisting of three layers fabricated from silicon nitride, photoresist and polyimide film. The chip features low X-ray scattering and X-ray absorption properties, and uses a customizable blend of hydrophobic and hydrophilic surface patterns to help localize microcrystals to defined regions. Microcrystals in their native growth conditions can be loaded into the chips with a standard pipette, allowing data collection at room temperature. Diffraction data collected from hen egg-white lysozyme microcrystals (10–15 µm) loaded into the chips yielded a complete, high-resolution (<1.6 Å) data set sufficient to determine a high-quality structure by molecular replacement. The features of the chip allow the rapid and user-friendly analysis of microcrystals grown under virtually any laboratory format at microfocus synchrotron beamlines and XFELs. PMID:26457423

Influence of Cu-Ti thin film surface properties on antimicrobial activity and viability of living cells.

PubMed

Wojcieszak, Damian; Kaczmarek, Danuta; Antosiak, Aleksandra; Mazur, Michal; Rybak, Zbigniew; Rusak, Agnieszka; Osekowska, Malgorzata; Poniedzialek, Agata; Gamian, Andrzej; Szponar, Bogumila

2015-11-01

The paper describes properties of thin-film coatings based on copper and titanium. Thin films were prepared by co-sputtering of Cu and Ti targets in argon plasma. Deposited coatings consist of 90at.% of Cu and 10at.% of Ti. Characterization of the film was made on the basis of investigations of microstructure and physicochemical properties of the surface. Methods such as scanning electron microscopy, x-ray microanalysis, x-ray diffraction, x-ray photoelectron spectroscopy, atomic force microscopy, optical profilometry and wettability measurements were used to assess the properties of deposited thin films. An impact of Cu-Ti coating on the growth of selected bacteria and viability of the living cells (line L929, NCTC clone 929) was described in relation to the structure, surface state and wettability of the film. It was found that as-deposited films were amorphous. However, in such surroundings the nanocrystalline grains of 10-15nm and 25-35nm size were present. High surface active area with a roughness of 8.9nm, had an effect on receiving relatively high water contact angle value (74.1°). Such wettability may promote cell adhesion and result in an increase of the probability of copper ion transfer from the film surface into the cell. Thin films revealed bactericidal and fungicidal effects even in short term-contact. High activity of prepared films was directly related to high amount (ca. 51 %) of copper ions at 1+ state as x-ray photoelectron spectroscopy results have shown. Copyright © 2015 Elsevier B.V. All rights reserved.

Effect of interparticle interactions on size determination of zirconia and silica based systems – A comparison of SAXS, DLS, BET, XRD and TEM

PubMed Central

Pabisch, Silvia; Feichtenschlager, Bernhard; Kickelbick, Guido; Peterlik, Herwig

2012-01-01

The aim of this work is a systematic comparison of size characterisation methods for two completely different model systems of oxide nanoparticles, i.e. amorphous spherical silica and anisotropic facet-shaped crystalline zirconia. Size and/or size distribution were determined in a wide range from 5 to 70 nm using small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), nitrogen sorption (BET), X-ray diffraction (XRD) and transmission electron microscopy (TEM). A nearly perfect coincidence was observed only for SAXS and TEM for both types of particles. For zirconia nanoparticles considerable differences between different measurement methods were observed. PMID:22347721

Synthesis and characterization of rare-earth-doped calcium tungstate nanocrystals

NASA Astrophysics Data System (ADS)

Suneeta, P.; Rajesh, Ch.; Ramana, M. V.

2018-02-01

In this paper, we report synthesis and characterization of rare-earth-ion-doped calcium tungstate (CaWO4) nanocrystals (NCs). Rare-earth ions, such as gadolinium (Gd), neodymium (Nd), praseodymium (Pr), samarium (Sm) and holmium (Ho), were successfully doped in the CaWO4 NCs by changing the synthesis conditions. The adopted synthesis route was found to be fast and eco-friendly. Structural characterizations, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and compositional analysis, were performed using energy dispersive analysis of X-rays (EDAX) on as-synthesized NCs. The results indicate the size of the NCs ranging between 47 to 68nm and incorporation of rare-earth ions in CaWO4 NCs.

In situ X-ray ptychography imaging of high-temperature CO{sub 2} acceptor particle agglomerates

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

Høydalsvik, Kristin; Bø Fløystad, Jostein; Esmaeili, Morteza

2014-06-16

Imaging nanoparticles under relevant reaction conditions of high temperature and gas pressure is difficult because conventional imaging techniques, like transmission electron microscopy, cannot be used. Here we demonstrate that the coherent diffractive imaging technique of X-ray ptychography can be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO{sub 2} capture material, was studied at a pressure of one atmosphere in air and in CO{sub 2}, at temperatures exceeding 600 °C. Images with a spatial resolution better than 200 nm were retrieved, and possibilities for improving the experiment are described.

Multislice imaging of integrated circuits by precession X-ray ptychography.

PubMed

Shimomura, Kei; Hirose, Makoto; Takahashi, Yukio

2018-01-01

A method for nondestructively visualizing multisection nanostructures of integrated circuits by X-ray ptychography with a multislice approach is proposed. In this study, tilt-series ptychographic diffraction data sets of a two-layered circuit with a ∼1.4 µm gap at nine incident angles are collected in a wide Q range and then artifact-reduced phase images of each layer are successfully reconstructed at ∼10 nm resolution. The present method has great potential for the three-dimensional observation of flat specimens with thickness on the order of 100 µm, such as three-dimensional stacked integrated circuits based on through-silicon vias, without laborious sample preparation.

Plasma-assisted reduction of silver ions impregnated into a natural zeolite framework

NASA Astrophysics Data System (ADS)

Osonio, Airah P.; Vasquez, Magdaleno R.

