Sample records for x-ray diffraction brunauer-emmett-teller

  1. A controlled release of ibuprofen by systematically tailoring the morphology of mesoporous silica materials

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

    Qu Fengyu; Chemistry and Pharmaceutical College, Jiamusi University, Jiamusi 154007; Zhu Guangshan

    2006-07-15

    A series of mesoporous silica materials with similar pore sizes, different morphologies and variable pore geometries were prepared systematically. In order to control drug release, ibuprofen was employed as a model drug and the influence of morphology and pore geometry of mesoporous silica on drug release profiles was extensively studied. The mesoporous silica and drug-loaded samples were characterized by X-ray diffraction, Fourier transform IR spectroscopy, N{sub 2} adsorption and desorption, scanning electron microscopy, and transmission electron microscopy. It was found that the drug-loading amount was directly correlated to the Brunauer-Emmett-Teller surface area, pore geometry, and pore volume; while the drugmore » release profiles could be controlled by tailoring the morphologies of mesoporous silica carriers. - Graphical abstract: The release of ibuprofen is controlled by tailoring the morphologies of mesoporous silica. The mesoporous silica and drug-loaded samples are characterized by powder X-ray diffraction, Fourier transform IR spectroscopy, N{sub 2} adsorption and desorption, scanning electron microscopy, and transmission electron microscopy. The drug-loading amount is directly correlated to the Brunauer-Emmett-Teller surface area, pore geometry, and pore volume; while the drug release profiles can be controlled by tailoring the morphologies of mesoporous silica carriers.« less

  2. Preparation of K-doped TiO2 nanostructures by wet corrosion and their sunlight-driven photocatalytic performance

    NASA Astrophysics Data System (ADS)

    Shin, Eunhye; Jin, Saera; Kim, Jiyoon; Chang, Sung-Jin; Jun, Byung-Hyuk; Park, Kwang-Won; Hong, Jongin

    2016-08-01

    K-doped TiO2 nanowire networks were prepared by the corrosion reaction of Ti nanoparticles in an alkaline (potassium hydroxide: KOH) solution. The prepared nanostructures were characterized by scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) analysis, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, X-ray diffraction (XRD) and photoluminescence (PL) spectra. Their sunlight-driven photocatalytic activity was also investigated with differently charged dye molecules, such as methylene blue, rhodamine B and methyl orange. The adsorption of the dye molecules on the photocatalyst surface would play a critical role in their selective photodegradation under sunlight illumination.

  3. Grafted chromium 13-membered dioxo-macrocyclic complex into aminopropyl-based nanoporous SBA-15

    NASA Astrophysics Data System (ADS)

    Tarlani, Aliakbar; Joharian, Monika; Narimani, Khashayar; Muzart, Jacques; Fallah, Mahtab

    2013-07-01

    In a new approach, chromium (III) tetraaza dioxo ligand was grafted onto functionalized SBA-15 after four step reactions by using coordinating ability of anchored amino functionalized SBA-15. After the termination of each step, the obtained product was characterized by FT-IR, low-angle X-ray diffraction (LA-XRD), N2 adsorption-desorption isotherms (Brunauer-Emmett-Teller (BET)-Barret-Joyner-Halenda (BJH)) and thermogravimetric analysis (TGA), and used as catalyst for the efficient and regioselective alcoholysis of styrene oxide to 2-alkoxy-1-phenylethanol product at ambient temperature.

  4. Efficiency enhancement in dye sensitized solar cells using dual function mesoporous silica as scatterer and back recombination inhibitor

    NASA Astrophysics Data System (ADS)

    Tanvi; Mahajan, Aman; Bedi, R. K.; Kumar, Subodh; Saxena, Vibha; Aswal, D. K.

    2016-08-01

    In the present work, we report the usage of mesoporous silica for improving light harvesting as well as for suppression of back recombination without affecting the extent of dye loading on TiO2 films. Synthesized mesoporous SiO2 was characterized by X-ray photoelectron spectroscopy, X-ray diffraction, Brunauer Emmett and Teller measurement, Scanning electron microscopy and Transmission electron microscopy. DSSCs were fabricated by incorporating different wt% of mesoporous SiO2 in TiO2 paste. An improvement of 50% was observed for devices fabricated using 0.75 wt% of mesoporous SiO2. The mechanism behind the improvement was investigated using electrochemical impedance spectroscopy and UV-Vis spectroscopy.

  5. 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.

  6. Conversion of nuclear waste to molten glass: Formation of porous amorphous alumina in a high-Al melter feed

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

    Xu, Kai; Hrma, Pavel; Washton, Nancy

    The transition of Al phases in a simulated high-Al high-level nuclear waste melter feed heated at 5 K min-1 to 700°C was investigated with transmission electron microscopy, 27Al nuclear magnetic resonance spectroscopy, the Brunauer-Emmett-Teller method, and X-ray diffraction. At temperatures between 300 and 500°C, porous amorphous alumina formed from the dehydration of gibbsite, resulting in increased specific surface area of the feed (~8 m2 g-1). The high-surface-area amorphous alumina formed in this manner could potentially stop salt migration in the cold cap during nuclear waste vitrification.

  7. Fabrication and electrochemical properties of activated CNF/Cu x Mn1- x Fe2O4 composite nanostructures

    NASA Astrophysics Data System (ADS)

    Nilmoung, Sukanya; Sonsupap, Somchai; Sawangphruk, Montree; Maensiri, Santi

    2018-06-01

    This work reports the fabrication and electrochemical properties of activated carbon nanofibers composited with copper manganese ferrite (ACNF/Cu x Mn1- x Fe2O4: x = 0.0, 0.2, 0.4, 0.6, 0.8) nanostructures. The obtained samples were characterized by means of X-ray diffraction, field emission scanning electron microscopy, Brunauer-Emmett-Teller analyzer, thermal gravimetric analysis, X-ray photoemission spectroscopy, and X-ray absorption spectroscopy. The supercapacitive behavior of the electrodes is tested using cyclic voltammetery, galvanostatic charge-discharge and electrochemical impedance spectroscopy. By varying ` x', the highest specific capacitance of 384 F/g at 2 mV/s using CV and 314 F/g at 2 A/g using GCD are obtained for the x = 0.2 electrode. The second one of 235 F/g at 2 mV/s using CV and 172 F/g at 2 A/g using GCD are observed for x = 0.8 electrode. The corresponding energy densities are 74 and 41 Wh/kg, respectively. It is observed that the cyclic stability of the prepared samples strongly depend on the amount of carbon, while the specific capacitance was enhanced by the sample with nearly proportional amount between carbon and CuMnFe2O4. Such results may arise from the synergetic effect between CuMnFe2O4 and ACNF.

  8. 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.

  9. Dye adsorption into transition metal-doped zinc oxide nanoparticles supported on natural zeolites to solve wastewater issue

    NASA Astrophysics Data System (ADS)

    Indra Pratiwi, Margaretha; Afifah, Nur; Saleh, Rosari

    2017-03-01

    In this work, Fe-doped zinc oxide/natural zeolite (Fe:ZnO/NZ) nanocomposites were prepared using the co-precipitation method with various NZ amounts. The nanocomposites were characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) surface area analysis and thermogravimetric analysis (TGA). The nanocomposites were used to remove methylene blue (MB) dye from an aqueous solution. The effect of various NZ amounts and initial MB concentration were tested. The Pseudo-first-order and pseudo-second-order kinetic models were used to explain the adsorption mechanism. The Langmuir and the Freundlich isotherm models were used to fit the adsorption isotherms of the nanocomposites.

  10. Synthesis and characterization of ZnO incorporated magnetically recoverable KIT-6 as a novel and efficient catalyst in the preparation of symmetrical N, N‧-alkylidene bisamides

    NASA Astrophysics Data System (ADS)

    Saadati-Moshtaghin, Hamid Reza; Zonoz, Farrokhzad Mohammadi; Amini, Mostafa M.

    2018-04-01

    A novel magnetically recoverable nanocomposite consisting of the NiFe2O4 core and KIT-6 mesoporous silica shell incorporated with ZnO nanoparticles was constructed. This nanocomposite was characterized by Fourier transform infrared (FT-IR), powder X-ray diffraction (XRD), Brunauer Emmett Teller (BET), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). This new nanocomposite demonstrated a catalytic performance in the synthesis of symmetrical N,N‧-alkylidene bisamides at the condensation reaction under solvent-free conditions. The nanocatalyst could simply be recovered from the reaction environment by using an exterior magnet and reused five times without a remarkable losing in the catalytic property.

  11. Speckle in the diffraction patterns of Hendricks-Teller and icosahedral glass models

    NASA Technical Reports Server (NTRS)

    Garg, Anupam; Levine, Dov

    1988-01-01

    It is shown that the X-ray diffraction patterns from the Hendricks-Teller model for layered systems and the icosahedral glass models for the icosahedral phases show large fluctuations between nearby scattering wave vectors and from sample to sample, that are quite analogous to laser speckle. The statistics of these fluctuations are studied analytically for the first model and via computer simulations for the second. The observability of these effects is discussed briefly.

  12. Leaching of manganese from electrolytic manganese residue by electro-reduction.

    PubMed

    Shu, Jiancheng; Liu, Renlong; Liu, Zuohua; Chen, Hongliang; Tao, Changyuan

    2017-08-01

    In this study, an improved process for leaching manganese from electrolytic manganese residue (EMR) by electro-reduction was developed. The mechanisms of the electro-reduction leaching were investigated through X-ray diffraction, scanning electron microscopy, X-ray fluorescence, and Brunauer Emmett Teller. The results show that the electric field could change the surface charge distribution of EMR particles, and the high-valent manganese can be reduced by electric field. The leaching efficient of manganese reached 84.1% under the optimal leaching condition: 9.2 wt% H 2 SO 4 , current density of 25 mA/cm 2 , solid-to-liquid ratio of 1:5, and leaching time for 1 h. It is 37.9% higher than that attained without an electric field. Meanwhile, the manganese content in EMR decreased from 2.57% to 0.48%.

  13. High Catalytic Efficiency of Nanostructured β-CoMoO₄ in the Reduction of the Ortho-, Meta- and Para-Nitrophenol Isomers.

    PubMed

    Al-Wadaani, Fahd; Omer, Ahmed; Abboudi, Mostafa; Oudghiri Hassani, Hicham; Rakass, Souad; Messali, Mouslim; Benaissa, Mohammed

    2018-02-09

    Nanostructured β-CoMoO₄ catalysts have been prepared via the thermal decomposition of an oxalate precursor. The catalyst was characterized by infrared spectroscopy (FTIR), X-ray diffraction (XRD), Brunauer-Emmett-Teller method (BET), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM). The efficiency of these nanoparticles in the reduction of ortho - and meta -nitrophenol isomers (2-NP, 3-NP, and 4-NP) to their corresponding aminophenols was tested using UV-visible spectroscopy measurements. It was found that, with a β-CoMoO₄ catalyst, NaBH₄ reduces 3-NP instantaneously, whilst the reduction of 2-NP and 4-NP is slower at 8 min. This difference is thought to arise from the lower acidity of 3-NP, where the negative charge of the phenolate could not be delocalized onto the oxygen atoms of the meta-nitro group.

  14. Calcium Oxide Derived from Waste Shells of Mussel, Cockle, and Scallop as the Heterogeneous Catalyst for Biodiesel Production

    PubMed Central

    Chaiyut, Nattawut; Worawanitchaphong, Phatsakon

    2013-01-01

    The waste shell was utilized as a bioresource of calcium oxide (CaO) in catalyzing a transesterification to produce biodiesel (methyl ester). The economic and environmen-friendly catalysts were prepared by a calcination method at 700–1,000°C for 4 h. The heterogeneous catalysts were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), and the Brunauer-Emmett-Teller (BET) method. The effects of reaction variables such as reaction time, reaction temperature, methanol/oil molar ratio, and catalyst loading on the yield of biodiesel were investigated. Reusability of waste shell catalyst was also examined. The results indicated that the CaO catalysts derived from waste shell showed good reusability and had high potential to be used as biodiesel production catalysts in transesterification of palm oil with methanol. PMID:24453854

  15. A Hydrothermal Route to the Synthesis of CaTiO3 Nanocuboids Using P25 as the Titanium Source

    NASA Astrophysics Data System (ADS)

    Yan, Yuxiang; Yang, Hua; Zhao, Xinxin; Zhang, Haimin; Jiang, Jinlong

    2018-03-01

    CaTiO3 nanocuboids (width 0.3-0.5 μm, length 0.8-1.1 μm) have been synthesized by a hydrothermal route using commercial P25 as the titanium source. The as-prepared sample was systematically characterized by means of x-ray powder diffraction, field-emission scanning electron microscopy, field-emission transmission electron microscopy, x-ray photoelectron spectroscopy, Brunauer-Emmett-Teller, ultraviolet-visible diffuse reflectance spectroscopy and electrochemical impedance spectroscopy. The photocatalytic activity of the sample was evaluated by degrading rhodamine B under simulated sunlight irradiation. It is demonstrated that CaTiO3 nanocuboids exhibit superior photocatalytic activity when compared with CaTiO3 nanoparticles. By investigating the effect of scavengers on the dye degradation and the yield of hydroxyl (·OH) radicals, it is concluded that ·OH is the dominant reactive species.

  16. Structure and magnetic/electrochemical properties of Cu-doped BiFeO3 nanoparticles prepared by a simple solution method

    NASA Astrophysics Data System (ADS)

    Khajonrit, Jessada; Phumying, Santi; Maensiri, Santi

    2016-06-01

    BiFe1- x Cu x O3 (x = 0, 0.05, 0.1, 0.2, and 0.3) nanoparticles were prepared by a simple solution method. The prepared nanoparticles were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) method analysis using the Barret-Joyner-Halenda (BJH) model, and X-ray absorption spectroscopy (XAS). Magnetization properties were obtained using a vibrating sample magnetometer (VSM) at room temperature. Magnetization was clearly enhanced by increasing Cu content and decreasing particle size. Zero-field-cooled (ZFC) and field-cooled (FC) temperature-dependent magnetization measurements showed that blocking temperature increased with increasing Cu content. Electrochemical properties were investigated by cyclic voltammetry (CV) and the galvanostatic charge-discharge (GCD) method. The performance of the fabricated supercapacitor was improved for the BiFe0.95Cu0.05O3 electrode. The highest specific capacitance was 568.13 F g-1 at 1 A g-1 and the capacity retention was 77.13% after 500 cycles.

  17. 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.

  18. Surfactant-free solvothermal synthesis of Hydroxyapatite nested bundles for the effective photodegradation of cationic dyes

    NASA Astrophysics Data System (ADS)

    Reeta Mary, I.; Sonia, S.; Navadeepthy, D.; Mangalaraj, D.; Viswanathan, C.; Ponpandian, N.

    2018-05-01

    In this study, hydroxyapatite nested bundles (HNBs) were successfully constructed from nanosticks as nanoscale building blocks via a facile, solvothermal process without using any surfactant. The fabricated HNBs were structurally analyzed using X-ray diffraction and Fourier transform infrared spectroscopy, which confirmed the purity of the HNBs. The surface characteristics were determined by field emission scanning electron microscopy and Brunauer-Emmett-Teller analysis, and the optical characteristics by ultraviolet (UV)-visible spectroscopy. The synthesized HNBs were tested to determine their activity during the degradation of methylene blue, methylene violet, and rhodamine B via photocatalysis under UV irradiation. The degradation efficiency of HNBs and the rate of degradation can be explained based on the properties of the HNBs and cationic dyes.

  19. Study of KOH/Al2O3 as heterogeneous catalyst for biodiesel production via in situ transesterification from microalgae.

    PubMed

    Ma, Guixia; Hu, Wenrong; Pei, Haiyan; Jiang, Liqun; Ji, Yan; Mu, Ruimin

    2015-01-01

    Heterogeneous KOH/Al2O3 catalysts, synthesized by the wet impregnation method with different KOH loadings (20-40 wt%) and calcination temperatures from 400°C to 800°C, were used to produce biodiesel from Chlorella vulgaris biomass by in situ transesterification. The highest yield of biodiesel of 89.53±1.58% was achieved at calcination temperature of 700°C for 2 h and 35 wt% loading of KOH, and at the optimal reaction condition of 10 wt% of catalyst content, 8 mL/g of methanol to biomass ratio and at 60°C for 5 h. The characteristics of the catalysts were analysed by X-ray diffraction, scanning electron microscopy and Brunauer-Emmett-Teller.

  20. Resolution dependence of petrophysical parameters derived from X-ray tomography of chalk

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

    Müter, D.; Sørensen, H. O.; Jha, D.

    2014-07-28

    X-ray computed tomography data from chalk drill cuttings were taken over a series of voxel dimensions, ranging from 320 to 25 nm. From these data sets, standard petrophysical parameters (porosity, surface area, and permeability) were derived and we examined the effect of the voxel dimension (i.e., image resolution) on these properties. We found that for the higher voxel dimensions, they are severely over or underestimated, whereas for 50 and 25 nm voxel dimension, the resulting values (5%–30% porosity, 0.2–2 m{sup 2}/g specific surface area, and 0.06–0.34 mD permeability) are within the expected range for this type of rock. We compared our resultsmore » to macroscopic measurements and in the case of surface area, also to measurements using the Brunauer-Emmett-Teller (BET) method and found that independent of the degree of compaction, the results from tomography amount to about 30% of the BET method. Finally, we concluded that at 25 nm voxel dimension, the essential features of the nanoscopic pore network in chalk are captured but better resolution is still needed to derive surface area.« less

  1. Preparation of Supported Palladium Catalysts using Deep Eutectic Solvents.

    PubMed

    Iwanow, Melanie; Finkelmeyer, Jasmin; Söldner, Anika; Kaiser, Manuela; Gärtner, Tobias; Sieber, Volker; König, Burkhard

    2017-09-12

    Deep eutectic solvents (DESs) dissolve metal salts or oxides and are used as solvent and carbon source for the preparation of supported palladium catalysts. After dissolving of the palladium salt in the DES, the pyrolysis of the mixture under nitrogen atmosphere yields catalytically active palladium on supporting material composed of carbon, nitrogen and oxygen (CNO) by a simple single step preparation method without further activation. The catalysts were characterized by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) and CHNS/O elementary analysis. The amount of functional groups on the surface of the supporting material was determined by Boehm titrations. Moreover, the activity of the prepared catalysts was evaluated in the hydrogenation of linear alkenes and compared with a commercial Pd/C catalyst. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. 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.

  3. 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.

  4. Fe3-xCuxO4 as highly active heterogeneous Fenton-like catalysts toward elemental mercury removal.

    PubMed

    Zhou, Changsong; Sun, Lushi; Zhang, Anchao; Wu, Xiaofeng; Ma, Chuan; Su, Sheng; Hu, Song; Xiang, Jun

    2015-04-01

    A series of novel spinel Fe3-xCuxO4 (0<x<0.71) composites, synthesized by chemical co-precipitation method, are proposed synthesized to use as highly active heterogeneous Fenton-like catalysts to remove elemental mercury (Hg0) from the simulated flue gases. Inductively coupled plasma-Atomic emission spectrometry (ICP-AES), X-ray diffraction patterns (XRD), scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET) surface area, and X-ray photoelectron spectrometer (XPS) were used to characterize the catalysts. The catalysts were confirmed the presence of the redox pairs Fesurf2+/Fesurf3+ and Cusurf+/Cusurf2+ on the surface of the cubic structure. The performance of heterogeneous Fenton-like reactions for Hg0 removal was evaluated in a lab-scale bubbling reactor at the solution temperature of 50°C. The systematic studies on the effects of different catalysts, H2O2 concentration and solution pH values on Hg0 removal efficiencies were performed. The recycling of the Fe3-xCuxO4 catalysts in Fenton-like solution is stable and Hg0 removal efficiency remain above 90% after 3 cycles. The active hydroxyl radical (OH) generated during heterogeneous Fenton-like reactions was confirmed through electron spin resonance (ESR) spin-trapping technique. The Hg0 removal mechanism has been discussed based on the experimental and analytical results. Copyright © 2015 Elsevier Ltd. All rights reserved.

  5. 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

  6. Two-photon x-ray diffraction

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

    Stohr, J.

    The interference pattern of a circular photon source has long been used to define the optical diffraction limit. Here we show the breakdown of conventional x-ray diffraction theory for the fundamental case of a “source”, consisting of a back-illuminated thin film in a circular aperture. When the conventional spontaneous x-ray scattering by atoms in the film is replaced at high incident intensity by stimulated resonant scattering, the film becomes the source of cloned photon twins and the diffraction pattern becomes self-focused beyond the diffraction limit. Furthermore, the case of cloned photon pairs is compared to and distinguished from entangled photonmore » pairs or biphotons.« less

  7. Two-photon x-ray diffraction

    DOE PAGES

    Stohr, J.