2018-02-01

A green, dry, and energy-efficient method for the fabrication of silver-zeolite (AgZ) composite via 13.56 MHz radio-frequency plasma reduction is demonstrated. Impregnation by soaking and ion-exchange deposition were performed to load the silver ions (Ag+) into the sodium-zeolite samples. Characterization was performed by optical emission spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, and Brunauer-Emmett-Teller analyses. Results indicate the successful reduction of Ag+ to its metallic state on the surface of the zeolite with a mean diameter of 165 nm. This plasma-induced reduction technique opens possibilities in several areas including catalysis, adsorption, water treatment, and medicine.

Local structure analysis of diluted magnetic semiconductor Co and Al co-doped ZnO nanoparticles

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

Hyodo, K.; Morimoto, S.; Yamazaki, T.

2016-02-01

In this study, Co and Al ions co-doped ZnO nanoparticles (Zn(Al, Co)O NPs) were prepared by our original chemical preparation method. The obtained samples prepared by this method, were encapsulated in amorphous SiO{sub 2}. X-ray diffraction (XRD) results showed Zn(Al, Co)O NPs had a single-phase nature with hexagonal wurtzite structure. These particle sizes could be controlled to be approximately 30 nm. We investigate the effect that the increase in the carrier has on the magnetization by doping Al to Co-doped ZnO NPs. The local structures were qualitatively analyzed using X-ray absorption fine structure (XAFS) measurements.

Compositional dependence of magnetic anisotropy in chemically synthesized Co3- x Fe x O4 (0 ≤ x ≤ 2)

NASA Astrophysics Data System (ADS)

Hayashi, Kensuke; Yamada, Keisuke; Shima, Mutsuhiro

2018-01-01

Magnetic anisotropy of Co3- x Fe x O4 (CFO, 0 ≤ x ≤ 2) thin-film and powder samples prepared by a sol-gel method has been investigated as a function of Fe composition x. Structural analyses by X-ray diffraction show that CFO powder samples exhibit diffraction peaks associated with the spinel structure when x < 2, while CFO thin-film samples with thickness of 130-510 nm yield the peaks when 0 ≤ x ≤ 2. CFO thin-film samples are highly (111)-oriented with the Lotgering factor greater than 0.9 when 0.6 ≤ x ≤ 1.3. The magnetic anisotropy constant K 1 of CFO powder samples estimated from their room-temperature hysteresis loops yields a minimum when x = 0.9. Relatively large in-plane magnetic anisotropy (K eff = 5.7 × 105 erg/cm3) is observed for the CFO thin-film sample when x = 1.3. With increasing x, the magnetic easy axis of the spinel CFO changes from 〈111〉 to 〈100〉 when x = 0.9.

Effect of fusion mixture treatment on the surface of low grade natural ruby

NASA Astrophysics Data System (ADS)

Sakthivel, R.; Pradhan, K. C.; Nayak, B. B.; Dash, Tapan; Sahu, R. K.; Mishra, B. K.

2017-05-01

Improvement in aesthetic look of low grade natural ruby (gemstone) surface was clearly evident after fusion mixture treatment. Surface impurities of the gemstone were significantly reduced to give it a face lift. The processing consists of heat treatment (1000 °C) of the raw gemstone with fusion mixture (sodium and potassium carbonates), followed by hydrochloric acid digestion (90 °C) and ultrasonic cleaning.Both the untreated and the treated gemstone were characterized by X-ray diffraction, UV-vis spectroscopy (diffuse reflectance),photoluminescence and X-ray photoelectron spectroscopy. The paper consolidates the results of these studies and presents the effect of the typical chemical treatment (stated above) on the low grade natural ruby. While X-ray diffraction study identifies the occurrence of alumina phase in both the treated and the untreated gemstones, the UV-vis spectra exhibit strong characteristic absorption of Cr3+at 400 and 550 nm wavelength for the treated gemstone in contrast to weak absorption observed for the untreated gemstone at such wavelengths, thus showing the beneficial effect of fusion mixture treatment. Peaks observed for the gemstone (for both treated and untreated samples) in the excitation spectra of photoluminescence show a good correlation with observed UV-vis (diffuse reflectance) spectra. Photoluminescence emission spectra of the untreated gemstone show characteristic emission at 695 nm for Cr3+ ion (as in alumina matrix), but its emission intensity significantly reduces after fusion mixture treatment. It is found that the surface of the fusion mixture treated ruby gemstone looks much brighter than the corresponding untreated surface.

Investigation of nanocrystalline zinc chromite obtained by two soft chemical routes

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

Gingasu, Dana; Mindru, Ioana, E-mail: imandru@yahoo.com; Culita, Daniela C.

2014-01-01

Graphical abstract: - Highlights: • Two soft chemical routes to synthesize zinc chromites are described. • Glycine is used as chelating agent (precursor method) and fuel (solution combustion method). • The synthesized chromites have crystallite size in the range of 18–27 nm. • An antiferromagnetic (AFM) transition is observed at about T{sub N} ∼ 18 K. - Abstract: Zinc chromite (ZnCr{sub 2}O{sub 4}) nanocrystalline powders were obtained by two different chemical routes: the precursor method and the solution combustion method involving glycine-nitrates. The complex compound precursors, [ZnCr{sub 2}(NH{sub 2}CH{sub 2}COO){sub 8}]·9H{sub 2}O and [ZnCr{sub 2}(NH{sub 2}CH{sub 2}COOH){sub 4.5}]·(NO{sub 3}){sub 8}·6H{submore » 2}O, were characterized by chemical analysis, infrared spectroscopy (IR), ultraviolet–visible spectroscopy (UV–vis) and thermal analysis. The structure, morphology, surface chemistry and magnetic properties of ZnCr{sub 2}O{sub 4} powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), infrared and Raman spectroscopy (RS), ultraviolet–visible spectroscopy (UV–vis) and magnetic measurements. X-ray diffraction patterns indicated the chromite spinel phase with good crystallinity and an average crystallite size of approximately 18–27 nm. The band gap values ranged between 3.31 and 3.33 eV. The magnetic measurements indicated an antiferromagnetic transition at T{sub N} ∼ 17.5/18 K.« less