    2017-01-11

    The interference pattern of a circular photon source has long been used to define the optical diffraction limit. Here we show the breakdown of conventional x-ray diffraction theory for the fundamental case of a “source”, consisting of a back-illuminated thin film in a circular aperture. When the conventional spontaneous x-ray scattering by atoms in the film is replaced at high incident intensity by stimulated resonant scattering, the film becomes the source of cloned photon twins and the diffraction pattern becomes self-focused beyond the diffraction limit. Furthermore, the case of cloned photon pairs is compared to and distinguished from entangled photonmore » pairs or biphotons.« less

  8. Reduced graphene oxide aerogel with high-rate supercapacitive performance in aqueous electrolytes

    NASA Astrophysics Data System (ADS)

    Si, Weijiang; Wu, Xiaozhong; Zhou, Jin; Guo, Feifei; Zhuo, Shuping; Cui, Hongyou; Xing, Wei

    2013-05-01

    Reduced graphene oxide aerogel (RGOA) is synthesized successfully through a simultaneous self-assembly and reduction process using hypophosphorous acid and I2 as reductant. Nitrogen sorption analysis shows that the Brunauer-Emmett-Teller surface area of RGOA could reach as high as 830 m2 g-1, which is the largest value ever reported for graphene-based aerogels obtained through the simultaneous self-assembly and reduction strategy. The as-prepared RGOA is characterized by a variety of means such as scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, and X-ray photoelectron spectroscopy. Electrochemical tests show that RGOA exhibits a high-rate supercapacitive performance in aqueous electrolytes. The specific capacitance of RGOA is calculated to be 211.8 and 278.6 F g-1 in KOH and H2SO4 electrolytes, respectively. The perfect supercapacitive performance of RGOA is ascribed to its three-dimensional structure and the existence of oxygen-containing groups.

  9. The synthesis of multifunctional porous honey comb-like La2O3 thin film for supercapacitor and gas sensor applications.

    PubMed

    Yadav, A A; Lokhande, A C; Pujari, R B; Kim, J H; Lokhande, C D

    2016-12-15

    The porous honey comb-like La 2 O 3 thin films have been synthesized using one step spray pyrolysis method. The influence of sprayed solution quantity on properties of La 2 O 3 thin films is studied using X-ray diffraction, Fourier transform spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, optical absorption and Brunauer-Emmett-Teller techniques. Morphology of La 2 O 3 electrode is controlled with sprayed solution quantity. The supercapacitive properties of La 2 O 3 thin film electrode are investigated using cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance techniques. The La 2 O 3 film electrode exhibited the specific capacitance of the 166Fg -1 with 85% stability for the 3000 cycles. The La 2 O 3 film electrode exhibited sensitivity of 68 at 523K for 500ppm CO 2 gas concentration. The possible CO 2 sensing mechanism is discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

  10. Nitrogen-doped 3D reduced graphene oxide/polyaniline composite as active material for supercapacitor electrodes

    NASA Astrophysics Data System (ADS)

    Liu, Zhisen; Li, Dehao; Li, Zesheng; Liu, Zhenghui; Zhang, Zhiyuan

    2017-11-01

    A facile strategy for the fabrication of a nitrogen-doped 3D reduced graphene oxide (N-3D-rGO) macroporous structure is proposed in this paper. The proposed strategy used polystyrene microspheres as the templates and melamine as the nitrogen source. Using β-MnO2 as the oxidant, the as-prepared N-3D-rGO was then composited with polyaniline (PANI) nanowires (denoted as N-3D-rGO/PANI-B). The structure, morphology, and electrochemical properties of the composites were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, Brunauer-Emmett-Teller analysis, scanning electron microscopy, transmission electron microscopy, cyclic voltammetry, charge-discharge test, and electrochemical impedance spectroscopy. Results revealed that the N-3D-rGO/PANI-B composite has a better specific capacity than the composites prepared with 3D-rGO as the support material and peroxydisulfate as the oxidant. These results suggested that N-3D-rGO/PANI-B has potential applications in supercapacitors.

  11. Reduced graphene oxide aerogel with high-rate supercapacitive performance in aqueous electrolytes.

    PubMed

    Si, Weijiang; Wu, Xiaozhong; Zhou, Jin; Guo, Feifei; Zhuo, Shuping; Cui, Hongyou; Xing, Wei

    2013-05-21

    Reduced graphene oxide aerogel (RGOA) is synthesized successfully through a simultaneous self-assembly and reduction process using hypophosphorous acid and I2 as reductant. Nitrogen sorption analysis shows that the Brunauer-Emmett-Teller surface area of RGOA could reach as high as 830 m2 g-1, which is the largest value ever reported for graphene-based aerogels obtained through the simultaneous self-assembly and reduction strategy. The as-prepared RGOA is characterized by a variety of means such as scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, and X-ray photoelectron spectroscopy. Electrochemical tests show that RGOA exhibits a high-rate supercapacitive performance in aqueous electrolytes. The specific capacitance of RGOA is calculated to be 211.8 and 278.6 F g-1 in KOH and H2SO4 electrolytes, respectively. The perfect supercapacitive performance of RGOA is ascribed to its three-dimensional structure and the existence of oxygen-containing groups.

  12. One-pot electrochemical growth of sponge-like polyaniline-intercalated phosphorous-doped graphene oxide on nickel foam as binder-free electrode material of supercapacitor

    NASA Astrophysics Data System (ADS)

    Bigdeli, Hadise; Moradi, Morteza; Borhani, Saeid; Jafari, Elnaz Abbasi; Hajati, Shaaker; Kiani, Mohammad Ali

    2018-06-01

    In this work, phosphor-doped graphene oxide (PGO) was synthesized by chemical technique. Also, the sponge-like PGO@polyaniline nanocomposite (PGO@PANI) film was coated on the nickel foam by one-step electropolymerization. The active materials were then characterized by Fourier transforms infrared spectroscopy, scanning electron microscopy and energy dispersive X-ray spectroscopy, X-ray diffraction, and Brunauer-Emmett-Teller technique. When PANI/PGO was used as supercapacitor electrode, under current density of 1 A/g, the specific capacitance of the prepared PGO@PANI was measured as 603 F/g, which is 6.0 times higher than that of pure PANI (102 F/g). Moreover, capacity stability of the PANI/PGO increased significantly as compared to PANI (65% vs. 44%) after increasing the current density from 1 to 15 A/g. The clear electrochemical performance of PANI/PGO was enhanced owing to the synergistic effect of PGO and PANI. Our results demonstrate that PANI/PGO nanosheet arrays are promising candidate for electrode supercapacitor applications.

  13. Novel synthesis of cobalt/poly vinyl alcohol/gamma alumina nanocomposite for catalytic application

    NASA Astrophysics Data System (ADS)

    Hatamie, Shadie; Ahadian, Mohammad Mahdi; Rashidi, Alimoradeh; Karimi, Ali; Akhavan, Omid

    2017-05-01

    In this manuscript, synthesis of cobalt/poly vinyl alcohol (PVA)/gamma alumina nanocomposite via a simple room temperature, as well as its catalyst performance were explored. Brunauer-Emmett-Teller analysis, X-ray diffraction, X-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy were conducted. The surface area of the polymeric composite was obtained to be 280 m2/g. The cobalt loading on the nanocomposite was measured using inductivity couple plasma. Transmission electron microscopy analysis showed that the size of cobalt crystalline encapsulate inside the polymer was confined to 5 nm. Magnetic property analysis, using vibrating sample magnetometer, confirmed ferromagnetic nature of the composite. Thermo-gravimetric analyses were employed to explain the degradation process for the polymeric base nanocomposite. Temperature-programmed reduction was used to evaluate the structural form of cobalt oxide in nanocomposite. The catalysis activity was determined by Fischer-Tropsch synthesize, which showed a high catalyst selectivity to C2-C4 hydrocarbons.

  14. Studies on the sensing behaviour of nanocrystalline CuGa(2)O(4) towards hydrogen, liquefied petroleum gas and ammonia.

    PubMed

    Biswas, Soumya Kanti; Sarkar, Arpita; Pathak, Amita; Pramanik, Panchanan

    2010-06-15

    In the present article, the gas sensing behaviour of nanocrystalline CuGa(2)O(4) towards H(2), liquefied petroleum gas (LPG) and NH(3) has been reported for the first time. Nanocrystalline powders of CuGa(2)O(4) having average particle sizes in the range of 30-60nm have been prepared through thermal decomposition of an aqueous precursor solution comprising copper nitrate, gallium nitrate and triethanol amine (TEA), followed by calcination at 750 degrees C for 2h. The synthesized nanocrystalline CuGa(2)O(4) powders have been characterised through X-ray diffraction (XRD), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM) study, energy dispersive X-ray (EDX) analysis and BET (Brunauer-Emmett-Teller) surface area measurement. The synthesized CuGa(2)O(4) having spinel structure with specific surface area of 40m(2)/g exhibits maximum sensitivity towards H(2), LPG, and NH(3) at 350 degrees C.

  15. Enhanced photoactivity of BiPO4/(001) facet-dominated square BiOBr flakes by combining heterojunctions with facet engineering effects

    NASA Astrophysics Data System (ADS)

    Shi, Jingzhi; Meng, Xiangying; Hao, Mengjian; Cao, Zhenzhu; He, Weiyan; Gao, Yanfang; Liu, Jinrong

    2018-02-01

    In this study, BiPO4/highly (001) facet exposed square BiOBr flake heterojunction photocatalysts with different molar ratios were fabricated via a two-step method. The synergetic effect of the heterojunction and facet engineering was systematically investigated. The physicochemical properties of the BiPO4/square BiOBr flake composites were characterized based on X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, Brunauer-Emmett-Teller method, X-ray photoelectron spectroscopy, ultraviolet-visible diffuse reflectance spectra, photoluminescence, electrochemical impedance spectroscopy, and the photocurrent response. The BiPO4/square BiOBr flake heterojunction photocatalyst exhibited much higher photocatalytic performance compared with the individual BiPO4 and BiOBr. In particular, the BiPO4/BiOBr composite where P/Br = 1/3 exhibited the highest photocatalytic activity. The intensified separation of photoinduced charges at the p-n heterojunction between the BiPO4 nanoparticle and (001) facet of BiOBr was mainly responsible for the enhanced photoactivity.

  16. Synthesis of BiOCl nanosheets with oxygen vacancies for the improved photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Cai, Yujie; Li, Dongya; Sun, Jingyu; Chen, Mengdie; Li, Yirui; Zou, Zhongwei; Zhang, Hua; Xu, Haiming; Xia, Dongsheng

    2018-05-01

    The square-sharped BiOCl nanosheets with oxygen vacancies were successfully synthesized via a facile hydrothermal route using xylitol as surfactant. The as-prepared BiOCl samples were characterized by Powder X-ray Diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), UV-Vis diffuse reflectance spectra (DRS), Brunauer-Emmett-Teller (BET), X-ray photoelectron spectroscopy (XPS) and Electron spin resonance (ESR). The as-prepared samples were phase-pure with the width and the thickness were about 50-400 nm and 20-50 nm respectively. Besides, the photodegradation performances showed the BiOCl nanosheets with 0.1 g concentration of xylitol (BOC-1) had the best photocatalytic activity under visible light due to its special polycrystalline structure, grain boundary and an optimum concentration of oxygen vacancies. The h+ and radO2- were the two main active species during the photocatalytic process and the possible photocatalytic mechanism was proposed.

  17. 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.

  18. Mesoporous activated carbon from corn stalk core for lithium ion batteries

    NASA Astrophysics Data System (ADS)

    Li, Yi; Li, Chun; Qi, Hui; Yu, Kaifeng; Liang, Ce

    2018-04-01

    A novel mesoporous activated carbon (AC) derived from corn stalk core is prepared via a facile and effective method which including the decomposition and carbonization of corn stalk core under an inert gas atmosphere and further activation process with KOH solution. The mesoporous activated carbon (AC) is characterized by X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) measurements. These biomass waste derived from activated carbon is proved to be promising anode materials for high specific capacity lithium ion batteries. The activated carbon anode possesses excellent reversible capacity of 504 mAh g-1 after 100 cycles at 0.2C. Compared with the unactivated carbon (UAC), the electrochemical performance of activated carbon is significantly improved due to its mesoporous structure.

  19. Impact of Plasma Surface Treatment on Bamboo Charcoal/silver Nanocomposite

    NASA Astrophysics Data System (ADS)

    Vignesh, K.; Vijayalakshmi, K. A.; Karthikeyan, N.

    2016-10-01

    Bamboo charcoal (BC) accompanied silver (Ag) nanocomposite is synthesized through sol-gel method. The produced BC/Ag nanocomposite was surface modified by air and oxygen plasma treatments. Silver ions (Ag+) will serve to improve the antibacterial activity as well as the surface area of BC. Plasma treatment has improved the surface functional groups, crystalline intensity and antibacterial activity of the prepared nanocomposite. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) studies show that Ag nanoparticles have good agreement with BC and the particle size has a mean diameter of 20-40nm. We observe the carboxyl functional groups in Fourier transform infrared spectroscopy (FTIR) after the oxygen plasma treatment. Moreover surface area and adsorption were analyzed by using the Brunauer, Emmett and Teller (BET) surface area (SBET) and UV-Vis spectroscopy.

  20. Preparation and characterization of nanosilica from oil shale ash.

    PubMed

    Li, Jinhong; Qian, Tingting; Tong, Lingxin; Shen, Jie

    2014-05-01

    Nano-sized silica powders was prepared using oil shale ash (OSA) as starting materials. A combined process was proposed for the utilization of OSA in the production of the nanosilica, including three stages: calcination, alkaline leaching and carbon dioxide separation. Effects of the calcining temperature, sodium hydroxide concentration and holding time on the desilication ratio were investigated. The microstructure and morphologies of the nano-sized silica were characterized by X-ray diffraction, transmission electron microscopy, and Brunauer-Emmett-Teller nitrogen-gas adsorption method. The results indicated that the obtained powders with particle size of about 40 nm are homegeneously dispersed and its specific surface area is 387 m2/g. The properties of the nano-sized silica powder meet the requirements of the Chinese Chemical Industry Standard HG/T 3061-1999.

  1. Synthesis of thoria nano-particles at low temperature through base electrogeneration on steel 316L surface: Effect of current density

    NASA Astrophysics Data System (ADS)

    Yousefi, Taher; Torab-Mostaedi, Meisam; Mobtaker, Hossein Ghasemi; Keshtkar, Ali Reza

    2016-10-01

    The strategy developed in this study, offers significant advantages (simplicity and cleanness of method and also a product purity and new morphology of the product) over the conventional routes for the synthesis of ThO2 nanostructure. The effect of current density on morphology was studied. The synthesized powder was characterized by means of Powder X-ray Diffraction (PXRD), Transmission Electron Microscopy (TEM, Phillips EM 2085) Brunauer-Emmett-Teller (BET) and Fourier Transform Infrared (FT-IR) spectroscopy. The results show that the current density has a great effect on the morphology of the samples. The average size of the particles decreases as the applied current density increases and the average size of the samples decreases from 50 to 15 nm when the current density increases from 2 to 5 mA cm-2.

  2. Mesoporous Nickel Oxide (NiO) Nanopetals for Ultrasensitive Glucose Sensing

    NASA Astrophysics Data System (ADS)

    Mishra, Suryakant; Yogi, Priyanka; Sagdeo, P. R.; Kumar, Rajesh

    2018-01-01

    Glucose sensing properties of mesoporous well-aligned, dense nickel oxide (NiO) nanostructures (NSs) in nanopetals (NPs) shape grown hydrothermally on the FTO-coated glass substrate has been demonstrated. The structural study based investigations of NiO-NPs has been carried out by X-ray diffraction (XRD), electron and atomic force microscopies, energy dispersive X-ray (EDX), and X-ray photospectroscopy (XPS). Brunauer-Emmett-Teller (BET) measurements, employed for surface analysis, suggest NiO's suitability for surface activity based glucose sensing applications. The glucose sensor, which immobilized glucose on NiO-NPs@FTO electrode, shows detection of wide range of glucose concentrations with good linearity and high sensitivity of 3.9 μA/μM/cm2 at 0.5 V operating potential. Detection limit of as low as 1 μΜ and a fast response time of less than 1 s was observed. The glucose sensor electrode possesses good anti-interference ability, stability, repeatability & reproducibility and shows inert behavior toward ascorbic acid (AA), uric acid (UA) and dopamine acid (DA) making it a perfect non-enzymatic glucose sensor.

  3. Investigations on structural, optical and magnetic properties of Dy-doped zinc ferrite nanoparticles

    NASA Astrophysics Data System (ADS)

    Vinosha, P. Annie; Deepapriya, S.; Rodney, John. D.; Das, S. Jerome

    2018-04-01

    A persuasive and thriftily feasible homogeneous co-precipitation route was adopted to fabricate dysprosium (Dy) doped zinc ferrite (Zn1-xDyxFe2O4)nanoparticles in order to examine their structural, optical and magnetic properties. Theas-synthesized Zn1-xDyxFe2O4 was studied for its momentous applications in photo-degradation of organic Methylene Blue (MB) dye. The paper marksthe connotation of zinc ferrite nanocatalyst in Photo-Fenton degradation. The chemical composition of dysprosium has a decisive feature of this research work. From X-ray diffraction analysis (XRD), spinel phase formation of theas-synthesized Zn1-xDyxFe2O4 nanoparticles was observedand the crystallite size was foundto increase as the doping concentration increased. Theabsorption bands peaked between 600-400 cm-l waspragmatic by Fourier Transform Infrared spectral analysis (FTIR). Transmission Electron Microscopy (TEM) micrograph elucidated the morphology and the speck size of as-synthesized nanoparticles. Surface area and pore size were determined by Brunauer-Emmett-Teller (BET) technique.

  4. Coherent x-ray diffraction imaging with nanofocused illumination.

    PubMed

    Schroer, C G; Boye, P; Feldkamp, J M; Patommel, J; Schropp, A; Schwab, A; Stephan, S; Burghammer, M; Schöder, S; Riekel, C

    2008-08-29

    Coherent x-ray diffraction imaging is an x-ray microscopy technique with the potential of reaching spatial resolutions well beyond the diffraction limits of x-ray microscopes based on optics. However, the available coherent dose at modern x-ray sources is limited, setting practical bounds on the spatial resolution of the technique. By focusing the available coherent flux onto the sample, the spatial resolution can be improved for radiation-hard specimens. A small gold particle (size <100 nm) was illuminated with a hard x-ray nanobeam (E=15.25 keV, beam dimensions approximately 100 x 100 nm2) and is reconstructed from its coherent diffraction pattern. A resolution of about 5 nm is achieved in 600 s exposure time.

  5. Insights into the dominant factors of porous gold for CO oxidation

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

    Kameoka, Satoshi, E-mail: kameoka@tagen.tohoku.ac.jp; Miyamoto, Kanji; Tanabe, Toyokazu

    2016-01-21

    Three different porous Au catalysts that exhibit high catalytic activity for CO oxidation were prepared by the leaching of Al from an intermetallic compound, Al{sub 2}Au, with 10 wt. %-NaOH, HNO{sub 3}, or HCl aqueous solutions. The catalysts were investigated using Brunauer-Emmett-Teller measurements, synchrotron X-ray powder diffraction, hard X-ray photoelectron spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy (TEM). Broad diffraction peaks generated during the leaching process correlated with high activity for all the porous Au catalysts. CO oxidation catalyzed by porous Au leached with NaOH and HNO{sub 3} is considered to be dominated by different mechanisms atmore » low (< 320 K) and high (> 370 K) temperatures. Activity in the low-temperature region is mainly attributed to the perimeter interface between residual Al species (AlO{sub x}) and porous Au, whereas activity in the high-temperature region results from a high density of lattice defects such as twins and dislocations, which were evident from diffraction peak broadening and were observed with high-resolution TEM in the porous Au leached with NaOH. It is proposed that atoms located at lattice defects on the surfaces of porous Au are the active sites for catalytic reactions.« less

  6. Dynamics analysis of extraction of manganese intensified by electric field

    NASA Astrophysics Data System (ADS)

    Ma, Wenrui; Tao, Changyuan; Li, Huizhan; Liu, Zuohua; Liu, Renlong

    2018-06-01

    In this study, a process reinforcement technology for leaching process of pyrolusite was developed. The electric field was introduced to decrease reaction temperature and improve the leaching rate of pyrolusite. The mechanisms of electric field intensifying leaching process of pyrolusite were investigated through X-ray diffraction (XRD), and Brunauer Emmett Teller (BET) in detail. The results showed that the electric field could decrease obviously the apparent activation energy of leaching process of pyrolusite. The apparent activation energy of the leaching of pyrolusite intensified by electric field was calculated to be 53.76 kJ.mol-1. In addition, the leaching efficiency of manganese was effectively increased by 10% to 20% than that without electric field under the same conditions. This was because that the electron conduit between Fe (II)/Fe (III) and pyrite was dredged effectively by electric field.