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

PubMed

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

2013-04-22

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

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

PubMed Central

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

2014-01-01

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

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

DTIC Science & Technology

2006-11-01

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

Synthesis, magnetic and ethanol gas sensing properties of semiconducting magnetite nanoparticles

NASA Astrophysics Data System (ADS)

Al-Ghamdi, Ahmed A.; Al-Hazmi, Faten; Al-Tuwirqi, R. M.; Alnowaiser, F.; Al-Hartomy, Omar A.; El-Tantawy, Farid; Yakuphanoglu, F.

2013-05-01

The superparamagnetic magnetite (Fe3O4) nanoparticles with an average size of 7 nm were synthesized using a rapid and facile microwave hydrothermal technique. The structure of the magnetite nanoparticles was characterized by X-ray diffraction (X-ray), field effect scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). The prepared Fe3O4 was shown to have a cubic phase of pure magnetite. Magnetization hysteresis loop shows that the synthesized magnetite exhibits no hysteretic features with a superparamagnetic behavior. The ethanol gas sensing properties of the synthesized magnetite were investigated, and it was found that the responsibility time is less than 10 s with good reproducibility for ethanol sensor. Accordingly, it is evaluated that the magnetite nanoparticles can be effectively used as a solid state ethanol sensor in industrial commercial product applications.

X-ray topography using the forward transmitted beam under multiple-beam diffraction conditions

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

Tsusaka, Y., E-mail: tsusaka@sci.u-hyogo.ac.jp; Takano, H.; Takeda, S.

2016-02-15

X-ray topographs are taken for a sapphire wafer with the [0001] surface normal, as an example, by forward transmitted synchrotron x-ray beams combined with two-dimensional electronic arrays in the x-ray detector having a spatial resolution of 1 μm. They exhibit no shape deformation and no position shift of the dislocation lines on the topographs. Since the topography is performed under multiple-beam diffraction conditions, the topographic images of a single diffraction (two-wave approximation condition) or plural diffractions (six-wave approximation condition) can be recorded without large specimen position changes. As usual Lang topographs, it is possible to determine the Burgers vector ofmore » each dislocation line. Because of high parallelism of the incoming x-rays and linear sensitivity of the electronic arrays to the incident x-rays, the present technique can be used to visualize individual dislocations in single crystals of the dislocation density as high as 1 × 10{sup 5} cm{sup −2}.« less

Hydroxyapatite-silver nanoparticles coatings on porous polyurethane scaffold.

PubMed

Ciobanu, Gabriela; Ilisei, Simona; Luca, Constantin

2014-02-01

The present paper is focused on a study regarding the possibility of obtaining hydroxyapatite-silver nanoparticle coatings on porous polyurethane scaffold. The method applied is based on a combined strategy involving hydroxyapatite biomimetic deposition on polyurethane surface using a Supersaturated Calcification Solution (SCS), combined with silver ions reduction and in-situ crystallization processes on hydroxyapatite-polyurethane surface by sample immersing in AgNO3 solution. The morphology, composition and phase structure of the prepared samples were characterized by scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray diffraction (XRD), UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS) measurements. The data obtained show that a layer of hydroxyapatite was deposited on porous polyurethane support and the silver nanoparticles (average size 34.71 nm) were dispersed among and even on the hydroxyapatite crystals. Hydroxyapatite/polyurethane surface acts as a reducer and a stabilizing agent for silver ions. The surface plasmon resonance peak in UV-Vis absorption spectra showed an absorption maximum at 415 nm, indicating formation of silver nanoparticles. The hydroxyapatite-silver polyurethane scaffolds were tested against Staphylococcus aureus and Escherichia coli and the obtained data were indicative of good antibacterial properties of the materials. © 2013.

Laser System for Photoelectron and X-Ray Production in the PLEIADES Compton Light Source

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

Gibson, D J; Barty, C J; Betts, S M

2005-04-21

The PLEIADES (Picosecond Laser-Electron Interaction for the Dynamic Evaluation of Structures) facility provides tunable short x-ray pulses with energies of 30-140 keV and pulse durations of 0.3-5 ps by scattering an intense, ultrashort laser pulse off a 35-75 MeV electron beam. Synchronization of the laser and electron beam is obtained by using a photoinjector gun, and using the same laser system to generate the electrons and the scattering laser. The Ti Ti:Sapphire, chirped pulse amplification based 500 mJ, 50 fs, 810 nm scattering laser and the similar 300 {micro}J, 5 ps, 266 nm photoinjector laser systems are detailed. Additionally, anmore » optical parametric chirped pulse amplification (OPCPA) system is studied as a replacement for part of the scattering laser front end. Such a change would significantly simplify the set-up the laser system by removing the need for active switching optics, as well as increase the pre-pulse contrast ratio which will be important when part of the scattering laser is used as a pump beam in pump-probe diffraction experiments using the ultrashort tunable x-rays generated as the probe.« less

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

Kaur, Maninder; McCloy, John S.; Kukkadapu, Ravi

Two sizes of iron/iron-oxide (Fe/Fe-oxide) nanoclusters (NCs) of 10 nm and 35 nm diameters were prepared using a cluster deposition technique. Both these NCs displayed XRD peaks due to body-centered cubic (bcc) Fe0 and magnetite-like phase. Mossbauer spectroscopy (MS) measurements: a) confirmed the core-shell nature of the NCs, b) the Fe-oxide shell to be nanocrystalline and partially oxidized, and c) the Fe-oxide spins are significantly canted. In addition to the bcc Fe and magnetite-like phases, a phase similar to tetragonal σ-Fe-Cr (8% Cr) was CLEARLY evident in the larger NC, based on X-ray diffraction. Origin of the tetragonallike phase inmore » the larger NC was not clear but could be due to significant distortion of the Fe0 core lattice planes; subtle peaks due to this phase were also apparent in the smaller NC. Unambiguous evidence for the presence of such a phase, however, was not clear from MS, X-ray photoelectron spectroscopy, vibrating sample magnetometry, X-ray magnetic circular dichroism, nor transmission electron microscopy. To our knowledge, this is the first report of tetragonallike phase in the Fe/Fe-oxide core-shell systems.« less

Ultrafast molecular processes mapped by femtosecond x-ray diffraction

NASA Astrophysics Data System (ADS)

Elsaesser, Thomas

2012-02-01

X-ray diffraction with a femtosecond time resolution allows for mapping photoinduced structural dynamics on the length scale of a chemical bond and in the time domain of atomic and molecular motion. In a pump-probe approach, a femtosecond excitation pulse induces structural changes which are probed by diffracting a femtosecond hard x-ray pulse from the excited sample. The transient angular positions and intensities of diffraction peaks give insight into the momentary atomic or molecular positions and into the distribution of electronic charge density. The simultaneous measurement of changes on different diffraction peaks is essential for determining atom positions and charge density maps with high accuracy. Recent progress in the generation of ultrashort hard x-ray pulses (Cu Kα, wavelength λ=0.154 nm) in laser-driven plasma sources has led to the implementation of the powder diffraction and the rotating crystal method with a time resolution of 100 fs. In this contribution, we report new results from powder diffraction studies of molecular materials. A first series of experiments gives evidence of a so far unknown concerted transfer of electrons and protons in ammonium sulfate [(NH4)2SO4], a centrosymmetric structure. Charge transfer from the sulfate groups results in the sub-100 fs generation of a confined electron channel along the c-axis of the unit cell which is stabilized by transferring protons from the adjacent ammonium groups into the channel. Time-dependent charge density maps display a periodic modulation of the channel's charge density by low-frequency lattice motions with a concerted electron and proton motion between the channel and the initial proton binding site. A second study addresses atomic rearrangements and charge dislocations in the non-centrosymmetric potassium dihydrogen phosphate [KH2PO4, KDP]. Photoexcitation generates coherent low-frequency motions along the LO and TO phonon coordinates, leaving the average atomic positions unchanged. The time-dependent maps of electron density demonstrate a concomitant oscillatory relocation of electronic charge with a spatial amplitude of the order of a chemical bond length, two orders of magnitude larger than the vibrational amplitudes. The coherent phonon motions drive the charge relocation, similar to a soft mode driven phase transition between the ferro- and paraelectric phase of KDP.

Multiple defocused coherent diffraction imaging: method for simultaneously reconstructing objects and probe using X-ray free-electron lasers.

PubMed

Hirose, Makoto; Shimomura, Kei; Suzuki, Akihiro; Burdet, Nicolas; Takahashi, Yukio

2016-05-30

The sample size must be less than the diffraction-limited focal spot size of the incident beam in single-shot coherent X-ray diffraction imaging (CXDI) based on a diffract-before-destruction scheme using X-ray free electron lasers (XFELs). This is currently a major limitation preventing its wider applications. We here propose multiple defocused CXDI, in which isolated objects are sequentially illuminated with a divergent beam larger than the objects and the coherent diffraction pattern of each object is recorded. This method can simultaneously reconstruct both objects and a probe from the coherent X-ray diffraction patterns without any a priori knowledge. We performed a computer simulation of the prposed method and then successfully demonstrated it in a proof-of-principle experiment at SPring-8. The prposed method allows us to not only observe broad samples but also characterize focused XFEL beams.

Angular rheology study of colloidal nanocrystals using Coherent X-ray Diffraction

NASA Astrophysics Data System (ADS)

Liang, Mengning; Harder, Ross; Robinson, Ian

2007-03-01

A new method using coherent x-ray diffraction provides a way to investigate the rotational motion of a colloidal suspension of crystals in real time. Coherent x-ray diffraction uses the long coherence lengths of synchrotron sources to illuminate a nanoscale particle coherently over its spatial dimensions. The penetration of high energy x-rays into various media allows for in-situ measurements making it ideal for suspensions. This technique has been used to image the structure of nanocrystals for some time but also has the capability of providing information about the orientation and dynamics of crystals. The particles are imaged in a specific diffraction condition allowing us to determine their orientation and observe how they rotate in real time with exceptional resolution. Such sensitivity allows for the study of rotational Brownian motion of nanocrystals in various suspensions and conditions. We present a study of the angular rheology of alumina and TiO2 colloidal nanocrystals in media using coherent x-ray diffraction.

Characterization of polycrystalline materials using synchrotron X-ray imaging and diffraction techniques

NASA Astrophysics Data System (ADS)

Ludwig, W.; King, A.; Herbig, M.; Reischig, P.; Marrow, J.; Babout, L.; Lauridsen, E. M.; Proudhon, H.; Buffière, J. Y.

2010-12-01

The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X-ray diffraction contrast tomography provides access to the 3-D shape, orientation, and elastic strain state of the individual grains from polycrystalline sample volumes containing up to thousand grains. Combining both imaging modalities, one obtains a comprehensive description of the materials microstructure at the micrometer length scale. Repeated observation during (interrupted) mechanical tests provide unprecedented insight into crystallographic and grain microstructure related aspects of polycrystalline deformation and degradation mechanisms.

Synthesis, growth, structural, optical, spectral, thermal and mechanical studies of 4-methoxy 4-nitrostilbene (MONS): a new organic nonlinear optical single crystal.