  7. Nanotubular polyaniline electrode for supercapacitor application

    NASA Astrophysics Data System (ADS)

    Athira, A. R.; Vimuna, V. M.; Vidya, K.; Xavier, T. S.

    2018-05-01

    Polyaniline(PANI) nanotubes have been successfully synthesised at room temperature by the chemical oxidative polymerization of aniline with Ammoniumpersulphate(APS) in aqueous acetic acid. Chemically synthesised PANI nanotubes were characterized using Field emission scanning electron microscopy(FESEM), Brunauer - Emmett-Teller (BET) analysis, X ray diffraction analysis (XRD) and Fourier transform infrared spectroscopy (FTIR). The super capacitive performance of the synthesised PANI nanotubes was tested using cyclic voltammetry (CV) technique in H2SO4 electrolyte with in potential range of -0.2 to 0.8V. The effect of scan rates on specific capacitance of PANI electrode was studied. The highest specific capacitance of 232.2Fg-1 was obtained for the scan rate of 5mVs-1. This study suggests that the synthesized PANI nanotubes are excellent candidate for developing electrode materials for supercapacitors.

  8. Diffusion of CO2 in Large Crystals of Cu-BTC MOF.

    PubMed

    Tovar, Trenton M; Zhao, Junjie; Nunn, William T; Barton, Heather F; Peterson, Gregory W; Parsons, Gregory N; LeVan, M Douglas

    2016-09-14

    Carbon dioxide adsorption in metal-organic frameworks has been widely studied for applications in carbon capture and sequestration. A critical component that has been largely overlooked is the measurement of diffusion rates. This paper describes a new reproducible procedure to synthesize millimeter-scale Cu-BTC single crystals using concentrated reactants and an acetic acid modulator. Microscopic images, X-ray diffraction patterns, Brunauer-Emmett-Teller surface areas, and thermogravimetric analysis results all confirm the high quality of these Cu-BTC single crystals. The large crystal size aids in the accurate measurement of micropore diffusion coefficients. Concentration-swing frequency response performed at varying gas-phase concentrations gives diffusion coefficients that show very little dependence on the loading up to pressures of 0.1 bar. The measured micropore diffusion coefficient for CO2 in Cu-BTC is 1.7 × 10(-9) m(2)/s.

  9. Hydrogen sensing properties of nanocomposite graphene oxide/Co-based metal organic frameworks (Co-MOFs@GO)

    NASA Astrophysics Data System (ADS)

    Fardindoost, Somayeh; Hatamie, Shadie; Iraji Zad, Azam; Razi Astaraei, Fatemeh

    2018-01-01

    This paper reports on hydrogen sensing based graphene oxide hybrid with Co-based metal organic frameworks (Co-MOFs@GO) prepared by the hydrothermal process. The texture and morphology of the hybrid were characterized by powder x-ray diffraction, scanning electron microscopy and Brunauer-Emmett-Teller analysis. Porous flower like structures assembled from Co-MOFs and GO flakes with sufficient specific surface area are obtained, which are ideal for gas molecules diffusion and interactions. Sensing performance of Co-MOFs@GO were tested and also improved by sputtering platinum (Pt) as a catalyst. The Pt-sputtered Co-MOFs@GO show outstanding hydrogen resistive-sensing with response and recovery times below 12 s at 15 °C. Also, they show stable, repeatable and selective responses to the target gas which make it suitable for the development of a high performance hydrogen sensor.

  10. 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.

  11. 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

  12. X-Ray Diffraction on NIF

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

    Eggert, J H; Wark, J

    2012-02-15

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

  13. Silica nanoparticles produced by DC arc plasma from a solid raw materials

    NASA Astrophysics Data System (ADS)

    Kosmachev, P. V.; Vlasov, V. A.; Skripnikova, N. K.

    2017-05-01

    Plasma synthesis of SiO2 nanoparticles in experimental atmospheric pressure plasma reactor on the basis of DC arc plasma generator was presented in this paper. Solid high-silica raw materials such as diatomite from Kamyshlovskoye deposit in Russia, quartzite from Chupinskoye deposit in Russia and milled window glass were used. The obtained nanoparticles were characterized based on their morphology, chemical composition and size distribution. Scanning electron microscopy, laser diffractometry, nitrogen absorption (Brunauer-Emmett-Teller method), X-ray photoelectron spectroscopy and energy-dispersive X-ray spectroscopy were used to characterize the synthesized products. The obtained silica nanoparticles are agglomerated, have spherical shape and primary diameters between 10-300 nm. All samples of synthesized nanopowders were compared with commercial nanopowders.

  14. Structure and Properties of Sio2 Nanopowder Obtained From High-Silica Raw Materials by Plasma Method

    NASA Astrophysics Data System (ADS)

    Kosmachev, P. V.; Vlasov, V. A.; Skripnikova, N. K.

    2017-06-01

    The paper presents a plasma-assisted generation of nanodisperse powder obtained from diatomite, a natural high-silica material. The structure and properties of the obtained material are investigated using the transmission electron microscopy, energy dispersive X-Ray spectroscopy, infrared and X-ray photoelectron spectroscopies, and Brunauer-Emmett-Teller method. It is clearly shown that the obtained SiO2 nanoparticles are spherical, polydisperse and represented in the form of agglomerates. The specific surface of this nanopowder is 32 m2/g. Thermodynamic modeling of the plasma-assisted process is used to obtain the equilibrium compositions of condensed and gaseous reaction products. The plasma process is performed within the 300-5000 K temperature range.

  15. Chemical Ni-C Bonding in Ni-Carbon Nanotube Composite by a Microwave Welding Method and Its Induced High-Frequency Radar Frequency Electromagnetic Wave Absorption.

    PubMed

    Sha, Linna; Gao, Peng; Wu, Tingting; Chen, Yujin

    2017-11-22

    In this work, a microwave welding method has been used for the construction of chemical Ni-C bonding at the interface between carbon nanotubes (CNTs) and metal Ni to provide a different surface electron distribution, which determined the electromagnetic (EM) wave absorption properties based on a surface plasmon resonance mechanism. Through a serial of detailed examinations, such as X-ray diffraction, scanning electron microscopy, transmission electron microscopy, high-resolution transmission electron microscopy, X-ray photoelectron spectroscopy, and Raman spectrum, the as-expected chemical Ni-C bonding between CNTs and metal Ni has been confirmed. And the Brunauer-Emmett-Teller and surface zeta potential measurements uncovered the great evolution of structure and electronic density compared with CNTs, metal Ni, and Ni-CNT composite without Ni-C bonding. Correspondingly, except the EM absorption due to CNTs and metal Ni in the composite, another wide and strong EM absorption band ranging from 10 to 18 GHz was found, which was induced by the Ni-C bonded interface. With a thinner thickness and more exposed Ni-C interfaces, the Ni-CNT composite displayed less reflection loss.

  16. Three-dimensional Co3O4@MWNTs nanocomposite with enhanced electrochemical performance for nonenzymatic glucose biosensors and biofuel cells

    NASA Astrophysics Data System (ADS)

    Jiao, Kailong; Jiang, Yu; Kang, Zepeng; Peng, Ruiyun; Jiao, Shuqiang; Hu, Zongqian

    2017-12-01

    Three-dimensional nanoarchitectures of Co3O4@multi-walled carbon nanotubes (Co3O4@MWNTs) were synthesized via a one-step process with hydrothermal growth of Co3O4 nanoparticles onto MWNTs. The structure and morphology of the Co3O4@MWNTs were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller, scanning electron microscopy and transmission electron microscopy. The electrocatalytic mechanism of the Co3O4@MWNTs was studied by X-ray photoelectron spectroscopy and cyclic voltammetry. Co3O4@MWNTs exhibited high electrocatalytic activity towards glucose oxidation in alkaline medium and could be used in nonenzymatic electrochemical devices for glucose oxidation. The open circuit voltage of the nonenzymatic glucose/O2 fuel cell was 0.68 V, with a maximum power density of 0.22 mW cm-2 at 0.30 V. The excellent electrochemical properties, low cost, and facile preparation of Co3O4@MWNTs demonstrate the potential of strongly coupled oxide/nanocarbon hybrid as effective electrocatalyst in glucose fuel cells and biosensors.

  17. Effect of calcination temperatures on microstructures and photocatalytic activity of tungsten trioxide hollow microspheres.

    PubMed

    Yu, Jiaguo; Qi, Lifang; Cheng, Bei; Zhao, Xiufeng

    2008-12-30

    Tungsten trioxide hollow microspheres were prepared by immersing SrWO4 microspheres in a concentrated HNO3 solution, and then calcined at different temperatures. The prepared tungsten oxide samples were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectra, differential thermal analysis-thermogravimetry, UV-visible spectrophotometry, scanning electron microscopy, N2 adsorption/desorption measurements. The photocatalytic activity of the samples was evaluated by photocatalytic decolorization of rhodamine B aqueous solution under visible-light irradiation. It was found that with increasing calcination temperatures, the average crystallite size and average pore size increased, on the contrary, Brunauer-Emmett-Teller-specific surface areas decreased. However, pore volume and porosity increased firstly, and then decreased. Increasing calcination temperatures resulted in the changes of surface morphology of hollow microspheres. The un-calcined and 300 degrees C-calcined samples showed higher photocatalytic activity than other samples. At 400 degrees C, the photocatalytic activity decreased greatly due to the decrease of specific surface areas. At 500 degrees C, the photocatalytic activity of the samples increased again due to the junction effect of two phases.

  18. Structure-property-composition relationships in doped zinc oxides: enhanced photocatalytic activity with rare earth dopants.

    PubMed

    Goodall, Josephine B M; Illsley, Derek; Lines, Robert; Makwana, Neel M; Darr, Jawwad A

    2015-02-09

    In this paper, we demonstrate the use of continuous hydrothermal flow synthesis (CHFS) technology to rapidly produce a library of 56 crystalline (doped) zinc oxide nanopowders and two undoped samples, each with different particle properties. Each sample was produced in series from the mixing of an aqueous stream of basic zinc nitrate (and dopant ion or modifier) solution with a flow of superheated water (at 450 °C and 24.1 MPa), whereupon a crystalline nanoparticle slurry was rapidly formed. Each composition was collected in series, cleaned, freeze-dried, and then characterized using analytical methods, including powder X-ray diffraction, transmission electron microscopy, Brunauer-Emmett-Teller surface area measurement, X-ray photoelectron spectroscopy, and UV-vis spectrophotometry. Photocatalytic activity of the samples toward the decolorization of methylene blue dye was assessed, and the results revealed that transition metal dopants tended to reduce the photoactivity while rare earth ions, in general, increased the photocatalytic activity. In general, low dopant concentrations were more beneficial to having greater photodecolorization in all cases.

  19. Facile Synthesis of Self-Assembled Flower-Like Mesoporous Zinc Oxide Nanoflakes for Energy Applications

    NASA Astrophysics Data System (ADS)

    Saranya, P. E.; Selladurai, S.

    Flower-shaped self-assembled zinc oxide (ZnO) nanoflakes were successfully synthesized via a temperature-controlled hydrothermal method. The crystallinity and phase formation of the compound were determined from powder X-ray diffraction (PXRD) result. Surface morphology investigations reveal the self-assembled ZnO nanoflakes to form a spherical flower-like structure. In addition, the particle size was determined from high-resolution transmission electron microscope measurement as 18nm which is in accord with XRD and UV results. X-ray photo electron spectroscopy studies reveal the chemical composition and oxidation state of the ZnO nanoparticle. The specific surface area was calculated, and mesoporous nature was confirmed using Brunauer-Emmett-Teller analysis. Results support the superior interaction between the electrode and electrolyte ions through surface pores. Capacitive performance of the ZnO electrode material was determined using cyclic voltammetry and galvanostatic charge/discharge studies, and a maximum specific capacitance of 322F/g was obtained at 5mV/sec. Electrochemical impedance spectrum reveals the materials fast charge transfer kinetics.

  20. Hydrogen evolution from aqueous-phase photocatalytic reforming of ethylene glycol over Pt/TiO2 catalysts: Role of Pt and product distribution

    NASA Astrophysics Data System (ADS)

    Li, Fuying; Gu, Quan; Niu, Yu; Wang, Renzhang; Tong, Yuecong; Zhu, Shuying; Zhang, Hualei; Zhang, Zizhong; Wang, Xuxu

    2017-01-01

    Pt nanoparticles were loaded on anatase TiO2 by the photodeposition method to investigate their photocatalytic activity for H2 evolution in an aqueous solution containing a certain amount of ethylene glycol (EG) as the sacrificial agent. The surface properties and chemical states of the Pt/TiO2 sample were characterized by X-ray powder diffraction analysis, Brunauer-Emmett-Teller surface area analysis, transmission electron microscopy, X-ray photoelectron spectroscopy, electron paramagnetic resonance, and electrochemical resistance. The aqueous-phase photocatalytic EG reforming using Pt/TiO2 and anatase TiO2 generated not only H2 and CO2, but also CO, CH4, C2H6, and C2H4. Moreover, the amount of formate and acetate complexes in the solution increased gradually. The EG adsorption and gas-phase intermediates during photocatalytic reaction processes were investigated by the in situ FTIR spectrum. Finally, the photocatalytic EG reforming reaction mechanism was elucidated. This helped to better understand the role of a sacrificial agent in a photocatalytic hydrogen production.

  1. Preparation of RHA-silica/graphene oxide nanocomposite for removal of nickel ions from water

    NASA Astrophysics Data System (ADS)

    Tien, Tran Thi Thuy; Tu, Tran Hoang; Thao, Huynh Nguyen Phuong; Hieu, Nguyen Huu

    2017-09-01

    In this study, silica was synthesized from rice husk ash (RHA-SiO2) by precipitation method. Graphene oxide (GO) was prepared by modified Hummers method. RHA-SiO2/GO nanocomposite was fabricated by in-situ one-step method using 3-Aminopropyltriethoxysilane (APS) as a coupling agent. The nanocomposite was characterized by using X-ray Fluorescence, X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy, Raman spectroscopy, and Brunauer-Emmett-Teller (BET) specific surface area. The adsorption of RHA-SiO2/GO for Ni2+ ions from water was investigated and compared with the precursors. Ultraviolet-visible (UV-Vis) spectroscopy was used to quantify the amount of the initial and the residual Ni2+ concentration. The maximum adsorption capacity of the nanocomposite for Ni2+ calculated from Langmuir isotherm model, which was 256.4 mg/g. In addition, the adsorption data were well-fitted to the pseudo-second-order kinetic equation. Accordingly, this study demonstrated that RHA-SiO2/GO could be used as a highly efficient adsorbent for removal Ni2+ ions from aqueous solution.

  2. Adsorption of an anionic dye on a novel low-cost mesoporous adsorbent: kinetic, thermodynamic and isotherm studies

    NASA Astrophysics Data System (ADS)

    Msaad, Asmaa; Belbahloul, Mounir; Zouhri, Abdeljalil

    2018-05-01

    Our activated carbon was prepared successfully using phosphoric acid as an activated agent. The activated carbon was characterized by Scanning Electron Micrograph (SEM), Brunauer-Emmett- Teller (BET), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The aim of our study is to evaluate the adsorption capacity of Methyl Orange (MO) on Ziziphus lotus activated carbon. Adsorption isotherms were studied according to Langmuir and Freundlich Model, and adsorption kinetics according to pseudo-first and second-order. Results show that the maximum adsorption was reached in the first 10min at ambient temperature with a yield of 96.31%. The Langmuir isotherm shows a correlation coefficient of 99.4 % higher than Freundlich model and the adsorption kinetic model follow a pseudo-second-order with a maximum adsorption capacity of 769.23 mg/g. FTIR and X-Ray spectroscopy indicate that our activated carbon has an amorphous structure with the presence of functional groups, where BET analysis revealed a high surface area of 553 mg/g, which facilitate the adsorption process

  3. Nanostructured Silica/Gold-Cellulose-Bonded Amino-POSS Hybrid Composite via Sol-Gel Process and Its Properties.

    PubMed

    Ramesh, Sivalingam; Kim, Heung Soo; Lee, Young-Jun; Hong, Gwang-Wook; Kim, Joo-Hyung

    2017-12-01

    It is demonstrated in this paper that silica nanoparticles coated with core/shell gold provide efficient thermal, optical, and morphological properties with respect to the cellulose-polyhedral oligomeric silsesquioxanes (POSS) hybrid system. The one-step synthesis of a silica/gold nanocomposite is achieved with a simultaneous hydrolysis and reduction of gold chloride in the presence of formic acid, and the trimethoxysilane group acts as a silica precursor. The focus here comprises the synthesis of cellulose-POSS and silica/gold hybrid nanocomposites using the following two methods: (1) an in situ sol-gel process and (2) a polyvinyl alcohol/tetrakis (hydroxymethyl)phosphonium chloride process. Accordingly, the silica/gold core/shell nanoparticles are synthesized. The growth and attachment of the gold nanoparticles onto the functionalized surface of the silica at the nanometer scale is achieved via both the sol-gel and the tetrakis (hydroxymethyl) phosphonium chloride processes. The cellulose-POSS-silica/gold nanocomposites are characterized according to Fourier transformed infrared spectroscopy, Raman, X-ray diffraction, UV, photoluminescence, SEM, energy-dispersive X-ray spectroscopy, TEM, thermogravimetric, and Brunauer-Emmett-Teller analyses.

  4. Nanostructured Silica/Gold-Cellulose-Bonded Amino-POSS Hybrid Composite via Sol-Gel Process and Its Properties

    NASA Astrophysics Data System (ADS)

    Ramesh, Sivalingam; Kim, Heung Soo; Lee, Young-June; Hong, Gwang-Wook; Kim, Joo-Hyung

    2017-06-01

    It is demonstrated in this paper that silica nanoparticles coated with core/shell gold provide efficient thermal, optical, and morphological properties with respect to the cellulose-polyhedral oligomeric silsesquioxanes (POSS) hybrid system. The one-step synthesis of a silica/gold nanocomposite is achieved with a simultaneous hydrolysis and reduction of gold chloride in the presence of formic acid, and the trimethoxysilane group acts as a silica precursor. The focus here comprises the synthesis of cellulose-POSS and silica/gold hybrid nanocomposites using the following two methods: (1) an in situ sol-gel process and (2) a polyvinyl alcohol/tetrakis (hydroxymethyl)phosphonium chloride process. Accordingly, the silica/gold core/shell nanoparticles are synthesized. The growth and attachment of the gold nanoparticles onto the functionalized surface of the silica at the nanometer scale is achieved via both the sol-gel and the tetrakis (hydroxymethyl) phosphonium chloride processes. The cellulose-POSS-silica/gold nanocomposites are characterized according to Fourier transformed infrared spectroscopy, Raman, X-ray diffraction, UV, photoluminescence, SEM, energy-dispersive X-ray spectroscopy, TEM, thermogravimetric, and Brunauer-Emmett-Teller analyses.

  5. Fe2O3/ZnO/ZnFe2O4 composites for the efficient photocatalytic degradation of organic dyes under visible light

    NASA Astrophysics Data System (ADS)

    Li, Xiaojuan; Jin, Bo; Huang, Jingwen; Zhang, Qingchun; Peng, Rufang; Chu, Shijin

    2018-06-01

    In this study, novel ternary Fe2O3/ZnO/ZnFe2O4 (ZFO) composites were successfully prepared through a simple hydrothermal reaction with subsequent thermal treatment. The as-prepared products were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Brunauer-Emmett-Teller (BET) analysis, Barrett-Joyner-Halenda (BJH) measurement, and UV-vis diffuse reflectance spectroscopy (UV-vis DRS). The photocatalytic degradation of rhodamine B (Rh B) under visible light irradiation indicated that the ZFO composites calcined at 500 °C has the best photocatalytic activity (the photocatalytic degradation efficiency can reach up to 95.7% within 60 min) and can maintain a stable photocatalytic degradation efficiency for at least three cycles. In addition, the photocatalytic activity of ZFO composites toward dye decomposition follows the order cationic Rh B > anionic methyl orange. Finally, using different scavengers, superoxide and hydroxyl radicals were identified as the primary active species during the degradation reaction of Rh B.

  6. Synthesis, characterization and adsorptive performance of MgFe2O4 nanospheres for SO2 removal.

    PubMed

    Zhao, Ling; Li, Xinyong; Zhao, Qidong; Qu, Zhenping; Yuan, Deling; Liu, Shaomin; Hu, Xijun; Chen, Guohua

    2010-12-15

    A type of uniform Mg ferrite nanospheres with excellent SO(2) adsorption capacity could be selectively synthesized via a facile solvothermal method. The size of the MgFe(2)O(4) nanospheres was controlled to be 300-400 nm in diameter. The structural, textural, and surface properties of the adsorbent have been fully characterized by a variety of techniques (Brunauer-Emmett-Teller, BET; X-ray diffraction analysis, XRD; scanning electron microscopy, SEM; and energy-dispersive X-ray spectroscopy, EDS). The valence states and the surface chemical compositions of MgFe(2)O(4) nanospheres were further identified by X-ray photoelectron spectroscopy (XPS). The behaviors of SO(2) oxidative adsorption on MgFe(2)O(4) nanospheres were studied using Fourier transform infrared spectroscopy (FTIR). Both the sulfite and sulfate species could be formed on the surface of MgFe(2)O(4). The adsorption equilibrium isotherm of SO(2) was analyzed using a volumetric method at 298 K and 473 K. The results indicate that MgFe(2)O(4) nanospheres possess a good potential as the solid-state SO(2) adsorbent for applications in hot fuel gas desulfurization. Copyright © 2010 Elsevier B.V. All rights reserved.

  7. Facile fabrication of CuO-Pb2O3 nanophotocatalyst for efficient degradation of Rose Bengal dye under visible light irradiation

    NASA Astrophysics Data System (ADS)

    Kamaraj, Eswaran; Somasundaram, Sivaraman; Balasubramani, Kavitha; Eswaran, Muthu Prema; Muthuramalingam, Rajarajan; Park, Sanghyuk

    2018-03-01

    A p-type CuO/n-type Pb2O3 heterojunction photocatalyst was prepared by a simple wet chemical process and the photocatalytic ability was evaluated for the degradation of Rose Bengal (RB) under visible light irradiation. Synthesized nanocatalysts were characterized by X-ray diffraction (XRD), UV-vis diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Energy-dispersive X-ray spectroscopy (EDS), Brunauer-Emmett-Teller (BET) surface area analysis, and X-ray photoelectron spectroscopy (XPS). The p-n heterojunction of CuO-Pb2O3 nanostructures can promote the light absorption capability of photocatalyst and charge separation of electron-hole pairs. Photodegradation assays showed that the addition of CuO effectively enhanced the photocatalytic activity of CuO-Pb2O3 under visible light irradiation (λmax > 420 nm). Compared with pure Pb2O3 and CuO, the CuO-Pb2O3 exhibited significantly enhanced photocatalytic degradation activity. The reaction rate constant of CuO-Pb2O3 is 0.092 min-1, which is much higher than those of CuO (0.073 min-1) and Pb2O3 (0.045 min-1).

  8. X-ray diffraction on radioactive materials

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

    Schiferl, D.; Roof, R.B.

    1978-01-01

    X-ray diffraction studies on radioactive materials are discussed with the aim of providing a guide to new researchers in the field. Considerable emphasis is placed on the safe handling and loading of not-too-exotic samples. Special considerations such as the problems of film blackening by the gamma rays and changes induced by the self-irradiation of the sample are covered. Some modifications of common diffraction techniques are presented. Finally, diffraction studies on radioactive samples under extreme conditions are discussed, with primary emphasis on high-pressure studies involving diamond-anvil cells.

  9. Preparation and catalytic performance of copper-containing magnetic catalysts for degradation of azo dye (direct violet).

    PubMed

    Duan, Qiannan; Lee, Jianchao; Chen, Han; Zheng, Yunyun

    2017-12-01

    A novel magnetically separable magnetic activated carbon supporting-copper (MCAC) catalyst for catalytic wet peroxide oxidation (CWPO) was prepared by chemical impregnation. The prepared samples were characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) method, and scanning electron microscopy (SEM) equipped with energy dispersive spectrometry (EDS). The catalytic performance of the catalysts was evaluated by direct violet (D-BL) degradation in CWPO experiments. The influence of preparative and operational parameters (dipping conditions, calcination temperature, catalyst loading H 2 O 2 dosage, pH, reaction temperature, additive salt ions and initial D-BL concentration) on degradation performance of CWPO process was investigated. The resulting MCAC catalyst showed higher reusability in direct violet oxidation than the magnetic activated carbon (MAC). Besides, dynamic tests also showed the maximal degradation rate reached 90.16% and its general decoloring ability of MCAC was 34 mg g -1 for aqueous D-BL.

  10. Hydrogen storage behaviors of Ni-doped graphene Oxide/MIL-101 hybrid composites.

    PubMed

    Lee, Seul-Yi; Park, Soo-Jin

    2013-01-01

    In this work, Ni-doped graphene oxide/MIL-101 hybrid composites (Ni--GO/MIL) were prepared to investigate their hydrogen storage behaviors. Ni--GO/MIL was synthesized by adding Ni--GO in situ during the synthesis of MIL-101 using a hydrothermal process, which was conducted by conventional convection heating with Cr(III) ion as a metal center and telephthalic acid as organic ligands. The crystalline structures and morphologies were measured by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The specific surface area and micropore volume were investigated by N2/77 K adsorption isotherms using the Brunauer-Emmett-Teller (BET) method and Dubinin-Radushkevic (D-R) equation, respectively. The hydrogen storage capacity was investigated by BEL-HP at 77 K and 1 bar. The obtained results show that Ni--GO/MIL presents new directions for achieving novel hybrid materials with higher hydrogen storage capacity.

  11. Sonochemically synthesized MnO2 nanoparticles as electrode material for supercapacitors.

    PubMed

    Gnana Sundara Raj, Balasubramaniam; Asiri, Abdullah M; Qusti, Abdullah H; Wu, Jerry J; Anandan, Sambandam

    2014-11-01

    In this study, manganese oxide (MnO2) nanoparticles were synthesized by sonochemical reduction of KMnO4 using polyethylene glycol (PEG) as a reducing agent as well as structure directing agent under room temperature in short duration of time and characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) analysis. A supercapacitor device constructed using the ultrasonically-synthesized MnO2 nanoparticles showed maximum specific capacitance (SC) of 282Fg(-1) in the presence of 1M Ca(NO3)2 as an electrolyte at a current density of 0.5mAcm(-2) in the potential range from 0.0 to 1.0V and about 78% of specific capacitance was retained even after 1000 cycles indicating its high electrochemical stability. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Mesoporous MnCo2O4 with a flake-like structure as advanced electrode materials for lithium-ion batteries and supercapacitors.

    PubMed

    Mondal, Anjon Kumar; Su, Dawei; Chen, Shuangqiang; Ung, Alison; Kim, Hyun-Soo; Wang, Guoxiu

    2015-01-19

    A mesoporous flake-like manganese-cobalt composite oxide (MnCo2O4) is synthesized successfully through the hydrothermal method. The crystalline phase and morphology of the materials are characterized by X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, and Brunauer-Emmett-Teller methods. The flake-like MnCo2O4 is evaluated as the anode material for lithium-ion batteries. Owing to its mesoporous nature, it exhibits a high reversible capacity of 1066 mA h g(-1), good rate capability, and superior cycling stability. As an electrode material for supercapacitors, the flake-like MnCo2O4 also demonstrates a high supercapacitance of 1487 F g(-1) at a current density of 1 A g(-1), and an exceptional cycling performance over 2000 charge/discharge cycles. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Sol-gel Synthesis, Photo- and Electrocatalytic Properties of Mesoporous TiO2 Modified with Transition Metal Ions

    NASA Astrophysics Data System (ADS)

    Smirnova, N.; Petrik, I.; Vorobets, V.; Kolbasov, G.; Eremenko, A.

    2017-03-01

    Mesoporous nanosized titania films modified with Co2+, Ni2+, Mn3+, and Cu2+ ions have been produced by templated sol-gel method and characterized by optical spectroscopy, X-ray diffraction (XRD), and Brunauer, Emmett, and Teller (BET) surface area measurement. Band gap energy and the position of flat band potentials were estimated by photoelectrochemical measurements. The films doped with transition metals possessed higher photocurrent quantum yield, as well as photo- and electrochemical activity compared to undoped samples. Mn+/TiO2 (M-Co, Ni, Mn, Cu) electrodes with low dopant content demonstrate high efficiency in electrocatalytic reduction of dissolved oxygen. Polarization curves of TiO2, TiO2/Ni2+, TiO2/Co2+/3+, and TiO2/Mn3+ electrodes contain only one current wave (oxygen reduction current). It means that reaction proceeds without the formation of an intermediate product H2O2.

  14. 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

  15. 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

  16. 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

  17. 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

  18. Enhancing resolution in coherent x-ray diffraction imaging.

    PubMed

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

    2016-12-14

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

  19. 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.

  20. 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

  1. 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.

  2. 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.

  3. Diffraction enhanced kinetic depth X-ray imaging

    NASA Astrophysics Data System (ADS)

    Dicken, A.

    An increasing number of fields would benefit from a single analytical probe that can characterise bulk objects that vary in morphology and/or material composition. These fields include security screening, medicine and material science. In this study the X-ray region is shown to be an effective probe for the characterisation of materials. The most prominent analytical techniques that utilise X-radiation are reviewed. The study then focuses on methods of amalgamating the three dimensional power of kinetic depth X-ray (KDFX) imaging with the materials discrimination of angular dispersive X-ray diffraction (ADXRD), thus providing KDEX with a much needed material specific counterpart. A knowledge of the sample position is essential for the correct interpretation of diffraction signatures. Two different sensor geometries (i.e. circumferential and linear) that are able to collect end interpret multiple unknown material diffraction patterns and attribute them to their respective loci within an inspection volume are investigated. The circumferential and linear detector geometries are hypothesised, simulated and then tested in an experimental setting with the later demonstrating a greater ability at discerning between mixed diffraction patterns produced by differing materials. Factors known to confound the linear diffraction method such as sample thickness and radiation energy have been explored and quantified with a possible means of mitigation being identified (i.e. via increasing the sample to detector distance). A series of diffraction patterns (following the linear diffraction approach) were obtained from a single phantom object that was simultaneously interrogated via KDEX imaging. Areas containing diffraction signatures matched from a threat library have been highlighted in the KDEX imagery via colour encoding and match index is inferred by intensity. This union is the first example of its kind and is called diffraction enhanced KDEX imagery. Finally an additional

  4. Remote X-Ray Diffraction and X-Ray Fluorescence Analysis on Planetary Surfaces

    NASA Technical Reports Server (NTRS)

    Blake, David F.; DeVincenzi, D. (Technical Monitor)

    1999-01-01

    The legacy of planetary X-ray Diffraction (XRD) and X-ray Fluorescence (XRF) began in 1960 when W. Parish proposed an XRD instrument for deployment on the moon. The instrument was built and flight qualified, but the Lunar XRD program was cancelled shortly before the first human landing in 1969. XRF chemical data have been collected in situ by surface landers on Mars (Viking 1 & 2, Pathfinder) and Venus (Venera 13 & 14). These highly successful experiments provide critical constraints on our current understanding of surface processes and planetary evolution. However, the mineralogy, which is more critical to planetary surface science than simple chemical analysis, will remain unknown or will at best be imprecisely constrained until X-ray diffraction (XRD) data are collected. Recent progress in X-ray detector technology allows the consideration of simultaneous XRD (mineralogic analysis) and high-precision XRF (elemental analysis) in systems miniaturized to the point where they can be mounted on fixed landers or small robotic rovers. There is a variety of potential targets for XRD/XRF equipped landers within the solar system, the most compelling of which are the poles of the moon, the southern highlands of Mars and Europa.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. Wavefront aberrations of x-ray dynamical diffraction beams.

    PubMed

    Liao, Keliang; Hong, Youli; Sheng, Weifan

    2014-10-01

    The effects of dynamical diffraction in x-ray diffractive optics with large numerical aperture render the wavefront aberrations difficult to describe using the aberration polynomials, yet knowledge of them plays an important role in a vast variety of scientific problems ranging from optical testing to adaptive optics. Although the diffraction theory of optical aberrations was established decades ago, its application in the area of x-ray dynamical diffraction theory (DDT) is still lacking. Here, we conduct a theoretical study on the aberration properties of x-ray dynamical diffraction beams. By treating the modulus of the complex envelope as the amplitude weight function in the orthogonalization procedure, we generalize the nonrecursive matrix method for the determination of orthonormal aberration polynomials, wherein Zernike DDT and Legendre DDT polynomials are proposed. As an example, we investigate the aberration evolution inside a tilted multilayer Laue lens. The corresponding Legendre DDT polynomials are obtained numerically, which represent balanced aberrations yielding minimum variance of the classical aberrations of an anamorphic optical system. The balancing of classical aberrations and their standard deviations are discussed. We also present the Strehl ratio of the primary and secondary balanced aberrations.

  11. Enhanced Hydrogen Evolution Reactions on Nanostructured Cu2ZnSnS4 (CZTS) Electrocatalyst

    NASA Astrophysics Data System (ADS)

    Digraskar, Renuka V.; Mulik, Balaji B.; Walke, Pravin S.; Ghule, Anil V.; Sathe, Bhaskar R.

    2017-08-01

    A novel and facile one-step sonochemical method is used to synthesize Cu2ZnSnS4 (CZTS) nanoparticles (2.6 ± 0.4 nm) as cathode electrocatalyst for hydrogen evolution reactions. The detailed morphology, crystal and surface structure, and composition of the CZTS nanostructures were characterized by high resolution transmission electron microscopy (HR-TEM), Selected area electron diffraction (SAED), X-ray diffraction, Raman spectroscopy, FTIR analysis, Brunauer-Emmett-Teller (BET) surface area measurements, Electron dispersive analysis, X-ray photoelectron spectroscopy respectively. Electrocatalytic abilities of the nanoparticles toward Hydrogen Evolution Reactions (HER) were verified through cyclic voltammograms (CV) and Linear sweep voltammetry (LSV), electrochemical impedance spectroscopy (EIS), and Tafel polarization measurements. It reveals enhanced activity at lower onset potential 300 mV v/s RHE, achieved at exceptionally high current density -130 mA/cm2, which is higher than the existing non-nobel metal based cathodes. Further result exhibits Tafel slope of 85 mV/dec, exchange current density of 882 mA/cm2, excellent stability (> 500 cycles) and lower charge transfer resistance. This sonochemically fabricated CZTSs nanoparticles are leading to significantly reduce cell cost and simplification of preparation process over existing high efficiency Pt and other nobel metal-free cathode electrocatalyst.

  12. Single photon energy dispersive x-ray diffraction

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

    Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando

    2014-03-15

    With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signalmore » from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored.« less

  13. Interlaced X-ray diffraction computed tomography

    PubMed Central

    Vamvakeros, Antonios; Jacques, Simon D. M.; Di Michiel, Marco; Senecal, Pierre; Middelkoop, Vesna; Cernik, Robert J.; Beale, Andrew M.

    2016-01-01

    An X-ray diffraction computed tomography data-collection strategy that allows, post experiment, a choice between temporal and spatial resolution is reported. This strategy enables time-resolved studies on comparatively short timescales, or alternatively allows for improved spatial resolution if the system under study, or components within it, appear to be unchanging. The application of the method for studying an Mn–Na–W/SiO2 fixed-bed reactor in situ is demonstrated. Additionally, the opportunities to improve the data-collection strategy further, enabling post-collection tuning between statistical, temporal and spatial resolutions, are discussed. In principle, the interlaced scanning approach can also be applied to other pencil-beam tomographic techniques, like X-ray fluorescence computed tomography, X-ray absorption fine structure computed tomography, pair distribution function computed tomography and tomographic scanning transmission X-ray microscopy. PMID:27047305

  14. 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

  15. X-ray Diffraction, Big and Small

    NASA Image and Video Library

    2012-10-30

    A conventional X-ray diffraction instrument left is the size of a large refrigerator, in contrast to the compact size of the Chemistry and Mineralogy CheMin instrument on NASA Curiosity rover top right.

  16. X-ray diffraction and X-ray standing-wave study of the lead stearate film structure

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

    Blagov, A. E.; Dyakova, Yu. A.; Kovalchuk, M. V.

    2016-05-15

    A new approach to the study of the structural quality of crystals is proposed. It is based on the use of X-ray standing-wave method without measuring secondary processes and considers the multiwave interaction of diffraction reflections corresponding to different harmonics of the same crystallographic reflection. A theory of multiwave X-ray diffraction is developed to calculate the rocking curves in the X-ray diffraction scheme under consideration for a long-period quasi-one-dimensional crystal. This phase-sensitive method is used to study the structure of a multilayer lead stearate film on a silicon substrate. Some specific structural features are revealed for the surface layer ofmore » the thin film, which are most likely due to the tilt of the upper layer molecules with respect to the external normal to the film surface.« less

  17. Modified microwave method for the synthesis of visible light-responsive TiO2/MWCNTs nanocatalysts

    PubMed Central

    2013-01-01

    Recently, TiO2/multi-walled carbon nanotube (MWCNT) hybrid nanocatalysts have been a subject of high interest due to their excellent structures, large surface areas and peculiar optical properties, which enhance their photocatalytic performance. In this work, a modified microwave technique was used to rapidly synthesise a TiO2/MWCNT nanocatalyst with a large surface area. X-ray powder diffraction, field-emission scanning electron microscopy, transmission electron microscopy and Brunauer-Emmett-Teller measurements were used to characterise the structure, morphology and the surface area of the sample. The photocatalytic activity of the hybrid nanocatalysts was evaluated through a comparison of the degradation of methylene blue dye under irradiation with ultraviolet and visible light. The results showed that the TiO2/MWCNT hybrid nanocatalysts degraded 34.9% of the methylene blue (MB) under irradiation with ultraviolet light, whereas 96.3% of the MB was degraded under irradiation with visible light. PMID:23919496

  18. The facile synthesis of hierarchical NiCoO2 nanotubes comprised ultrathin nanosheets for supercapacitors

    NASA Astrophysics Data System (ADS)

    Xu, Xin; Zhou, Han; Ding, Shujiang; Li, Jun; Li, Beibei; Yu, Demei

    2014-12-01

    Hierarchical NiCoO2 nanosheets nanotubes are successfully prepared by a mild solution method based on the template of polymeric nanotubes (PNT) followed by a thermal annealing treatment. The microstructure and chemical composition of NiCoO2 nanosheets nanotubes are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) analyzer, X-ray diffraction (XRD) and Thermogravimetric analysis (TGA). When evaluated as an electrode material for supercapacitors, the results of electrochemical test show that the unique NiCoO2 nanosheets nanotubes exhibit relatively high specific capacitance of 1468, 1352, 1233, 1178, 1020 and 672 F g-1 at the discharge current densities of 2, 4, 8, 10, 20 and 40 A g-1, respectively. They also reveal an excellent cycling stability of 99.2% retention after 3000 cycles at 10 A g-1. The smart nanostructures of the NiCoO2 nanosheets nanotubes make a prominent contribution to the excellent electrochemical performance.

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

    Matyas, Josef; Fryxell, Glen E.; Robinson, Matthew J.

    This is a letter report to complete level 3 milestone "Assess aging characteristics of silica aerogels" for DOE FCRD program. Recently, samples of Ag0-functionalized silica aerogel were aged in flowing dry air for up to 6 months and then loaded with iodine. This dry-air aging simulated the impact of long-term exposure to process gases during process idling. The 6-month aged sample exhibited an iodine sorption capacity of 32 mass%, which was 9 mass % lower than that for an un-aged Ag0-functionalized silica aerogel. In an attempt to understand this decrease in sorption capacity, we characterized physical properties of the agedmore » samples with Brunauer-Emmett-Teller (BET) nitrogen adsorption, X-ray diffraction (XRD), and high resolution scanning electron microscopy (SEM). The results showed no impact of aging on the aerogel microstructure or the silver nanoparticles in the aerogel, including their spatial distribution and morphology.« less

  20. Nanoscale Fe/Ag particles activated persulfate: optimization using response surface methodology.

    PubMed

    Silveira, Jefferson E; Barreto-Rodrigues, Marcio; Cardoso, Tais O; Pliego, Gema; Munoz, Macarena; Zazo, Juan A; Casas, José A

    2017-05-01

    This work studied the bimetallic nanoparticles Fe-Ag (nZVI-Ag) activated persulfate (PS) in aqueous solution using response surface methodology. The Box-Behnken design (BBD) was employed to optimize three parameters (nZVI-Ag dose, reaction temperature, and PS concentration) using 4-chlorophenol (4-CP) as the target pollutant. The synthesis of nZVI-Ag particles was carried out through a reduction of FeCl 2 with NaBH 4 followed by reductive deposition of Ag. The catalyst was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) surface area. The BBD was considered a satisfactory model to optimize the process. Confirmatory tests were carried out using predicted and experimental values under the optimal conditions (50 mg L -1 nZVI-Ag, 21 mM PS at 57 °C) and the complete removal of 4-CP achieved experimentally was successfully predicted by the model, whereas the mineralization degree predicted (90%) was slightly overestimated against the measured data (83%).