PubMed

Dinakaran, Paul M; Bhagavannarayana, G; Kalainathan, S

2012-11-01

4-Methoxy 4-nitrostilbene (MONS), a new organic nonlinear optical material has been synthesized. Based on the solubility data good quality single crystal with dimensions up to 38×11×3 mm(3) has been grown by slow evaporation method using ethyl methyl ketone (MEK) as a solvent. Powder XRD confirms the crystalline property and also the diffraction planes have been indexed. The lattice parameters for the grown MONS crystals were determined by using single crystal X-ray diffraction analysis and it reveals that the crystal lattice system is triclinic. The crystalline perfection of the grown crystals has been analysed by high resolution X-ray diffraction (HRXRD) rocking curve measurements. Fourier transform infrared (FTIR) spectrum for powdered MONS sample confirms the functional groups present in the grown crystal. The UV-vis absorption spectrum has been recorded in the range of 190-1100 nm and the cut off wavelength 499 nm has been determined. The optical constants of MONS have been determined through UV-vis-NIR spectroscopy. The MONS crystals were further subjected to other characterizations. i.e., (1)H NMR, TG/DTA, photoluminescence and microhardness test. The Kurtz and Perry powder technique confirms the NLO property of the grown crystal and the SHG efficiency of MONS was found to be 1.55× greater than that of KDP crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

Investigation of structural, optical, catalytic, fluorescence studies of eco-friendly synthesized Bi2S3 nanostructures

NASA Astrophysics Data System (ADS)

Ayodhya, Dasari; Veerabhadram, Guttena

2017-02-01

A simple solution phase method has been developed for the synthesis of ribonucleosides capped Bi2S3 nanostructures (NSs) with an average diameter of 15 nm and length of below 100 nm. Transmission electron microscopy (TEM), selected-area electron diffraction (SAED), and X-ray diffraction (XRD) studies revealed that these NSs were grown from a colloidal dispersion of amorphous Bi2S3 particles, which was first formed through a thermal reaction at a temperature of 60 °C. The phase and structure of the Bi2S3 NSs have been identified by using X-ray powder diffraction. The crystal structure had orthorhombic structure. The surface properties and morphology have been investigated using scanning electron microscope (SEM) technique. The N2 sorption-desorption experiments showed that the surface area of the NSs was 6.35 m2 g-1 by Brunauer-Emmett-Teller (BET). The experiments showed that the Bi2S3 NSs prepared in the present work could be used as catalyst for the reduction of SO dye using a reducing agent. It was found that the as-obtained Bi2S3 NSs contributed to the best catalytic activity. Photoluminescence experiments showed a quenching of the Bi2S3 fluorescence with increasing L-cysteine (Cys) content in the solution. Furthermore, the proposed NSs as sensor were employed for the determination of metal ions with satisfactory results.

Quantitative analysis of thoria phase in Th-U alloys using diffraction studies

NASA Astrophysics Data System (ADS)

Thakur, Shital; Krishna, P. S. R.; Shinde, A. B.; Kumar, Raj; Roy, S. B.

2017-05-01

In the present study the quantitative phase analysis of Th-U alloys in bulk form namely Th-52 wt% U and Th-3wt%U has been performed over the data obtained from both X ray diffraction and neutron diffraction technique using Rietveld method of FULLPROF software. Quantifying thoria (ThO2) phase present in bulk of the sample is limited due to surface oxidation and low penetration of x rays in high Z material. Neutron diffraction study probing bulk of the samples has been presented in comparison with x-ray diffraction study.

Synthesis and characterization of spinel type high-power cathode materials Li MxMn2-x O4 (M=Ni, Co, Cr)

NASA Astrophysics Data System (ADS)

Yoon, Y. K.; Park, C. W.; Ahn, H. Y.; Kim, D. H.; Lee, Y. S.; Kim, J.

2007-05-01

The transition metal-doped spinel cathode materials, LiM0.5Mn1.5O4 (M=Ni. Co, Cr) were prepared by solid-state reaction. The structure and morphology of the samples were investigated by X-ray diffraction, Rietveld refinement and scanning electron microscopy (SEM). The diffraction peaks of all the samples corresponded to a single phase of cubic spinel structure with a space group Fd3m. Field-emission SEM shows octahedron like shapes and the primary particles size was between 500 nm and 2 μm. Oxidation states of Ni, Co and Cr were found to be 2+, 2+ and 3+ as revealed by X-ray photoelectron spectroscopy. During discharging, LiNi0.5Mn1.5O4 and LiCo0.5Mn1.5O4 sample shows more than 130 mAh/g between 3.5 and 5.2 V at a current density of 0.65 mA/cm2 and well developed plateau around 5 V, respectively.

Nearly amorphous Mo-N gratings for ultimate resolution in extreme ultraviolet interference lithography

NASA Astrophysics Data System (ADS)

Wang, L.; Kirk, E.; Wäckerlin, C.; Schneider, C. W.; Hojeij, M.; Gobrecht, J.; Ekinci, Y.

2014-06-01

We present fabrication and characterization of high-resolution and nearly amorphous Mo1 - xNx transmission gratings and their use as masks for extreme ultraviolet (EUV) interference lithography. During sputter deposition of Mo, nitrogen is incorporated into the film by addition of N2 to the Ar sputter gas, leading to suppression of Mo grain growth and resulting in smooth and homogeneous thin films with a negligible grain size. The obtained Mo0.8N0.2 thin films, as determined by x-ray photoelectron spectroscopy, are characterized to be nearly amorphous using x-ray diffraction. We demonstrate a greatly reduced Mo0.8N0.2 grating line edge roughness compared with pure Mo grating structures after e-beam lithography and plasma dry etching. The amorphous Mo0.8N0.2 thin films retain, to a large extent, the benefits of Mo as a phase grating material for EUV wavelengths, providing great advantages for fabrication of highly efficient diffraction gratings with extremely low roughness. Using these grating masks, well-resolved dense lines down to 8 nm half-pitch are fabricated with EUV interference lithography.