  1. Encapsulated heterogeneous base catalysts onto SBA-15 nanoporous material as highly active catalysts in the transesterification of sunflower oil to biodiesel

    NASA Astrophysics Data System (ADS)

    Albayati, Talib M.; Doyle, Aidan M.

    2015-02-01

    Alkali metals and their hydroxides, Na, NaOH, Li, and LiOH, were encapsulated onto SBA-15 nanoporous material as highly active catalysts for the production of biodiesel fuel from sunflower oil. The incipient wetness impregnation method was adopted for the prepared catalysts. The characterization properties of the catalysts and unmodified SBA-15 were determined using X-ray diffraction, scanning electron microscopy, EDAX, nitrogen adsorption-desorption porosimetry (Brunauer-Emmett-Teller), Fourier-transform infrared spectroscopy, and transmission electron microscopy. Transesterification was conducted in a batch reactor at atmospheric pressure and 65 °C. The catalysts were highly active with yields of fatty acid methyl ester (FAME) in the range 96-99 %. Na/SBA-15 catalyst was reused for seven consecutive cycles under the same reaction conditions; the yield to FAME on the final cycle was 96 %. This study shows that the alkali metals and their hydroxides supported on SBA-15-based catalyst are excellent catalysts for the biodiesel reaction.

  2. Synthesis of MoS2/rGO nanosheets hybrid materials for enhanced visible light assisted photocatalytic activity

    NASA Astrophysics Data System (ADS)

    Pal, Shreyasi; Dutta, Shibsankar; De, Sukanta

    2018-04-01

    A facile hydrothermal method has been adopted to synthesize pure MoS2 nanosheets and MoS2/rGO nanosheets hybrid. The samples were characterized using field emission scanning electron microscopy (FESEM), transmission electron microscopy (HRTEM), X-ray diffraction spectroscopy (XRD), Brunauer-Emmett-Teller (BET). The photocatalytic performance and reusability of MoS2 nanosheets and MoS2/rGO hybrids was evaluated by discoloring of RhB under visible light irradiation. Results indicated that MoS2/rGO photocatalysts with large surface area of 69.5 m2 g-1 could completely degrade 50 mL of 8 mg L-1 RhB aqueous solution in 90 min with excellent recycling and structural stability as compared with pure MoS2 nanosheets (53%). Such enhanced performance could be explained due to the high surface area, enhanced light absorption and the increased dye adsorptivity and reduced electron-hole pair recombination with the presence of rGO.

  3. Morphology and crystalline phase study of electrospun TiO2 SiO2 nanofibres

    NASA Astrophysics Data System (ADS)

    Ding, Bin; Kim, Hakyong; Kim, Chulki; Khil, Myungseob; Park, Soojin

    2003-05-01

    Nanofibres of TiO2-SiO2 (Ti:Si = 50: 50 mol%) with diameters of 50-400 nm were prepared by calcining electrospun nanofibres of polyvinyl acetate (PVac)/titania-silica composite as precursor. These PVac/titania-silica hybrid nanofibres were obtained from a homogenous solution of PVac with a sol-gel of titanium isopropoxide (TiP) and tetraethoxysilane by using the electrospinning technique. The nanofibres were characterized by scanning electron microscopy (SEM), wide-angle x-ray diffraction (WAXD), Fourier transform infrared (FTIR) spectroscopy and Brunauer-Emmett-Teller (BET) surface area. SEM, WAXD and FTIR results indicated that the morphology and crystalline phase of TiO2-SiO2 nanofibres were strongly influenced by the calcination temperature and the content of titania and silica in the nanofibres. Additionally, the BET results showed that the surface area of TiO2-SiO2 nanofibres was decreased with increasing calcination temperature and the content of titania and silica in nanofibres.

  4. Catalytic copyrolysis of particle board and polypropylene over Al-MCM-48

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

    Kim, Hannah; Choi, Suek Ju; Kim, Ji Man

    Highlights: • Al-MCM-48 was used for catalytic copyrolysis of particle board and polypropylene. • Catalytic produced mainly hydrocarbons. • The hydrocarbons produced were mainly in the diesel range. - Abstract: Particle board and polypropylene (PP) at a mixing ratio of 1:1 were copyrolyzed over two Al-MCM-48 catalysts with Si/Al ratios of 20 and 80. The catalyst characteristics were examined by measuring the Brunauer-Emmett-Teller surface area, temperature programmed desorption of ammonia, and X-ray diffraction. The main pyrolysis products of particle board were oxygenates, acids, and phenolics, whereas a large quantity of hydrocarbons within the diesel fuel range was produced from copyrolysismore » with polypropylene. The catalytic copyrolysis of particle board and PP over the Al-MCM-48 catalysts produced bio-oil with a much larger hydrocarbon content than that from the catalytic pyrolysis of particle board only. The hydrocarbons produced were mainly in the diesel range, highlighting the potential for the production of high-quality fuel.« less

  5. Synthesis of porous Co3O4/C nanoparticles as anode for Li-ion battery application

    NASA Astrophysics Data System (ADS)

    Yang, Qian; Feng, Chuanqi; Liu, Jianwen; Guo, Zaiping

    2018-06-01

    The porous Co3O4 with electrospun carbon (Co3O4/C) was synthesized simply through annealing the Co-based metal-organic-framework/polyacrylonitrile (ZIF-67/PAN) templates. The samples were characterized by X-ray diffraction (XRD), scanning electronic microscopy (SEM) and Brunauer-Emmett-Teller (BET) techniques. The content of electrospun carbon in Co3O4/C was tested by thermogravimetric analysis (TG). The Co3O4/C not only shows a remarkable capacity of 1024.1 mAh g-1 after 100 cycles but also behaves superior rate capability. The superior electrochemical properties could be attributed to the electrospun carbon, which serves as a buffer layer to slow down the volumetric stresses and provides conductive paths for fast Li+ diffusion and easy electric charge transfer. Therefore, superior performance of the Co3O4/C electrode makes it possible to be used as promising anode for lithium ion battery application.

  6. Conversion of glycerol to polyglycerol over waste duck-bones as a catalyst in solvent free etherification process

    NASA Astrophysics Data System (ADS)

    Ayoub, Muhammad; Sufian, Suriati; Mekuria Hailegiorgis, Sintayehu; Ullah, Sami; Uemura, Yoshimitsu

    2017-08-01

    The alkaline catalyst derived from the duck-bones was used for conversion of glycerol to polyglycerol via solvent free etherification process. The physicochemical properties of prepared materials were duck-bones were systematically investigated as a catalyst by latest techniques of Thermo gravimetric analysis (TGA), X-ray diffraction (XRD), and Brunauer-Emmett-Teller (BET) surface properties. TGA showed different trends of duck-bones decomposition from room temperature to 1000C. XRD pattern showed a clear and sharp peaks of a crystalline phase of CaO. The activity of the catalysts was in line with the basic amount of the strong base sites, surface area, and crystalline phase in the catalysts. The prepared catalyst derived from duck-bones provided high activity (99 %) for glycerol conversion and around 68 % yield for polyglycerol production. These ample wastes of duck-bones have good potential to be used as polyglycerol production catalysts due to have high quantity of Ca compare to other types of bones like cow, chicken and fish bones.

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

    Wang, Yong; State Key Laboratory of Multiphase Complex System, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100080; Zhu, Qingshan, E-mail: qszhu@home.ipe.ac.cn

    {beta}-Ni(OH){sub 2} hierarchical micro-flowers, hierarchical hollow microspheres and nanosheets were synthesized via a facile, single-step and selected-control hydrothermal method. Both hierarchical micro-flowers and hierarchical hollow microspheres were built from two-dimensional nanosheets with thickness of 50-100 nm. The as-obtained products were characterized by Brunauer-Emmett-Teller (BET) surface area analysis, X-ray powder diffraction (XRD) and field emission scanning electron microscopy (FESEM). It was observed that marked morphological changes in {beta}-Ni(OH){sub 2} depended on the initial concentrations of Ni{sup 2+} ions and glycine. A possible growth mechanism was proposed based on experimental results. In addition, the effect of morphology on the electrochemical properties wasmore » also investigated. Both hierarchical micro-flowers and hierarchical hollow microspheres exhibited enhanced specific capacity and high-rate discharge ability as compared with pure Ni(OH){sub 2} nanosheets. Investigations confirmed that hierarchical structures had a pronounced influence upon the electrochemical performance of nickel hydroxide.« less

  8. Preparation and characterization of CuO catalyst for the thermolysis treatment of distillery wastewater.

    PubMed

    Sharma, Deepak; Prajapati, Abhinesh Kumar; Choudhary, Rumi; Kaushal, Rajesh Kumar; Pal, Dharm; Sawarkar, Ashish N

    2017-08-16

    CuO catalyst was prepared from copper sulfate by alkali precipitation method followed by drying and calcination. Characterization of CuO catalyst using X-ray diffraction, Brunauer-Emmett-Teller, and Barrett-Joyner-Halenda surface area analysis envisaged the effectiveness of CuO as a catalyst for the treatment of biodigester effluent (BDE) emanated from distilleries. The catalytic thermolysis is an efficient advance treatment method for distillery biodigester effluent (BDE). CT treatment of BDE was carried out in a 0.5 dm 3 thermolytic batch reactor using CuO as a catalyst at different pH (1-9), temperatures (80-110°C), and catalyst loadings (1-4 kg/m 3 ). With CuO catalyst, a temperature of 110°C, catalyst loading of 4 kg/m 3 , and pH of 2 was found to be optimal, providing a maximum reduction in chemical oxygen demand of 65%. The settling characteristics at different temperatures of CT-treated sludge were also presented.

  9. Adsorption of Pb(II) from aqueous solution using a magnetic chitosan/graphene oxide composite and its toxicity studies.

    PubMed

    Samuel, Melvin S; Shah, Sk Sheriff; Bhattacharya, Jayanta; Subramaniam, Kalidass; Pradeep Singh, N D

    2018-05-02

    This study involves the adsorption of lead using magnetic chitosan/graphene oxide (MCGO) composite material in batch mode. The MCGO composite material was synthesized via modified Hummers method. The MCGO composite material was characterized by powder x-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), Tunnelling electron microscopy (TEM), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET) and UV-vis diffusive reflectance spectra. The adsorption mechanism of MCGO composite material was well described by Langmuir isotherm and pseudo second order kinetic model, with a high regression coefficient (<0.99). The MCGO composite material was applied for the removal of lead metal from aqueous solution. We have also evaluated toxicity of synthesized MCGO composite material by examining on A549 cells. The results have shown that MCGO material showed viable cell percentage of 53.7% at 50 μg and 44.8% at 100 μg. Copyright © 2018 Elsevier B.V. All rights reserved.

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

    DOE PAGES

    Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; ...

    2009-11-01

    We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

  11. Three-dimensional x-ray diffraction nanoscopy

    NASA Astrophysics Data System (ADS)

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

    2008-08-01

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

  12. 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.

  13. 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.

  14. Utilizing broadband X-rays in a Bragg coherent X-ray diffraction imaging experiment

    DOE PAGES

    Cha, Wonsuk; Liu, Wenjun; Harder, Ross; ...

    2016-07-26

    A method is presented to simplify Bragg coherent X-ray diffraction imaging studies of complex heterogeneous crystalline materials with a two-stage screening/imaging process that utilizes polychromatic and monochromatic coherent X-rays and is compatible with in situ sample environments. Coherent white-beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three-dimensional reciprocal-space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifyingin situchamber design. This approach was demonstrated with Au nanoparticles and will enable,more » for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load.« less

  15. Utilizing broadband X-rays in a Bragg coherent X-ray diffraction imaging experiment.

    PubMed

    Cha, Wonsuk; Liu, Wenjun; Harder, Ross; Xu, Ruqing; Fuoss, Paul H; Hruszkewycz, Stephan O

    2016-09-01

    A method is presented to simplify Bragg coherent X-ray diffraction imaging studies of complex heterogeneous crystalline materials with a two-stage screening/imaging process that utilizes polychromatic and monochromatic coherent X-rays and is compatible with in situ sample environments. Coherent white-beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three-dimensional reciprocal-space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifying in situ chamber design. This approach was demonstrated with Au nanoparticles and will enable, for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load.

  16. Spectroscopic imaging, diffraction, and holography with x-ray photoemission

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

    Not Available

    1992-02-01

    X-ray probes are capable of determining the spatial structure of an atom in a specific chemical state, over length scales from about a micron all the way down to atomic resolution. Examples of these probes include photoemission microscopy, energy-dependent photoemission diffraction, photoelectron holography, and X-ray absorption microspectroscopy. Although the method of image formation, chemical-state sensitivity, and length scales can be very different, these X-ray techniques share a common goal of combining a capability for structure determination with chemical-state specificity. This workshop will address recent advances in holographic, diffraction, and direct imaging techniques using X-ray photoemission on both theoretical and experimentalmore » fronts. A particular emphasis will be on novel structure determinations with atomic resolution using photoelectrons.« less

  17. 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.

  18. Photocatalytic performance of Ag doped SnO2 nanoparticles modified with curcumin

    NASA Astrophysics Data System (ADS)

    Vignesh, K.; Hariharan, R.; Rajarajan, M.; Suganthi, A.

    2013-07-01

    Visible light active Ag doped SnO2 nanoparticles modified with curcumin (Cur-Ag-SnO2) have been prepared by a combined precipitation and chemical impregnation route. The optical properties, phase structures and morphologies of the as-prepared nanoparticles were characterized using UV-visible diffuse reflectance spectra (UV-vis-DRS), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS). The surface area was measured by Brunauer. Emmett. Teller (B.E.T) analysis. Compared to bare SnO2, the surface modified photocatalysts (Ag-SnO2 and Cur-Ag-SnO2) showed a red shift in the visible region. The photocatalytic activity was monitored via the degradation of rose bengal (RB) dye and the results revealed that Cur-Ag-SnO2 shows better photocatalytic activity than that of Ag-SnO2 and SnO2. The superior photocatalytic activity of Cur-Ag-SnO2 could be attributed to the effective electron-hole separation by surface modification. The effect of photocatalyst concentration, initial dye concentration and electron scavenger on the photocatalytic activity was examined in detail. Furthermore, the antifungal activity of the photocatalysts and the reusability of Cur-Ag-SnO2 were tested.

  19. Cobalt terephthalate MOF-templated synthesis of porous nano-crystalline Co3O4 by the new indirect solid state thermolysis as cathode material of asymmetric supercapacitor

    NASA Astrophysics Data System (ADS)

    Bigdeli, Hadise; Moradi, Morteza; Hajati, Shaaker; Kiani, Mohammad Ali; Toth, Jozsef

    2017-10-01

    In this work, two different types of Co3O4 nano-crystals were synthesized by (i) conventional direct solid state thermolysis of cobalt terephthalate metal-organic framework (MOF-71) and (ii) new indirect solid state thermolysis of Co(OH)2 derived by alkaline aqueous treatment of MOF-71. The products were then characterized by X-ray diffraction technique (XRD), Fourier transforms infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Reflection electron energy loss spectroscopy (REELS), Brunauer, Emmett, and Teller (BET), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) techniques. By REELS analysis the energy band gap of MOF-71 was determined to be 3.7 eV. Further, electrochemical performance of each Co3O4 nanostructure was studied by the cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS) in a three-electrode system in KOH electrolyte. An asymmetric supercapacitor was fabricated using indirect Co3O4 nanoparticles as cathode and electrochemically reduced graphene oxide as anode, and the electrochemical properties were studied and showed a high energy density of 13.51 Wh kg-1 along with a power density of 9775 W kg-1 and good cycling stability with capacitance retention rate of 85% after 2000 cycles.

  20. Neutron and X-ray investigations of the Jahn–Teller switch in partially deuterated ammonium copper Tutton salt, (NH 4 ) 2 [Cu(H 2 O) 6 ](SO 4 ) 2

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

    Jørgensen, Mads R. V.; Piccoli, Paula M. B.; Hathwar, Venkatesha R.

    2017-01-31

    The structural phase transition accompanied by a Jahn–Teller switch has been studied over a range of H/D ratios in (NH 4) 2[Cu(H 2O) 6](SO 4) 2(ACTS). In particular, single-crystal neutron diffraction investigations of crystals with deuteration in the range 50 to 82% are shown to be consistent with previous electron paramagnetic resonance (EPR) experiments exhibiting a phase boundary at 50% deuteration under ambient pressure. Polycrystalline samples show that the two phases can co-exist. In addition, single-crystal neutron and polycrystalline X-ray diffraction pressure experiments show a shift to lower pressure at 60% deuterationversusprevious measurements at 100% deuteration.

  1. Composite nanofibers prepared from metallic iron nanoparticles and polyaniline: high performance for water treatment applications.

    PubMed

    Bhaumik, Madhumita; Choi, Hyoung J; McCrindle, Rob I; Maity, Arjun

    2014-07-01

    Presented here is a simple preparation of metallic iron nanoparticles, supported on polyaniline nanofibers at room temperature. The preparation is based on polymerization of interconnected nanofibers by rapid mixing of the aniline monomer with Fe(III) chloride as the oxidant, followed by reductive deposition of Fe(0) nanoparticles, using the polymerization by-products as the Fe precursor. The morphology and other physico-chemical properties of the resulting composite were characterized by scanning and transmission electron microscopy, Brunauer-Emmett-Teller method, X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and vibrating-sample magnetometry. The composite fibers were 80-150 nm in diameter and exhibited the expected ferromagnetic behavior. The composite rapidly and efficiently removed As(V), Cr(VI), and also Congo red dye, from aqueous solutions suggesting their usefulness for removal of toxic materials from wastewater. The composite fibers have high capacity for toxin removal: 42.37 mg/g of As(V), 434.78 mg/g of Cr(VI), and 243.9 mg/g of Congo red. The fibers are easily recovered from fluids by exploiting their ferromagnetic properties. Copyright © 2014 Elsevier Inc. All rights reserved.

  2. Kinetic and isotherm studies of bisphenol A adsorption onto orange albedo(Citrus sinensis): Sorption mechanisms based on the main albedo components vitamin C, flavones glycosides and carotenoids.

    PubMed

    Kamgaing, Theophile; Doungmo, Giscard; Melataguia Tchieno, Francis Merlin; Gouoko Kouonang, Jimmy Julio; Mbadcam, Ketcha Joseph

    2017-07-03

    Orange albedo and its adsorption capacity towards bisphenol A (BPA) were studied. Adsorption experiments were conducted in batch mode at 25-55°C. Scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) and Fourier transform infrared (FTIR) spectroscopy were used to characterise the biosorbent. The effects of various parameters including adsorption time, equilibrium pH, adsorbent dosage and initial adsorbate concentration were investigated. The optimum contact time and pH for the removal of BPA were 60 min and 2, respectively. It was found that the adsorption isotherms best matched the Freundlich model, the adsorption of BPA being multilayer and that of the albedo surface heterogeneous. From the kinetic studies, it was found that the removal of BPA best matched the pseudo-second order kinetic model. An adsorption mechanism based on the albedo surface molecules is proposed and gives a good account of π-π interactions and hydrogen bonding. Orange albedo, with a maximum BPA loading capacity of 82.36 mg g -1 (significantly higher than that of most agricultural residues), is a good candidate for BPA adsorption in aqueous media.

  3. Cu2S-Cu-TiO2 mesoporous carbon composites for the degradation of high concentration of methyl orange under visible light

    NASA Astrophysics Data System (ADS)

    Zhang, Liang; Zhao, Yuan; Zhong, Lvling; Wang, Yang; Chai, Shouning; Yang, Tao; Han, Xuanli

    2017-11-01

    A Schiff base compound was used to prepare a Cu2S-Cu-TiO2 mesoporous carbon composite photocatalyst (Cu2S-Cu-TiO2/MC) by a simple precipitation-carbonization method with a carbonization temperature of 750 °C. X-ray diffraction and x-ray photoelectron spectroscopy studies show that Cu2S, Cu, and TiO2 exist in Cu2S-Cu-TiO2/MC in the form of nanometer-sized particles. Scanning electron microscope and transmission electron microscope images show that the composites form a spherical carbon structure inlaid with Cu2S and Cu and coated TiO2. The Brunauer-Emmett-Teller test shows that the material has a large specific surface area (76.14 m2/g) and mesoporous structure. UV-vis diffuse reflection spectroscopy and photoluminescence spectroscopy indicate that the recombination of photo-generated electrons and holes in the samples were inhibited. The composites show good degradation performance in a high concentration (300 mg/L) of methyl orange (MO) solution under visible light. The composites exhibit great potential in the treatment of dyes for wastewater treatment.

  4. Enhanced visible light photocatalytic activity of copper-doped titanium oxide-zinc oxide heterojunction for methyl orange degradation

    NASA Astrophysics Data System (ADS)

    Dorraj, Masoumeh; Alizadeh, Mahdi; Sairi, Nor Asrina; Basirun, Wan Jefrey; Goh, Boon Tong; Woi, Pei Meng; Alias, Yatimah

    2017-08-01

    A novel Cu-doped TiO2 coupled with ZnO nanoparticles (Cu-TiO2/ZnO) was prepared by sol-gel method and subsequent precipitation for methyl orange (MO) photodegradation under visible light irradiation. The compositions and shapes of the as-prepared Cu-TiO2/ZnO nanocomposites were characterized by photoluminescence spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, field emission scanning electron microscopy, transmission electron microscopy, UV-vis diffuse reflectance spectra and Brunauer-Emmett-Teller adsorption isotherm techniques. The Cu-TiO2/ZnO nanocomposites showed considerably higher photocatalytic activity for MO removal from water under visible light irradiation than that of single-doped semiconductors. The effects of Cu-TiO2 and ZnO mass ratios on the photocatalytic reaction were also studied. A coupling percentage of 30% ZnO exhibited the highest photocatalytic activity. The enhanced photocatalytic activity of the Cu-TiO2/ZnO nanocomposites was mainly attributed to heterojunction formation, which allowed the efficient separation of photoinduced electron-hole pairs at the interface. Moreover, these novel nanocomposites could be recycled during MO degradation in a three-cycle experiment without evident deactivation, which is particularly important in environmental applications.

  5. Structural properties and optical characterization of flower-like Mg doped NiO

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

    Allaedini, Ghazaleh, E-mail: jiny-ghazaleh@yahoo.com; Tasirin, Siti Masrinda; Aminayi, Payam

    In this study, un-doped and Mg doped NiO nanoparticles have been synthesized through a simple sol-gel method. To investigate the effect of Mg-doping on the structure of NiO, the obtained nanoparticles were characterized using scanning electron microscopy (SEM). Flower/star like morphology was clearly observed in the SEM micrographs. The BET (Brunauer-Emmett-Teller) nitrogen absorption isotherm exhibits high specific surface area (∼37 m{sup 2} /g) for the Mg doped NiO nanoparticles. X-Ray diffraction (XRD) of the prepared Mg-NiO nanoparticles showed a face-centered cubic (f.c.c) structure, and the average particle size was estimated to be 32 nm using Scherrer’s formula. Energy Dispersive X-Ray (EDX)more » confirms that the NiO particles are successfully doped with Mg. Photoluminescence (PL) and UV-Vis optical absorption characteristics of the prepared nanoparticles have also been investigated in this study. The PL emission response showed a blue shift when NiO was doped with Mg, which is indicative of interstitial oxygen. The UV-Vis results demonstrate a band gap increase as NiO nanoparticles are doped with Mg.« less

  6. Sodium-promoted Pd/TiO2 for catalytic oxidation of formaldehyde at ambient temperature.

    PubMed

    Zhang, Changbin; Li, Yaobin; Wang, Yafei; He, Hong

    2014-05-20

    Catalytic oxidation of formaldehyde (HCHO) to CO2 at ambient conditions is of great interest for indoor HCHO purification. Here, we report that sodium-doped Pd/TiO2 is a highly effective catalyst for the catalytic oxidation of HCHO at room temperature. It was observed that Na doping has a dramatic promotion effect on the Pd/TiO2 catalyst and that nearly 100% HCHO conversion could be achieved over the 2Na-Pd/TiO2 catalyst at a GHSV of 95000 h(-1) and HCHO inlet concentration of 140 ppm at 25 °C. The mechanism of the Na-promotion effect was investigated by using Brunauer-Emmett-Teller (BET), X-ray diffraction (XRD), CO chemisorption, Temperature-programmed reduction by H2 (H2-TPR), X-ray photoelectron spectroscopy (XPS) and temperature-programmed desorption of O2 (O2-TPD) methods. The results showed that Na species addition can induce and further stabilize a negatively charged and well-dispersed Pd species, which then facilitates the activation of H2O and chemisorbed oxygen, therefore resulting in the high performance of the 2Na-Pd/TiO2 catalyst for the ambient HCHO destruction.

  7. Synthesis of Zn1- x Co x Al2O4 Spinel Nanoparticles by Liquid-Feed Flame Spray Pyrolysis: Ceramic Pigments Application

    NASA Astrophysics Data System (ADS)

    Betancur Granados, Natalia; Yi, Eongyu; Laine, Richard M.; Restrepo Baena, Oscar Jaime

    2016-01-01

    Zn1- x Co x Al2O4 ( x = 0.0, 0.2, 0.4, 0.6, 0.8, and 1.0) spinel nanoparticles were synthesized by a liquid-feed flame spray pyrolysis (LF-FSP) method by combusting metallorganic precursor solutions to produce nanopowders with precise composition control. The precursor solutions were aerosolized into a methane/oxygen flame where it was combusted in an oxygen-rich environment to result in nanopowders at a single step. The nanopowders were analyzed by x-ray diffraction, Fourier transform infrared spectroscopy, colorimetry, field emission scanning electron microscopy, transmission electron microscopy, and BET (Brunauer-Emmett-Teller) N2 adsorption. Results show formation of spherical nanopowders with specific surface areas of 42 m2/g to 50 m2/g, which correspond to average particle sizes of 26 nm to 31 nm. Single-phase materials were obtained with a high control of composition, which indicates that LF-FSP is an excellent method to produce mixed-metal oxides for applications in which powder homogeneity is crucial. The products were evaluated for ceramic pigment application, where the ratio of Zn to Co was gradually changed to observe the color change in the structure with the increase of cobalt concentration. The resulting pigments were calcined at 1200°C, which aimed to identify the color stability after a high-temperature process, whereby the colors were measured using the color space CIE L*a*b* under standardized light, D65. Finally, the powders were tested for ceramic decoration using transparent glazes and ceramic bodies. The application was carried out at 1250°C to evaluate the color performance after a decoration process.

  8. 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.

  9. 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.

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

    DOE PAGES

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

    2006-01-01

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

  11. 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.

  12. 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

  13. 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.

  14. Coherent convergent-beam time-resolved X-ray diffraction

    PubMed Central

    Spence, John C. H.; Zatsepin, Nadia A.; Li, Chufeng

    2014-01-01

    The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic laser radiation of a free-electron X-ray laser is unsuitable. We discuss the possibility of obtaining single-shot, angle-integrated rocking curves from CCB patterns, and the dependence of the resulting patterns on the focused beam coordinate when the beam diameter is larger or smaller than a nanocrystal, or smaller than one unit cell. We show how structure factor phase information is provided at overlapping interfering orders and how a common phase origin between different shots may be obtained. Their use in refinement of the phase-sensitive intensity between overlapping orders is suggested. PMID:24914153

  15. Illicit drug detection using energy dispersive x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Cook, E. J.; Griffiths, J. A.; Koutalonis, M.; Gent, C.; Pani, S.; Horrocks, J. A.; George, L.; Hardwick, S.; Speller, R.

    2009-05-01

    Illicit drugs are imported into countries in myriad ways, including via the postal system and courier services. An automated system is required to detect drugs in parcels for which X-ray diffraction is a suitable technique as it is non-destructive, material specific and uses X-rays of sufficiently high energy to penetrate parcels containing a range of attenuating materials. A database has been constructed containing the measured powder diffraction profiles of several thousand materials likely to be found in parcels. These include drugs, cutting agents, packaging and other innocuous materials. A software model has been developed using these data to predict the diffraction profiles which would be obtained by X-ray diffraction systems with a range of suggested detector (high purity germanium, CZT and scintillation), source and collimation options. The aim of the model was to identify the most promising system geometries, which was done with the aid of multivariate analysis (MVA). The most promising systems were constructed and tested. The diffraction profiles of a range of materials have been measured and used to both validate the model and to identify the presence of drugs in sample packages.

  16. Biological imaging by soft x-ray diffraction microscopy

    DOE PAGES

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

    2005-10-25

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

  17. Cryogenic x-ray diffraction microscopy utilizing high-pressure cryopreservation

    NASA Astrophysics Data System (ADS)

    Lima, Enju; Chushkin, Yuriy; van der Linden, Peter; Kim, Chae Un; Zontone, Federico; Carpentier, Philippe; Gruner, Sol M.; Pernot, Petra

    2014-10-01

    We present cryo x-ray diffraction microscopy of high-pressure-cryofixed bacteria and report high-convergence imaging with multiple image reconstructions. Hydrated D. radiodurans cells were cryofixed at 200 MPa pressure into ˜10-μm-thick water layers and their unstained, hydrated cellular environments were imaged by phasing diffraction patterns, reaching sub-30-nm resolutions with hard x-rays. Comparisons were made with conventional ambient-pressure-cryofixed samples, with respect to both coherent small-angle x-ray scattering and the image reconstruction. The results show a correlation between the level of background ice signal and phasing convergence, suggesting that phasing difficulties with frozen-hydrated specimens may be caused by high-background ice scattering.

  18. 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.

  19. Dynamical diffraction imaging (topography) with X-ray synchrotron radiation

    NASA Technical Reports Server (NTRS)

    Kuriyama, M.; Steiner, B. W.; Dobbyn, R. C.

    1989-01-01

    By contrast to electron microscopy, which yields information on the location of features in small regions of materials, X-ray diffraction imaging can portray minute deviations from perfect crystalline order over larger areas. Synchrotron radiation-based X-ray optics technology uses a highly parallel incident beam to eliminate ambiguities in the interpretation of image details; scattering phenomena previously unobserved are now readily detected. Synchrotron diffraction imaging renders high-resolution, real-time, in situ observations of materials under pertinent environmental conditions possible.

  20. 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.

  1. The synthesis of Fe3O4/MWCNT nanocomposites from local iron sands for electrochemical sensors

    NASA Astrophysics Data System (ADS)

    Rahmawati, Retno; Taufiq, Ahmad; Sunaryono, Yuliarto, Brian; Suyatman, Nugraha, Noviandri, Indra; Setyorini, Dian Ayu; Kurniadi, Deddy

    2018-05-01

    The aim of this research is producing the electrochemical sensor, especially for working electrodes based on the nanocomposites of multi-walled carbon nanotube (MWCNT) and magnetite (Fe3O4) nanoparticles from iron sands. The sonochemical method by ultrasonic horn was successfully used for the synthesis of the nanocomposites. The characterizations of the sample were conducted via X-Ray Diffractometer (XRD), Fourier Transform Infra-Red (FTIR) Spectrometer, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Brunauer-Emmett-Teller (BET) method for surface area, Vibrating Sample Magnetometer (VSM) and Cyclic Voltammetry (CV). The analysis of X-Ray Diffraction (XRD) pattern showed two phases of crystalline, namely MWCNT and Fe3O4, peak of MWCNT comes from (002) plan while peaks of Fe3O4 come from (2 2 0), (3 1 1), (4 0 0), (4 2 2), (5 1 1), and (4 4 0) plans. From XRD data, MWCNT has a hexagonal structure and Fe3O4 has inverse spinel cubic structure, respectively. The FTIR spectra revealed that the functionalization process of MWCNT successfully generated carboxyl and carbonyl groups to bind Fe3O4 on MWCNT surfaces. Moreover, the functional groups of Fe-O bonding that showed the existence of Fe3O4 in the nanocomposites were also detected in those spectra. Meanwhile, the SEM and TEM images showed that the nanoparticles of Fe3O4 attached on the MWCNT surface and formed agglomeration between particles due to magnetic forces. Through Brunauer-Emmett-Teller (BET) method, it is identified that the nanocomposite has a large surface area 318 m2/g that makes this material very suitable for electrochemical sensor applications. Moreover, the characterization of magnetic properties via Vibrating Sample Magnetometer (VSM) showed that the nanocomposites have superparamagnetic behavior at room temperature and the presence of the MWCNT reduced the magnetic properties of Fe3O4. Lastly, the electrochemical characterization with Cyclic Voltammetry (CV) proved that

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

    PubMed Central

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

    2010-01-01

    X-ray diffraction microscopy complements other x-ray microscopy methods by being free of lens-imposed radiation dose and resolution limits, and it allows for high-resolution imaging of biological specimens too thick to be viewed by electron microscopy. We report here the highest resolution (11–13 nm) x-ray diffraction micrograph of biological specimens, and a demonstration of molecular-specific gold labeling at different depths within cells via through-focus propagation of the reconstructed wavefield. The lectin concanavalin A conjugated to colloidal gold particles was used to label the α-mannan sugar in the cell wall of the yeast Saccharomyces cerevisiae. Cells were plunge-frozen in liquid ethane and freeze-dried, after which they were imaged whole using x-ray diffraction microscopy at 750 eV photon energy. PMID:20368463

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

    DOE PAGES

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

    2010-04-20

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

  4. 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.

  5. Toward in situ x-ray diffraction imaging at the nanometer scale

    NASA Astrophysics Data System (ADS)

    Zatsepin, Nadia A.; Dilanian, Ruben A.; Nikulin, Andrei Y.; Gable, Brian M.; Muddle, Barry C.; Sakata, Osami

    2008-08-01

    We present the results of preliminary investigations determining the sensitivity and applicability of a novel x-ray diffraction based nanoscale imaging technique, including simulations and experiments. The ultimate aim of this nascent technique is non-destructive, bulk-material characterization on the nanometer scale, involving three dimensional image reconstructions of embedded nanoparticles and in situ sample characterization. The approach is insensitive to x-ray coherence, making it applicable to synchrotron and laboratory hard x-ray sources, opening the possibility of unprecedented nanometer resolution with the latter. The technique is being developed with a focus on analyzing a technologically important light metal alloy, Al-xCu (where x is 2.0-5.0 %wt). The mono- and polycrystalline samples contain crystallographically oriented, weakly diffracting Al2Cu nanoprecipitates in a sparse, spatially random dispersion within the Al matrix. By employing a triple-axis diffractometer in the non-dispersive setup we collected two-dimensional reciprocal space maps of synchrotron x-rays diffracted from the Al2Cu nanoparticles. The intensity profiles of the diffraction peaks confirmed the sensitivity of the technique to the presence and orientation of the nanoparticles. This is a fundamental step towards in situ observation of such extremely sparse, weakly diffracting nanoprecipitates embedded in light metal alloys at early stages of their growth.

  6. 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.

  7. Characterization of X80 and X100 Microalloyed Pipeline Steel Using Quantitative X-ray Diffraction

    NASA Astrophysics Data System (ADS)

    Wiskel, J. B.; Li, X.; Ivey, D. G.; Henein, H.

    2018-06-01

    Quantitative X-ray diffraction characterization of four (4) X80 and three (3) X100 microalloyed steels was undertaken. The effect of through-thickness position, processing parameters, and composition on the measured crystallite size, microstrain, and J index (relative magnitude of crystallographic texture) was determined. Microstructure analysis using optical microscopy, scanning electron microscopy, transmission electron microscopy, and electron-backscattered diffraction was also undertaken. The measured value of microstrain increased with increasing alloy content and decreasing cooling interrupt temperature. Microstructural features corresponding to crystallite size in the X80 steels were both above and below the detection limit for quantitative X-ray diffraction. The X100 steels consistently exhibited microstructure features below the crystallite size detection limit. The yield stress of each steel increased with increasing microstrain. The increase in microstrain from X80 to X100 is also associated with a change in microstructure from predominantly polygonal ferrite to bainitic ferrite.

  8. Three-Dimensional BiOI/BiOX (X = Cl or Br) Nanohybrids for Enhanced Visible-Light Photocatalytic Activity

    PubMed Central

    Liu, Yazi; Xu, Jian; Wang, Liqiong; Zhang, Huayang; Xu, Ping; Duan, Xiaoguang; Sun, Hongqi; Wang, Shaobin

    2017-01-01

    Three-dimensional flower-like BiOI/BiOX (X = Br or Cl) hybrids were synthesized via a facile one-pot solvothermal approach. With systematic characterizations by X-ray diffraction (XRD), scanning electron microscopy (SEM), Transmission electron microscopy (TEM), the Brunauer-Emmett-Teller (BET)specific surface area, X-ray photoelectron spectroscopy (XPS), and the UV-Vis diffuse reflectance spectra (DRS), the BiOI/BiOCl composites showed a fluffy and porous 3-D architecture with a large specific surface area (SSA) and high capability for light absorption. Among all the BiOX (X = Cl, Br, I) and BiOI/BiOX (X = Cl or Br) composites, BiOI/BiOCl stands out as the most efficient photocatalyst under both visible and UV light irradiations for methyl orange (MO) oxidation. The reaction rate of MO degradation on BiOI/BiOCl was 2.1 times higher than that on pure BiOI under visible light. Moreover, BiOI/BiOCl exhibited enhanced water oxidation efficiency for O2 evolution which was 1.5 times higher than BiOI. The enhancement of photocatalytic activity could be attributed to the formation of a heterojunction between BiOI and BiOCl, with a nanoporous structure, a larger SSA, and a stronger light absorbance capacity especially in the visible-light region. The in situ electron paramagnetic resonance (EPR) revealed that BiOI/BiOCl composites could effectively evolve superoxide radicals and hydroxyl radicals for photodegradation, and the superoxide radicals are the dominant reactive species. The superb photocatalytic activity of BiOI/BiOCl could be utilized for the degradation of various industrial dyes under natural sunlight irradiation which is of high significance for the remediation of industrial wastewater in the future. PMID:28336897

  9. Studies on X-ray diffraction microscopy

    NASA Astrophysics Data System (ADS)

    Miao, Huijie

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

  10. 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.

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

    NASA Astrophysics Data System (ADS)

    Mahato, Dip Narayan

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

  12. Novel mesoporous FeAl bimetal oxides for As(III) removal: Performance and mechanism.

    PubMed

    Ding, Zecong; Fu, Fenglian; Cheng, Zihang; Lu, Jianwei; Tang, Bing

    2017-02-01

    In this study, novel mesoporous FeAl bimetal oxides were successfully synthesized, characterized, and employed for As(III) removal. Batch experiments were conducted to investigate the effects of Fe/Al molar ratio, dosage, and initial solution pH values on As(III) removal. The results showed that the FeAl bimetal oxide with Fe/Al molar ratio 4:1 (shorten as FeAl-4) can quickly remove As(III) from aqueous solution in a wide pH range. The FeAl-4 before and after reaction with As(III) was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED), Brunauer-Emmett-Teller (BET) surface area measurement, and X-ray photoelectron spectroscopy (XPS). The BET results showed that the original FeAl-4 with a high surface area of 223.9 m 2 /g was a mesoporous material. XPS analysis indicated that the surface of FeAl-4 possessed a high concentration of M-OH (where M represents Fe and Al), which was beneficial to the immobility of As(III). The excellent performance of FeAl-4 makes it a potentially attractive material for As(III) removal from aqueous solution. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Mayenite Synthesized Using the Citrate Sol-Gel Method

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

    Ude, Sabina N; Rawn, Claudia J; Meisner, Roberta A

    2014-01-01

    A citrate sol-gel method has been used to synthesize mayenite (Ca12Al14O33). X-ray powder diffraction data show that the samples synthesized using the citrate sol-gel method contained CaAl2O4 and CaCO3 along with mayenite when fired ex-situ in air at 800 C but were single phase when fired at 900 C and above. Using high temperature x-ray diffraction, data collected in-situ in air at temperatures of 600 C and below showed only amorphous content; however, data collected at higher temperatures indicated the first phase to crystallize is CaCO3. High temperature x-ray diffraction data collected in 4% H2/96% N2 does not show themore » presence of CaCO3, and Ca12Al14O33 starts to form around 850 C. In comparison, x-ray powder diffraction data collected ex-situ on samples synthesized using traditional solid-state synthesis shows that single phase was not reached until samples were fired at 1350 C. DTA/TGA data collected either in a nitrogen environment or air on samples synthesized using the citrate gel method suggest the complete decomposition of metastable phases and the formation of mayenite at 900 C, although the phase evolution is very different depending on the environment. Brunauer-Emmett-Teller (BET) measurements showed a slightly higher surface area of 7.4 0.1 m2/g in the citrate gel synthesized samples compared to solid-state synthesized sample with a surface area of 1.61 0.02 m2/g. SEM images show a larger particle size for samples synthesized using the solid-state method compared to those synthesized using the citrate gel method.« less

  14. Cryogenic X-Ray Diffraction Microscopy for Biological Samples

    NASA Astrophysics Data System (ADS)

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

    2009-11-01

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

  15. 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.

  16. 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

  17. 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…

  18. 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.

  19. 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.