Selenium single-wavelength anomalous diffraction de novo phasing using an X-ray-free electron laser

DOE PAGES

Hunter, Mark S.; Yoon, Chun Hong; DeMirci, Hasan; ...

2016-11-04

Structural information about biological macromolecules near the atomic scale provides important insight into the functions of these molecules. To date, X-ray crystallography has been the predominant method used for macromolecular structure determination. However, challenges exist when solving structures with X-rays, including the phase problem and radiation damage. X-ray-free electron lasers (X-ray FELs) have enabled collection of diffraction information before the onset of radiation damage, yet the majority of structures solved at X-ray FELs have been phased using external information via molecular replacement. De novo phasing at X-ray FELs has proven challenging due in part to per-pulse variations in intensity andmore » wavelength. Here we report the solution of a selenobiotinyl-streptavidin structure using phases obtained by the anomalous diffraction of selenium measured at a single wavelength (Se-SAD) at the Linac Coherent Light Source. Finally, our results demonstrate Se-SAD, routinely employed at synchrotrons for novel structure determination, is now possible at X-ray FELs.« less

Macromolecular structures probed by combining single-shot free-electron laser diffraction with synchrotron coherent X-ray imaging.

PubMed

Gallagher-Jones, Marcus; Bessho, Yoshitaka; Kim, Sunam; Park, Jaehyun; Kim, Sangsoo; Nam, Daewoong; Kim, Chan; Kim, Yoonhee; Noh, Do Young; Miyashita, Osamu; Tama, Florence; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Tono, Kensuke; Kohmura, Yoshiki; Yabashi, Makina; Hasnain, S Samar; Ishikawa, Tetsuya; Song, Changyong

2014-05-02

Nanostructures formed from biological macromolecular complexes utilizing the self-assembly properties of smaller building blocks such as DNA and RNA hold promise for many applications, including sensing and drug delivery. New tools are required for their structural characterization. Intense, femtosecond X-ray pulses from X-ray free-electron lasers enable single-shot imaging allowing for instantaneous views of nanostructures at ambient temperatures. When combined judiciously with synchrotron X-rays of a complimentary nature, suitable for observing steady-state features, it is possible to perform ab initio structural investigation. Here we demonstrate a successful combination of femtosecond X-ray single-shot diffraction with an X-ray free-electron laser and coherent diffraction imaging with synchrotron X-rays to provide an insight into the nanostructure formation of a biological macromolecular complex: RNA interference microsponges. This newly introduced multimodal analysis with coherent X-rays can be applied to unveil nano-scale structural motifs from functional nanomaterials or biological nanocomplexes, without requiring a priori knowledge.

Exploration of New Principles in Spintronics Based on Topological Insulators (Option 1)

DTIC Science & Technology

2012-05-14

on the surface and found that our crystals are exceedingly homogeneous (Supplementary Information). The persistently narrow X - ray diffraction peaks...modified Bridgman method (see Supplementary Information for details). X - ray diffraction measurements indicated the monotonic shrinkage of a and c axis...and annealing at that temperature for 4 days. X - ray diffraction analyses confirmed that all the samples have the same crystal structure (R 3m

Synthesis and characterization of colloidal CdTe nanocrystals

NASA Astrophysics Data System (ADS)

Semendy, Fred; Jaganathan, Gomatam; Dhar, Nibir; Trivedi, Sudhir; Bhat, Ishwara; Chen, Yuanping

2008-08-01

We synthesized CdTe nano crystals (NCs) in uniform sizes and in good quality as characterized by photoluminescence (PL), AFM, and X-ray diffraction. In this growth procedure, CdTe nano-crystal band gap is strongly dependent on the growth time and not on the injection temperature or organic ligand concentration. This is very attractive because of nano-crystal size can be easily controlled by the growth time only and is very attractive for large scale synthesis. The color of the solution changes from greenish yellow to light orange then to deep orange and finally grayish black to black over a period of one hour. This is a clear indication of the gradual growth of different size (and different band gap) of CdTe nano-crystals as a function of the growth time. In other words, the size of the nano-crystal and its band gap can be controlled by adjusting the growth time after injection of the tellurium. The prepared CdTe NCs were characterized by absorption spectra, photoluminescence (PL), AFM and X-ray diffraction. Measured absorption maxima are at 521, 560, 600 and 603 nm corresponding to band gaps of 2.38, 2.21,2,07 and 2.04 eV respectively for growth times of 15, 30, 45 and 60 minutes. From the absorption data nano-crystal growth size saturates out after 45 minutes. AFM scanning of these materials indicate that the size of these particles is between 4 - 10 nm in diameter for growth time of 45 minutes. XD-ray diffraction indicates that these nano crystals are of cubic zinc blende phase. This paper will present growth and characterization data on CdTe nano crystals for various growth times.

Efficient modeling of Bragg coherent x-ray nanobeam diffraction

DOE PAGES

Hruszkewycz, S. O.; Holt, M. V.; Allain, M.; ...

2015-07-02

X-ray Bragg diffraction experiments that utilize tightly focused coherent beams produce complicated Bragg diffraction patterns that depend on scattering geometry, characteristics of the sample, and properties of the x-ray focusing optic. In this paper, we use a Fourier-transform-based method of modeling the 2D intensity distribution of a Bragg peak and apply it to the case of thin films illuminated with a Fresnel zone plate in three different Bragg scattering geometries. Finally, the calculations agree well with experimental coherent diffraction patterns, demonstrating that nanodiffraction patterns can be modeled at nonsymmetric Bragg conditions with this approach—a capability critical for advancing nanofocused x-raymore » diffraction microscopy.« less

Hydrogen bonded supra-molecular framework in inorganic-organic hybrid compounds: Syntheses, structures, and photoluminescent properties

NASA Astrophysics Data System (ADS)

Yan, Li; Liu, Wei; Li, Chuanbi; Wang, Yifei; Ma, Li; Dong, Qinqin

2013-03-01

Two novel compounds constructed from aromatic acid and N-Heterocyclic ligands have been synthesized by hydrothermal reaction: [Cd(mip)(1,8-NDC)(H2O)]2 (1) [mip = 2-(3-methoxyphenyl)-1H-imidazo[4,5-f][1,10]phenanthroline, 1,8-NDC = naphthalene-1,8-dicarboxylic acid] and Cd(mip)2(NTC)2 (2) [NTC = nicotinic acid]. Compounds 1 and 2 are characterized by elemental analysis, IR, single crystal X-ray diffraction and thermogravimetric analysis (TGA). Single-crystal X-ray investigation reveals that compounds 1-2 are 0 dimensional (0D) structures, and the existence of hydrogen bonds and π-π interactions lead the 0D to 2D novel framework. Hydrogen bonds and π-π interactions are powerful non-covalent intermolecular interactions for directing supra-molecular architectures. TG analysis shows clear courses of weight loss, which corresponds to the decomposition of different ligands. At room temperature, compound 1 exhibits emission at 449 nm upon excitation at 325 nm, and compound 2 shows a strong emission at 656 nm upon excitation at 350 nm. Fluorescent spectrum displays that compounds 1 and 2 are potential luminescent materials.

The influence of an MgO nanolayer on the planar Hall effect in NiFe films

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

Li, Minghua, E-mail: mhli@ustb.edu.cn; Department of Electrical Engineering, University of California, Los Angeles, California 90095; Zhao, Zhiduo

2015-03-28

The Planar Hall Effect (PHE) in NiFe films was studied using MgO as the buffer and capping layer to reduce the shunt effect. The thermal annealing was found to be effective in increasing the sensitivity. The sensitivity of the magnetic field reached as high as 865 V/AT in a MgO (3 nm)/NiFe (5 nm)/MgO(3 nm)/Ta(3 nm) structure after annealing at 500 °C for 2 h, which is close to the sensitivity of semiconductor Hall Effect (HE) sensors. X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) were used to study the sample. The results show that the top crystallization of MgO and NiFemore » (111) texture were improved by proper annealing. The smooth and clear bottom MgO/NiFe and top NiFe/MgO interface is evident from our data. In addition, the shunt current of Ta was decreased. These combined factors facilitate the improvement of the sensitivity of the magnetic field.« less

Optimum deposition conditions of ultrasmooth silver nanolayers

PubMed Central

2014-01-01

Reduction of surface plasmon-polariton losses due to their scattering on metal surface roughness still remains a challenge in the fabrication of plasmonic devices for nanooptics. To achieve smooth silver films, we study the dependence of surface roughness on the evaporation temperature in a physical vapor deposition process. At the deposition temperature range 90 to 500 K, the mismatch of thermal expansion coefficients of Ag, Ge wetting layer, and sapphire substrate does not deteriorate the metal surface. To avoid ice crystal formation on substrates, the working temperature of the whole physical vapor deposition process should exceed that of the sublimation at the evaporation pressure range. At optimum room temperature, the root-mean-square (RMS) surface roughness was successfully reduced to 0.2 nm for a 10-nm Ag layer on sapphire substrate with a 1-nm germanium wetting interlayer. Silver layers of 10- and 30-nm thickness were examined using an atomic force microscope (AFM), X-ray reflectometry (XRR), and two-dimensional X-ray diffraction (XRD2). PACS 63.22.Np Layered systems; 68. Surfaces and interfaces; thin films and nanosystems (structure and nonelectronic properties); 81.07.-b Nanoscale materials and structures: fabrication and characterization PMID:24685115

Fabrication of water-repellent cellulose fiber coated with magnetic nanoparticles under supercritical carbon dioxide

NASA Astrophysics Data System (ADS)

Xu, Shengjie; Shen, Danping; Wu, Peiyi

2013-04-01

Hematite nanoparticle-coated magnetic composite fiber was prepared in supercritical carbon dioxide (scCO2). With the help of scCO2, cellulose did not need to be dissolved and regenerated and it could be in any form (e.g., cotton wool, filter paper, textile, etc.). The penetrating and swelling effect of scCO2, the slowing reaction rate of weak alkalis, and the template effect of cellulose fibers were discovered to be the key factors for the fabrication of ordered cellulose/Fe2O3 composite fibers. The structures of the composite fibers as well as the layers of Fe2O3 particles were characterized by means of scanning/transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and Raman investigation. It was found that α-Fe2O3 granules which ranged from 30 to 85 nm with average diameter around 55 nm would be generated on the surface of cellulose fibers via potassium acetate, while irregular square prisms (ranged from 200 to 600 nm) which were composed of smaller nanoparticles ( 10 nm) would be fabricated via urea. And, the obtained composite was highly water repellent with superparamagnetic or ferromagnetic properties.