  20. Characterization of X-Ray Diffraction System with a Microfocus X-Ray Source and a Polycapillary Optic

    NASA Technical Reports Server (NTRS)

    Gubarev, Mikhail; Marshall, Joy K.; Ciszak, Ewa; Ponomarev, Igor

    2000-01-01

    We present here an optimized microfocus x-ray source and polycapillary optic system designed for diffraction of small protein crystals. The x-ray beam is formed by a 5.5mm focal length capillary collimator coupled with a 40 micron x-ray source operating at 46Watts. Measurements of the x-ray flux, the divergence and the spectral characteristics of the beam are presented, This optimized system provides a seven fold greater flux than our recently reported configuration [M. Gubarev, et al., J. of Applied Crystallography (2000) 33, in press]. We now make a comparison with a 5kWatts rotating anode generator (Rigaku) coupled with confocal multilayer focusing mirrors (Osmic, CMF12- 38Cu6). The microfocus x-ray source and polycapillary collimator system delivers 60% of the x-ray flux from the rotating anode system. Additional ways to improve our microfocus x-ray system, and thus increase the x-ray flux will be discussed.

  1. Long-Wavelength X-Ray Diffraction and Its Applications in Macromolecular Crystallography.

    PubMed

    Weiss, Manfred S

    2017-01-01

    For many years, diffraction experiments in macromolecular crystallography at X-ray wavelengths longer than that of Cu-K α (1.54 Å) have been largely underappreciated. Effects caused by increased X-ray absorption result in the fact that these experiments are more difficult than the standard diffraction experiments at short wavelengths. However, due to the also increased anomalous scattering of many biologically relevant atoms, important additional structural information can be obtained. This information, in turn, can be used for phase determination, for substructure identification, in molecular replacement approaches, as well as in structure refinement. This chapter reviews the possibilities and the difficulties associated with such experiments, and it provides a short description of two macromolecular crystallography synchrotron beam lines dedicated to long-wavelength X-ray diffraction experiments.

  2. Diffractive-refractive optics: (+,-,-,+) X-ray crystal monochromator with harmonics separation.

    PubMed

    Hrdý, Jaromír; Mikulík, Petr; Oberta, Peter

    2011-03-01

    A new kind of two channel-cut crystals X-ray monochromator in dispersive (+,-,-,+) position which spatially separates harmonics is proposed. The diffracting surfaces are oriented so that the diffraction is inclined. Owing to refraction the diffracted beam is sagittally deviated. The deviation depends on wavelength and is much higher for the first harmonics than for higher harmonics. This leads to spatial harmonics separation. The idea is supported by ray-tracing simulation.

  3. 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.

  4. 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.

  5. Diffractive-refractive optics: X-ray splitter.

    PubMed

    Hrdý, Jaromír

    2010-01-01

    The possibility of splitting a thin (e.g. undulator) X-ray beam based on diffraction-refraction effects is discussed. The beam is diffracted from a crystal whose diffracting surface has the shape of a roof with the ridge lying in the plane of diffraction. The crystal is cut asymmetrically. One half of the beam impinges on the left-hand part of the roof and the other half impinges on the right-hand side of the roof. Owing to refraction the left part of the beam is deviated to the left whereas the right part is deviated to the right. The device proposed consists of two channel-cut crystals with roof-like diffraction surfaces; the crystals are set in a dispersive position. The separation of the beams after splitting is calculated at a distance of 10 m from the crystals for various asymmetry and inclination angles. It is shown that such a splitting may be utilized for long beamlines. Advantages and disadvantages of this method are discussed.

  6. 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.

  7. AUSPEX: a graphical tool for X-ray diffraction data analysis.

    PubMed

    Thorn, Andrea; Parkhurst, James; Emsley, Paul; Nicholls, Robert A; Vollmar, Melanie; Evans, Gwyndaf; Murshudov, Garib N

    2017-09-01

    In this paper, AUSPEX, a new software tool for experimental X-ray data analysis, is presented. Exploring the behaviour of diffraction intensities and the associated estimated uncertainties facilitates the discovery of underlying problems and can help users to improve their data acquisition and processing in order to obtain better structural models. The program enables users to inspect the distribution of observed intensities (or amplitudes) against resolution as well as the associated estimated uncertainties (sigmas). It is demonstrated how AUSPEX can be used to visually and automatically detect ice-ring artefacts in integrated X-ray diffraction data. Such artefacts can hamper structure determination, but may be difficult to identify from the raw diffraction images produced by modern pixel detectors. The analysis suggests that a significant portion of the data sets deposited in the PDB contain ice-ring artefacts. Furthermore, it is demonstrated how other problems in experimental X-ray data caused, for example, by scaling and data-conversion procedures can be detected by AUSPEX.

  8. Fabrication, characterization and gamma rays shielding properties of nano and micro lead oxide-dispersed-high density polyethylene composites

    NASA Astrophysics Data System (ADS)

    Mahmoud, Mohamed E.; El-Khatib, Ahmed M.; Badawi, Mohamed S.; Rashad, Amal R.; El-Sharkawy, Rehab M.; Thabet, Abouzeid A.

    2018-04-01

    Polymer composites of high-density polyethylene (HD-PE) filled with powdered lead oxide nanoparticles (PbO NPs) and bulk lead oxide (PbO Blk) were prepared with filler weight fraction [10% and 50%]. These polymer composites were investigated for radiation-shielding of gamma-rays emitted from radioactive point sources [241Am, 133Ba, 137Cs, and 60Co]. The polymer was found to decrease the heaviness of the shielding material and increase the flexibility while the metal oxide fillers acted as principle radiation attenuators in the polymer composite. The prepared composites were characterized by Fourier transform infrared spectrophotometer (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscope (SEM), Brunauer-Emmett-Teller surface area (BET) and field emission transmission electron microscope (FE-TEM). The morphological analysis of the assembled composites showed that, PbO NPs and PbO Blk materials exhibited homogenous dispersion in the polymer-matrix. Thermogravimetric analysis (TGA) demonstrated that the thermal-stability of HD-PE was enhanced in the presence of both PbO Blk and PbO NPs. The results declared that, the density of polymer composites was increase with the percentage of filler contents. The highest density value was identified as 1.652 g cm-3 for 50 wt% of PbO NPs. Linear attenuation coefficients (μ) have been estimated from the use of XCOM code and measured results. Reasonable agreement was attended between theoretical and experimental results. These composites were also found to display excellent percentage of heaviness with respect to other conventional materials.

  9. A simple large-scale synthesis of mesoporous In2O3 for gas sensing applications

    NASA Astrophysics Data System (ADS)

    Zhang, Su; Song, Peng; Yan, Huihui; Yang, Zhongxi; Wang, Qi

    2016-08-01

    In this paper, large-scale mesoporous In2O3 nanostructures were synthesized by a facile Lewis acid catalytic the furfural alcohol resin (FAR) template route for the high-yield. Their morphology and structure were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential thermal and thermogravimetry analysis (DSC-TG) and the Brunauer-Emmett-Teller (BET) approach. The as-obtained mesoporous In2O3 nanostructures possess excellent mesoporous and network structure, which increases the contact area with the gases, it is conducive for adsorption-desorption of gas on the surface of In2O3. The In2O3 particles and pores were both about 15 nm and very uniform. In gas-sensing measurements with target gases, the gas sensor based on mesoporous In2O3 nanostructures showed a good response, short response-recovery time, good selectivity and stability to ethanol. These properties are due to the large specific surface area of mesoporous structure. This synthetic method could use as a new design concept for functional mesoporous nanomaterials and for mass production.

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

    Stengl, Vaclav, E-mail: stengl@iic.cas.cz; Bludska, Jana; Oplustil, Frantisek

    Highlights: {yields} New nano-dispersive materials for warfare agents decontamination. {yields} 95% decontamination activities for sulphur mustard. {yields} New materials base on titanium and manganese oxides. -- Abstract: Titanium(IV)-manganese(IV) nano-dispersed oxides were prepared by a homogeneous hydrolysis of potassium permanganate and titanium(IV) oxo-sulphate with 2-chloroacetamide. Synthesised samples were characterised using Brunauer-Emmett-Teller (BET) surface area and Barrett-Joiner-Halenda porosity (BJH), X-ray diffraction (XRD), infrared spectroscopy (IR), and scanning electron microscopy (SEM). These oxides were taken for an experimental evaluation of their reactivity with sulphur mustard (HD or bis(2-chloroethyl)sulphide) and soman (GD or (3,3'-dimethylbutan-2-yl)-methylphosphonofluoridate). Mn{sup 4+} content affects the decontamination activity; with increasing Mn{supmore » 4+} content the activity increases for sulphur mustard and decreases for soman. The best decontamination activities for sulphur mustard and soman were observed for samples TiMn{sub 3}7 with 18.6 wt.% Mn and TiMn{sub 5} with 2.1 wt.% Mn, respectively.« less

  11. Physicochemical of pillared clays prepared by several metal oxides

    NASA Astrophysics Data System (ADS)

    Rinaldi, Nino; Kristiani, Anis

    2017-03-01

    Natural clays could be modified by the pillarization method, called as Pillared Clays (PILCs). PILCs have been known as porous materials that can be used for many applications, one of the fields is catalysis. PILCs as two dimensional materials are interesting because their structures and textural properties can be controlled by using a metal oxide as the pillar. Different metal oxide used as the pillar causes different properties results of pillared clays. Usually, natural smectite clays/bentonites are used as a raw material. Therefore, a series of bentonite pillared by metal oxides was prepared through pillarization method. Variation of metals pillared into bentonite are aluminium, chromium, zirconium, and ferro. The physicochemical properties of catalysts were characterized by using X-ray Diffraction (XRD), Thermo Gravimetric Analysis (TGA), Brunauer-Emmett-Teller (BET) and Barret-Joyner-Halenda (BJH) analysis, and Fourier transform infrared spectroscopy (FTIR) measurement. Noteworthy characterization results showed that different metals pillared into bentonite affected physical and chemical properties, i.e. basal spacing, surface area, pore size distribution, thermal stability and acidity.

  12. TiO2-PANI/Cork composite: A new floating photocatalyst for the treatment of organic pollutants under sunlight irradiation.

    PubMed

    Sboui, Mouheb; Nsib, Mohamed Faouzi; Rayes, Ali; Swaminathan, Meenakshisundaram; Houas, Ammar

    2017-10-01

    A novel photocatalyst based on TiO 2 -PANI composite supported on small pieces of cork has been reported. It was prepared by simple impregnation method of the polyaniline (PANI)-modified TiO 2 on cork. The TiO 2 -PANI/Cork catalyst shows the unique feature of floating on the water surface. The as-synthesized catalyst was characterized by X-ray diffraction (XRD), scanning electron micrograph (SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), UV-vis diffuse reflectance spectra (UV-vis DRS) and the Brunauer-Emmett-Teller (BET) surface area analysis. Characterization suggested the formation of anatase highly dispersed on the cork surface. The prepared floating photocatalyst showed high efficiency for the degradation of methyl orange dye and other organic pollutants under solar irradiation and constrained conditions, i.e., no-stirring and no-oxygenation. The TiO 2 -PANI/Cork floating photocatalyst can be reused for at least four consecutive times without significant decrease of the degradation efficiency. Copyright © 2017. Published by Elsevier B.V.

  13. Characterization and Leaching Tests of the Fluidized Bed Steam Reforming (FBSR) Waste Form for LAW Immobilization

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

    Neeway, James J.; Qafoku, Nikolla; Brown, Christopher F.

    2013-10-01

    Several supplemental technologies for treating and immobilizing Hanford low activity waste (LAW) have been evaluated. One such immobilization technology is the Fluidized Bed Steam Reforming (FBSR) granular product. The FBSR granular product is composed of insoluble sodium aluminosilicate (NAS) feldspathoid minerals. Production of the FBSR mineral product has been demonstrated both at the industrial and laboratory scale. Pacific Northwest National Laboratory (PNNL) was involved in an extensive characterization campaign. This goal of this campaign was study the durability of the FBSR mineral product and the mineral product encapsulated in a monolith to meet compressive strength requirements. This paper gives anmore » overview of results obtained using the ASTM C 1285 Product Consistency Test (PCT), the EPA Test Method 1311 Toxicity Characteristic Leaching Procedure (TCLP), and the ASTMC 1662 Single-Pass Flow-Through (SPFT) test. Along with these durability tests an overview of the characteristics of the waste form has been collected using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), microwave digestions for chemical composition, and surface area from Brunauer, Emmett, and Teller (BET) theory.« less

  14. Characterization and Leaching Tests of the Fluidized Bed Steam Reforming (FBSR) Waste Form for LAW Immobilization - 13400

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

    Neeway, James J.; Qafoku, Nikolla P.; Peterson, Reid A.

    2013-07-01

    Several supplemental technologies for treating and immobilizing Hanford low activity waste (LAW) have been evaluated. One such immobilization technology is the Fluidized Bed Steam Reforming (FBSR) granular product. The FBSR granular product is composed of insoluble sodium aluminosilicate (NAS) feldspathoid minerals. Production of the FBSR mineral product has been demonstrated both at the industrial and laboratory scale. Pacific Northwest National Laboratory (PNNL) was involved in an extensive characterization campaign. The goal of this campaign was to study the durability of the FBSR mineral product and the encapsulated FBSR product in a geo-polymer monolith. This paper gives an overview of resultsmore » obtained using the ASTM C 1285 Product Consistency Test (PCT), the EPA Test Method 1311 Toxicity Characteristic Leaching Procedure (TCLP), and the ASTMC 1662 Single-Pass Flow-Through (SPFT) test. Along with these durability tests an overview of the characteristics of the waste form has been collected using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), microwave digestions for chemical composition, and surface area from Brunauer, Emmett, and Teller (BET) theory. (authors)« less

  15. A microwave synthesis of mesoporous NiCo2O4 nanosheets as electrode materials for lithium-ion batteries and supercapacitors.

    PubMed

    Mondal, Anjon Kumar; Su, Dawei; Chen, Shuangqiang; Kretschmer, Katja; Xie, Xiuqiang; Ahn, Hyo-Jun; Wang, Guoxiu

    2015-01-12

    A facile microwave method was employed to synthesize NiCo2 O4 nanosheets as electrode materials for lithium-ion batteries and supercapacitors. The structure and morphology of the materials were characterized by X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy and Brunauer-Emmett-Teller methods. Owing to the porous nanosheet structure, the NiCo2 O4 electrodes exhibited a high reversible capacity of 891 mA h g(-1) at a current density of 100 mA g(-1) , good rate capability and stable cycling performance. When used as electrode materials for supercapacitors, NiCo2 O4 nanosheets demonstrated a specific capacitance of 400 F g(-1) at a current density of 20 A g(-1) and superior cycling stability over 5000 cycles. The excellent electrochemical performance could be ascribed to the thin porous structure of the nanosheets, which provides a high specific surface area to increase the electrode-electrolyte contact area and facilitate rapid ion transport. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Hybrids of NiCo2O4 nanorods and nanobundles with graphene as promising electrode materials for supercapacitors.

    PubMed

    Wang, Zhuo; Zhang, Xin; Zhang, Zhongshen; Qiao, Nanli; Li, Yang; Hao, Zhengping

    2015-12-15

    High dispersion of NiCo2O4 nanorods and porous NiCo2O4 nanobundles decorated on RGO have been synthesized by a facile hydrothermal method, followed by calcination in one step. By adjusting the starting metal sources to realize the synthesis of different morphologies of NiCo2O4. The morphology and the microstructure of the as-prepared composites were characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) and transmission electron microscope (TEM) techniques. Among them, the porous RGO/NiCo2O4 nanobundles gives a higher specific capacitance of 1278F/g at 1A/g and 719F/g at 20A/g, showing a remarkable rate capability. The excellent electrochemical performances could ascribed to the unique structural feature with higher surface area. It could be anticipated that the synthesized electrode material will gain promising applications in supercapacitors and other devices because of their outstanding characteristics of controllable capacitance and facilely synthesized. Copyright © 2015 Elsevier Inc. All rights reserved.

  17. Synthesis Properties and Electron Spin Resonance Properties of Titanic Materials (abstract)

    NASA Astrophysics Data System (ADS)

    Cho, Jung Min; Lee, Jun; Kim, Tak Hee; Sun, Min Ho; Jang, Young Bae; Cho, Sung June

    2009-04-01

    Titanic materials were synthesized by hydrothermal method of TiO2 anatase in 10M LiOH, 10M NaOH, and 14M KOH at 130° C for 30 hours. Alkaline media were removed from the synthesized products using 0.1N HCl aqueous solution. The as-prepared samples were characterized by scanning electron microscope, transmission electron microscope, X-ray diffraction, Brunauer-Emmett-Teller isotherm, and electron spin resonance. Different shapes of synthesized products were observed through the typical electron microscope and indicated that the formation of the different morphologies depends on the treatment conditions of highly alkaline media. Many micropores were observed in the cubic or octahedral type of TiO2 samples through the typical electron microscope and Langmuir adsorption-desorption isotherm of liquid nitrogen at 77° K. Electron spin resonance studies have also been carried out to verify the existence of paramagnetic sites such as oxygen vacancies on the titania samples. The effect of alkali metal ions on the morphologies and physicochemical properties of nanoscale titania are discussed.

  18. One-Pot Route towards Active TiO2 Doped Hierarchically Porous Cellulose: Highly Efficient Photocatalysts for Methylene Blue Degradation

    PubMed Central

    Sun, Xiaoxia; Wang, Kunpeng; Shu, Yu; Zou, Fangdong; Zhang, Boxing; Sun, Guangwu; Uyama, Hiroshi; Wang, Xinhou

    2017-01-01

    In this study, novel photocatalyst monolith materials were successfully fabricated by a non-solvent induced phase separation (NIPS) technique. By adding a certain amount of ethyl acetate (as non-solvent) into a cellulose/LiCl/N,N-dimethylacetamide (DMAc) solution, and successively adding titanium dioxide (TiO2) nanoparticles (NPs), cellulose/TiO2 composite monoliths with hierarchically porous structures were easily formed. The obtained composite monoliths possessed mesopores, and two kinds of macropores. Scanning Electron Microscope (SEM), Energy Dispersive Spectroscopy (EDS), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray Diffraction (XRD), Brunauer-Emmett-Teller (BET), and Ultraviolet-visible Spectroscopy (UV-Vis) measurements were adopted to characterize the cellulose/TiO2 composite monolith. The cellulose/TiO2 composite monoliths showed high efficiency of photocatalytic activity in the decomposition of methylene blue dye, which was decomposed up to 99% within 60 min under UV light. Moreover, the composite monoliths could retain 90% of the photodegradation efficiency after 10 cycles. The novel NIPS technique has great potential for fabricating recyclable photocatalysts with highly efficiency. PMID:28772734

  19. The effect of synthesis parameters on the geometry and dimensions of mesoporous hydroxyapatite nanoparticles in the presence of 1-dodecanethiol as a pore expander.

    PubMed

    Bakhtiari, L; Rezaie, H R; Javadpour, J; Erfan, M; Shokrgozar, M A

    2015-08-01

    Mesoporous hydroxyapatite with different pore diameters and pore volumes were synthesized by the self-assembly method using Cetyltrimethylammonium bromide (CTAB) as the cationic surfactant and 1-dodecanethiol as the pore expander at different micellization pHs, solvent types and surfactant concentrations. Results of field emission scanning electron microscopy (FESEM) showed a decrease in length/diameter ratio of rod-like particles by an increase in micellization pH and also a sphere to rod transition in morphology by an increase in CTAB concentration. Brunauer-Emmett-Teller (BET) surface area and Low angle X-ray diffraction analysis revealed that the optimized mesoporous hydroxyapatite with controlled pore structure can be obtained under basic micellization pH (about 12, pH of complete ionization of 1-dodecanethiol) by using water as the solvent and a high content of cationic surfactant. The results also show that micellization pH has a strong effect on pore structure and changing the pH can shift the mesostructure to a macroporous structure with morphological changes. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. A novel biochar from Manihot esculenta Crantz waste: application for the removal of Malachite Green from wastewater and optimization of the adsorption process.

    PubMed

    Beakou, Buscotin Horax; El Hassani, Kaoutar; Houssaini, Mohammed Amine; Belbahloul, Mounir; Oukani, Elhassan; Anouar, Abdellah

    2017-09-01

    The adsorptive removal of Malachite Green (MG) by a novel biochar namely Cassava Rind Carbon (CRC) was studied in a batch system. Moreover, Box-Behnken Response Surface Methodology was used to optimize operating conditions of the adsorption process. Characterization was done by Thermo Gravimetric Analysis (TGA), Attenuated Total Reflectance Fourier Transform Infra-Red Spectroscopy (ATR/FTIR), Brunauer-Emmett-Teller (BET) surface area, Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD) and pH zero charge point (pH ZCP ). The pseudo-second-order model and Langmuir model provided the best fit for kinetic and isotherm, respectively. The maximum capacity of dye adsorbed was 932.98 mg/g at 25 °C. The influence of temperature, the mass of adsorbent and the concentration of dye was studied. The optimal amount of adsorbed MG was 1,363.58 mg/g corresponding to 50 °C, 5 mg of CRC and 150 mg/L of dye. According to the high performance exhibited by CRC in this study, Manihot esculenta Crantz waste can be used as a better and low-cost biomass for wastewater decolourization.