Optoelectronic and Electrochemical Properties of Vanadium Pentoxide Nanowires Synthesized by Vapor-Solid Process

PubMed Central

Pan, Ko-Ying; Wei, Da-Hua

2016-01-01

Substantial synthetic vanadium pentoxide (V2O5) nanowires were successfully produced by a vapor-solid (VS) method of thermal evaporation without using precursors as nucleation sites for single crystalline V2O5 nanowires with a (110) growth plane. The micromorphology and microstructure of V2O5 nanowires were analyzed by scanning electron microscope (SEM), energy-dispersive X-ray spectroscope (EDS), transmission electron microscope (TEM) and X-ray diffraction (XRD). The spiral growth mechanism of V2O5 nanowires in the VS process is proved by a TEM image. The photo-luminescence (PL) spectrum of V2O5 nanowires shows intrinsic (410 nm and 560 nm) and defect-related (710 nm) emissions, which are ascribable to the bound of inter-band transitions (V 3d conduction band to O 2p valence band). The electrical resistivity could be evaluated as 64.62 Ω·cm via four-point probe method. The potential differences between oxidation peak and reduction peak are 0.861 V and 0.470 V for the first and 10th cycle, respectively. PMID:28335268

Deposition of GdVO4:Eu3+ nanoparticles on silica nanospheres by a simple sol gel method

NASA Astrophysics Data System (ADS)

Liu, Guixia; Hong, Guangyan; Wang, Jinxian; Dong, Xiangting

2006-07-01

The deposition and coating of GdVO4:Eu3+ nanoparticles on spherical silica was carried out using a simple sol-gel method at low temperature. The GdVO4:Eu3+-coated silica composites obtained were characterized by differential thermal analysis (DTA), thermogravimetric (TG) analysis, x-ray diffraction (XRD), Fourier-transform IR spectroscopy (FT-IR), transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS), photoluminescence spectra, and kinetic decay. It is found that the ~5 nm GdVO4:Eu3+ nanoparticles coating the silica spheres are crystal in the as-prepared samples and the crystallinity increases with increasing annealing temperature. The composites obtained are spherical in shape with an average size of 100 nm. The GdVO4:Eu3+ nanoparticles are linked with silica cores by a chemical bond. The photoluminescence spectra of the obtained GdVO4:Eu3+-coated silica composites are similar to those of the bulk GdVO4:Eu3+ phosphors. The strongest peak is near 617 nm, which indicates that Eu3+ is located in the low symmetry site with non-inversion centre.

Ultrasonically assisted synthesis of lead oxide nanoflowers using ball milling

NASA Astrophysics Data System (ADS)

Bangi, Uzma K. H.; Park, Hyung-Ho; Han, Wooje; Prakshale, Vipul M.; Deshmukh, Lalasaheb P.

2017-05-01

The experimental results on the ultrasonically assisted synthesis of lead oxide nanoflowers using ball milling have been reported in the present work. Lead oxide nanoflowers were prepared employing mixed ligands by subjecting the formed precipitate to ultrasonication and grinding/ball milling. The effect of ball milling as well as fine grinding in agate mortar on the microstructure and surface morphology of the lead oxide was studied. The characteristics of synthesized PbO were studied using X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and field emission scanning electron microscopy techniques. XRD results demonstrated the tetragonal phase of PbO with crystallite size of around 25 nm and strain of 3.6 × 10-3 calculated from Williamson-Hall plot. FESEM images manifested the formation of nanodiscs and nanoflowers with a diameter of around 300 nm and thickness of 50 nm. XPS spectra revealed the formation of PbO with photoelectron peak of Pb 4f and O 1 s lied at 137.68 and 529.96 eV. Moreover, FTIR spectrum exhibited Pb-O bond peak in the range of 400-530 cm-1.

On the Discontinuity of Polycrystalline Silicon Thin Films Realized by Aluminum-Induced Crystallization of PECVD-Deposited Amorphous Si

NASA Astrophysics Data System (ADS)

Pan, Qingtao; Wang, Tao; Yan, Hui; Zhang, Ming; Mai, Yaohua

2017-04-01

Crystallization of glass/Aluminum (50, 100, 200 nm) /hydrogenated amorphous silicon (a-Si:H) (50, 100, 200 nm) samples by Aluminum-induced crystallization (AIC) is investigated in this article. After annealing and wet etching, we found that the continuity of the polycrystalline silicon (poly-Si) thin films was strongly dependent on the double layer thicknesses. Increasing the a-Si:H/Al layer thickness ratio would improve the film microcosmic continuity. However, too thick Si layer might cause convex or peeling off during annealing. Scanning electron microscopy (SEM) and Energy Dispersive X-ray spectroscopy (EDX) are introduced to analyze the process of the peeling off. When the thickness ratio of a-Si:H/Al layer is around 1 to 1.5 and a-Si:H layer is less than 200 nm, the poly-Si film has a good continuity. Hall measurements are introduced to determine the electrical properties. Raman spectroscopy and X-ray diffraction (XRD) results show that the poly-Si film is completely crystallized and has a preferential (111) orientation.

Intercalation of cellulase enzyme into a hydrotalcite layer structure

NASA Astrophysics Data System (ADS)

Zou, N.; Plank, J.

2015-01-01

A new inorganic-organic hybrid material whereby cellulase enzyme is incorporated into a hydrotalcite type layered double hydroxide (LDH) structure is reported. The Mg2Al-cellulase-LDH was synthesized via co-precipitation from Mg/Al nitrate at pH=9.6. Characterization was performed using X-ray powder diffraction (XRD), small angle X-ray scattering (SAXS), elemental analysis, infrared spectroscopy (IR) and thermogravimetry (TG). From XRD and SAXS measurements, a d-value of ~5.0 nm was identified for the basal spacing of the Mg2Al-cellulase-LDH. Consequently, the cellulase enzyme (hydrodynamic diameter ~6.6 nm) attains a slightly compressed conformation when intercalated. Formation of the LDH hybrid was also confirmed via scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Mg2Al-cellulase-LDH phases appear as ~20 nm thin foils which are intergrown to flower-like aggregates. Activity of the enzyme was retained after deintercalation from the Mg2Al-LDH framework using anion exchange. Accordingly, cellulase is not denatured during the intercalation process, and LDH presents a suitable host structure for time-controlled release of the biomolecule.