  1. Direct synthesis of carbon nanofibers from South African coal fly ash

    NASA Astrophysics Data System (ADS)

    Hintsho, Nomso; Shaikjee, Ahmed; Masenda, Hilary; Naidoo, Deena; Billing, Dave; Franklyn, Paul; Durbach, Shane

    2014-08-01

    Carbon nanofibers (CNFs), cylindrical nanostructures containing graphene, were synthesized directly from South African fly ash (a waste product formed during the combustion of coal). The CNFs (as well as other carbonaceous materials like carbon nanotubes (CNTs)) were produced by the catalytic chemical vapour deposition method (CCVD) in the presence of acetylene gas at temperatures ranging from 400°C to 700°C. The fly ash and its carbonaceous products were characterized by transmission electron microscopy (TEM), thermogravimetric analysis (TGA), laser Raman spectroscopy and Brunauer-Emmett-Teller (BET) surface area measurements. It was observed that as-received fly ash was capable of producing CNFs in high yield by CCVD, starting at a relatively low temperature of 400°C. Laser Raman spectra and TGA thermograms showed that the carbonaceous products which formed were mostly disordered. Small bundles of CNTs and CNFs observed by TEM and energy-dispersive spectroscopy (EDS) showed that the catalyst most likely responsible for CNF formation was iron in the form of cementite; X-ray diffraction (XRD) and Mössbauer spectroscopy confirmed these findings.

  2. Multifunctional materials such as MCM-41÷Fe3O4÷folic acid as drug delivery system.

    PubMed

    Popescu, Simona; Ardelean, Ioana Lavinia; Gudovan, Dragoş; Rădulescu, Marius; Ficai, Denisa; Ficai, Anton; Vasile, Bogdan Ştefan; Andronescu, Ecaterina

    2016-01-01

    In this study, MCM-41 mesoporous silica nanoparticles (NPs) and MCM-41÷Fe3O4 mesoporous silica NPs were prepared by sol-gel method using CTAB (cetyltrimethylammonium bromide) as template and TEOS (tetraethyl orthosilicate) as silica precursor in order to use these materials as drug delivery system (DDS) for different biologically active agents. The MCM-41 and MCM-41÷Fe3O4 mesoporous silica NPs were characterized using specific physico-chemical methods [transmission electron microscopy (TEM), scanning electron microscopy (SEM), nitrogen adsorption and desorption studies - BET (Brunauer-Emmett-Teller) method, X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy], while the release studies were done by a high-performance liquid chromatography (HPLC)-modified method. The pH dependence of the delivery of folic acid from the mesoporous structures was analyzed and found that the release is pH sensitive. The lower delivery at strongly acid pH comparing with neutral/slightly alkaline pH could be beneficial because in stomach the folic acid can be destroyed.

  3. Electrochemical Properties of Graphene Oxide/Resol Composites as Electrode Materials for Supercapacitor Applications.

    PubMed

    Park, Geon Woo; Jeon, Sang Kwon; Yang, Jin Yong; Choi, Sung Dae; Kim, Geon Joong

    2016-05-01

    RGO/Resol carbon composites were prepared from a mixture of reduced GO and a low-molecular-weight phenolic resin (Resol) solution. The effects of the calcination temperature, amount of Resol added and KOH treatment on the electrochemical performance of the RGO/Resol composites were investigated. The physical and electrochemical properties of the composite materials were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Brunauer, Emmett and Teller (BET) surface areas measurements, and cyclic voltammetry (CV). The relationships between their physical properties and their electrochemical performance were examined for use as super-capacitors (SCs). The RGO/Resol composite calcined at 400 degrees C after the KOH loading showed dramatically improved electrochemical properties, showing a high BET surface and capacitance of 2190 m2/g and 220 F/g, respectively. The RGO/Resol composites calcined after the KOH treatment showed much better capacitor performance than those treated only thermally at the same temperature without KOH impregnation. The fabrication of high surface electrodes was essential for improving the SCs properties.

  4. Understanding the effect of annealing temperature on crystalline structure, morphology, and photocatalytic activity of silver-loaded TiO2 nanotubes

    NASA Astrophysics Data System (ADS)

    Viet, Pham Van; Phuong Trang, Duong Dao; Phat, Bui Dai; Hieu, Le Van; Thi, Cao Minh

    2018-05-01

    In this study, we classified the effect of the annealing temperature on silver-loaded TiO2 nanotubes (Ag/TNTs). X-ray diffraction results demonstrate that TNTs have a tendency of phase transformation owing to silver nanoparticles (Ag NPs). The Brunauer-Emmett-Teller method indicates that Ag/TNTs is a mesopore material and the surface area of Ag/TNTs decreases when the annealing temperature increases. This research concluded that the TNT structure begins to break at high annealing temperatures (>400 °C) and is completely broken at 500 °C. The average diameter of the Ag NPs in Ag/TNTs increases linearly with the annealing temperature. In addition, this study clearly explained the oxidation state transformation of Ag in Ag/TNTs under the impact of the annealing temperature, therein, the Ag0 state is transferred completely to Ag+ at 400 °C, and some Ag+ is oxidized to form Ag2+. The Ag/TNTs and Ag/TNTs annealed at 300 °C provided the good methylene blue photodegradation ability for 150 min under sunlight condition.

  5. 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.

  6. Fabricating Blazed Diffraction Gratings by X-Ray Lithography

    NASA Technical Reports Server (NTRS)

    Mouroulis, Pantazis; Hartley, Frank; Wilson, Daniel

    2004-01-01

    Gray-scale x-ray lithography is undergoing development as a technique for fabricating blazed diffraction gratings. As such, gray-scale x-ray lithography now complements such other grating-fabrication techniques as mechanical ruling, holography, ion etching, laser ablation, laser writing, and electron-beam lithography. Each of these techniques offers advantages and disadvantages for implementing specific grating designs; no single one of these techniques can satisfy the design requirements for all applications. Gray-scale x-ray lithography is expected to be advantageous for making gratings on steeper substrates than those that can be made by electron-beam lithography. This technique is not limited to sawtooth groove profiles and flat substrates: various groove profiles can be generated on arbitrarily shaped (including highly curved) substrates with the same ease as sawtooth profiles can be generated on flat substrates. Moreover, the gratings fabricated by this technique can be made free of ghosts (spurious diffraction components attributable to small spurious periodicities in the locations of grooves). The first step in gray-scale x-ray lithography is to conformally coat a substrate with a suitable photoresist. An x-ray mask (see Figure 1) is generated, placed between the substrate and a source of collimated x-rays, and scanned over the substrate so as to create a spatial modulation in the exposure of the photoresist. Development of the exposed photoresist results in a surface corrugation that corresponds to the spatial modulation and that defines the grating surface. The grating pattern is generated by scanning an appropriately shaped x-ray area mask along the substrate. The mask example of Figure 1 would generate a blazed grating profile when scanned in the perpendicular direction at constant speed, assuming the photoresist responds linearly to incident radiation. If the resist response is nonlinear, then the mask shape can be modified to account for the

  7. One-step synthesis of free-standing α-Ni(OH)2 nanosheets on reduced graphene oxide for high-performance supercapacitors

    NASA Astrophysics Data System (ADS)

    Dong, Bitao; Zhou, Han; Liang, Jin; Zhang, Lusi; Gao, Guoxin; Ding, Shujiang

    2014-10-01

    In this work, a hierarchical hybrid structure of reduced graphene oxide (rGO) supported ultrathin α-Ni(OH)2 nanosheets (denoted as α-Ni(OH)2@rGO NSs) has been developed successfully via an environmentally friendly one-step solution method. The resulting product of α-Ni(OH)2@rGO NSs was further characterized by scanning electron microscope, transmission electron microscope, x-ray diffraction, Raman spectroscopy, x-ray photoelectron spectroscopy, and Brunauer-Emmett-Teller. The ultrathin α-Ni(OH)2 nanosheets of around 6 nm in thickness are uprightly coated on the double sides of rGO substrate. When evaluated as electrodes for supercapacitors, the hybrid α-Ni(OH)2@rGO NSs demonstrate excellent supercapacitor performance and cycling stability, compared with the self-aggregated α-Ni(OH)2 powder. Even after 2000 cycles, the hybrid electrodes still can deliver a specific capacitance of 1300 F g-1 at the current density of 5 A g-1, corresponding to no capacity loss of the initial cycle. Such excellent electrochemical performance should be attributed to the ultrathin, free-standing, and hierarchical nanosheets of α-Ni(OH)2, which not only promote efficient charge transport and facilitate the electrolyte diffusion, but also prevent aggregation of electro-active materials effectively during the charge-discharge process.

  8. One-step synthesis of free-standing α-Ni(OH)₂ nanosheets on reduced graphene oxide for high-performance supercapacitors.

    PubMed

    Dong, Bitao; Zhou, Han; Liang, Jin; Zhang, Lusi; Gao, Guoxin; Ding, Shujiang

    2014-10-31

    In this work, a hierarchical hybrid structure of reduced graphene oxide (rGO) supported ultrathin α-Ni(OH)2 nanosheets (denoted as α-Ni(OH)2@rGO NSs) has been developed successfully via an environmentally friendly one-step solution method. The resulting product of α-Ni(OH)2@rGO NSs was further characterized by scanning electron microscope, transmission electron microscope, x-ray diffraction, Raman spectroscopy, x-ray photoelectron spectroscopy, and Brunauer-Emmett-Teller. The ultrathin α-Ni(OH)2 nanosheets of around 6 nm in thickness are uprightly coated on the double sides of rGO substrate. When evaluated as electrodes for supercapacitors, the hybrid α-Ni(OH)2@rGO NSs demonstrate excellent supercapacitor performance and cycling stability, compared with the self-aggregated α-Ni(OH)2 powder. Even after 2000 cycles, the hybrid electrodes still can deliver a specific capacitance of 1300 F g(-1) at the current density of 5 A g(-1), corresponding to no capacity loss of the initial cycle. Such excellent electrochemical performance should be attributed to the ultrathin, free-standing, and hierarchical nanosheets of α-Ni(OH)2, which not only promote efficient charge transport and facilitate the electrolyte diffusion, but also prevent aggregation of electro-active materials effectively during the charge-discharge process.

  9. Enhanced visible light photocatalytic activity of sulfated CuO-Bi2O3 photocatalyst

    NASA Astrophysics Data System (ADS)

    Liu, Xinlu; Zeng, Jun; Zhong, Junbo; Li, Jianzhang

    2015-09-01

    Sulfate (SO4 2-)-modified CuO-Bi2O3 composite photocatalysts with different loadings of SO4 2- were prepared by a facile pore impregnating method using ammonium persulfate (NH4)2S2O8 solution. The surface parameters, structure, morphology, the response ability to light, the binding energy of Bi 4 f and O 1 s, the hydroxyl content on the surface and the separation rate of photoinduced hole-electron pairs were characterized by Brunauer-Emmett-Teller method, X-ray diffraction, scanning electron microscopy, UV-Vis diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy and surface photovoltage spectroscopy, respectively. The results reveal that sulfating of CuO-Bi2O3 decreases the band gap, increases the hydroxyl content on the surface, the separation rate of photoinduced hole-electron pairs and the adsorption of Rhodamine B on the sulfated photocatalysts. The photocatalytic activity of SO4 2-/CuO-Bi2O3 for decolorization of Rhodamine B aqueous solution was evaluated. The result shows that when the molar ratio of S/Bi is 5 %, SO4 2-/CuO-Bi2O3 exhibits the best photocatalytic activity under visible light irradiation and the possible reason is discussed.

  10. Influence of two different template removal methods on the micromorphology, crystal structure, and photocatalytic activity of hollow CdS nanospheres

    NASA Astrophysics Data System (ADS)

    Wang, Han; Jin, Tingting; Zheng, Xing; Jiang, Bo; Zhu, Chaosheng; Yuan, Xiangdong; Zheng, Jingtang; Wu, Mingbo

    2016-11-01

    Hollow cadmium sulfide (CdS) nanospheres of about 260 nm average diameters and about 30 nm shell thickness can be easily synthesized via a sonochemical process, in which polystyrene (PS) nanoparticles were employed as templates. In order to remove the PS templates, both etching and calcination were applied in this paper. The influence of the two different template removal methods on the surface micromorphology, crystal structure, and photocatalytic activity of hollow CdS nanospheres was carefully performed a comparative study. Results of X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray, FT-IR, thermogravimetric analysis, Brunauer-Emmett-Teller, diffused reflectance spectra, and decolorization experiments showed that the different template removal methods exhibited a significant influence on the surface micromorphology, crystal structure, and photocatalytic activity of hollow CdS nanospheres. The CdS hollow nanospheres as-prepared by etching had pure cubic sphalerite structure, higher -OH content, less defects and exhibited good photocatalytic activity for rhodamine-B, Methylene Blue and methyl orange under UV-vis light irradiation. However, CdS hollow nanospheres obtained by calcination with a hexagonal crystal structure, less -OH content, more defects have shown worse photocatalytic activity. This indicated that surface micromorphology and crystalline phase were mainly factors influencing photocatalytic activity of hollow CdS nanospheres.

  11. Synthesis and characterization of supported polysugar-stabilized palladium nanoparticle catalysts for enhanced hydrodechlorination of trichloroethylene

    NASA Astrophysics Data System (ADS)

    Bacik, Deborah B.; Zhang, Man; Zhao, Dongye; Roberts, Christopher B.; Seehra, Mohinar S.; Singh, Vivek; Shah, Naresh

    2012-07-01

    Palladium (Pd) nanoparticle catalysts were successfully synthesized within an aqueous phase using sodium carboxymethyl cellulose (CMC) as a capping ligand which offers a green alternative to conventional nanoparticle synthesis techniques. The CMC-stabilized Pd nanoparticles were subsequently dispersed within support materials using the incipient wetness impregnation technique for utilization in heterogeneous catalyst systems. The unsupported and supported (both calcined and uncalcined) Pd nanoparticle catalysts were characterized using transmission electron microscopy, energy dispersive x-ray spectrometry, x-ray diffraction, and Brunauer-Emmett-Teller surface area measurement and their catalytic activity toward the hydrodechlorination of trichloroethylene (TCE) in aqueous media was examined using homogeneous and heterogeneous catalyst systems, respectively. The unsupported Pd nanoparticles showed considerable activity toward the degradation of TCE, as demonstrated by the reaction kinetics. Although the supported Pd nanoparticle catalysts had a lower catalytic activity than the unsupported particles that were homogeneously dispersed in the aqueous solutions, the supported catalysts retained sufficient activity toward the degradation of TCE. In addition, the use of the hydrophilic Al2O3 support material induced a mass transfer resistance to TCE that affected the initial hydrodechlorination rate. This paper demonstrates that supported Pd catalysts can be applied to the heterogeneous catalytic hydrodechlorination of TCE.

  12. Persulfate activation by iron oxide-immobilized MnO2 composite: identification of iron oxide and the optimum pH for degradations.

    PubMed

    Jo, Young-Hoon; Do, Si-Hyun; Kong, Sung-Ho

    2014-01-01

    Iron oxide-immobilized manganese oxide (MnO2) composite was prepared and the reactivity of persulfate (PS) with the composite as activator was investigated for degradation of carbon tetrachloride and benzene at various pH levels. Brunauer-Emmett-Teller (BET) surface area of the composite was similar to that of pure MnO2 while the pore volume and diameter of composite was larger than those of MnO2. Scanning electron microscopy couples with energy dispersive spectroscopy (SEM-EDS) showed that Fe and Mn were detected on the surface of the composite, and X-ray diffraction (XRD) analysis indicated the possibilities of the existence of various iron oxides on the composite surface. Furthermore, the analyses of X-ray photoelectron (XPS) spectra revealed that the oxidation state of iron was identified as 1.74. In PS/composite system, the same pH for the highest degradation rates of both carbon tetrachloride and benzene were observed and the value of pH was 9. Scavenger test was suggested that both oxidants (i.e. hydroxyl radical, sulfate radical) and reductant (i.e. superoxide anion) were effectively produced when PS was activated with the iron-immobilized MnO2. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Characterization and activity of Pd-modified TiO2 catalysts for photocatalytic oxidation of NO in gas phase.

    PubMed

    Wu, Zhongbiao; Sheng, Zhongyi; Liu, Yue; Wang, Haiqiang; Tang, Nian; Wang, Jie

    2009-05-30

    Pd-modified TiO(2) prepared by thermal impregnation method was used in this study for photocatalytic oxidation of NO in gas phase. The physico-chemical properties of Pd/TiO(2) catalysts were characterized by X-ray diffraction analysis (XRD), Brunauer-Emmett-Teller measurements (BET), X-ray photoelectron spectrum analysis (XPS), transmission electron microscopy (TEM), high resolution-transmission electron microscopy (HR-TEM), UV-vis diffuse reflectance spectra (UV-vis DRS) and photoluminescence spectra (PL). It was found that Pd dopant existed as PdO particles in as-prepared photocatalysts. The results of PL spectra indicated that the photogenerated electrons and holes were efficiently separated after Pd doping. During in situ XPS study, it was found that the content of hydroxyl groups on the surface of Pd/TiO(2) increased when the catalyst was irradiated by UV light, which could result in the improvement of photocatalytic activity. The activity test showed that the optimum Pd dopant content was 0.05 wt.%. And the maximum conversion of NO was about 72% higher than that of P25 when the initial concentration of NO was 200 ppm, which showed that Pd/TiO(2) photocatalysts could be potentially applied to oxidize higher concentration of NO.

  14. Enhanced electrochemical capacitance and oil-absorbability of N-doped graphene aerogel by using amino-functionalized silica as template and doping agent

    NASA Astrophysics Data System (ADS)

    Du, Yongxu; Liu, Libin; Xiang, Yu; Zhang, Qiang

    2018-03-01

    The development of novel energy storage devices with high power density and energy density is highly desired. However, as a promising material, the strong π-π interaction of graphene inhibits its applications. Herein, we provide a new approach that amino-functionalized silica are used as both templates to prevent the restacking of the graphene sheets and doping agents simultaneously. The microstructures, porous properties and chemical composition of the resulted N-doped reduced graphene oxide (RGO) aerogels, characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman, X-ray photoelectron spectroscopy and Brunauer-Emmett-Teller measurement, indicate that the amount of SiO2-NH2 has profound effects on the surface area and carbon activity of the graphene sheets. Benefiting from the large specific surface area of 481.8 m2 g-1, low series resistances and high nitrogen doping content (4.4 atom%), the as-fabricated 3D hierarchical porous N-doped RGO aerogel electrode exhibits outstanding electrochemical performance in aqueous and organic electrolyte, such as ultrahigh specific capacitances of 350 F g-1 at a current density of 1 A g-1 and excellent reversibility with a cycling efficiency of 88% after 10000 cycles. In addition, the N-doped RGO aerogels possess high oil-absorbability with long recyclability.

  15. Enhanced sunlight-driven photocatalytic performance of Bi-doped CdMoO4 benefited from efficient separation of photogenerated charge pairs

    NASA Astrophysics Data System (ADS)

    Huang, Jiao; Liu, Huanhuan; Zhong, Junbo; Yang, Qi; Chen, Jiufu; Li, Jianzhang; Ma, Dongmei; duan, Ran

    2018-06-01

    In this paper, to further boost the photocatalytic performance of CdMoO4, Bi3+ was successfully doped into CdMoO4 by a facile microwave hydrothermal method. The Bi-doped CdMoO4 photocatalysts prepared were characterized by Brunauer-Emmett-Teller (BET) method, X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), electron spin-resonance (ESR) and surface photovoltage spectroscopy (SPS). The results exhibit that doping Bi3+ into CdMoO4 remarkably boosts the separation rate of photoinduced charge pairs and the specific surface area, decrease the crystal size, narrows the band gap of the CdMoO4 and induces the binding energy shift of Cd, all these advantageous factors result in the promoted photocatalytic performance of CdMoO4. Using rhodamine B (RhB) as model toxic pollutant, the photocatalytic activities of the photocatalysts were evaluated under a 500 W Xe lamp irradiation. When the molar ratio of Bi/Cd is 0.2%, Bi-CdMoO4 prepared displays the best photocatalytic performance, the photocatalytic performance of the 0.2% sample is more than twice of that of the reference CdMoO4.

  16. Catalytic conversion of aliphatic alcohols on carbon nanomaterials: The roles of structure and surface functional groups

    NASA Astrophysics Data System (ADS)

    Tveritinova, E. A.; Zhitnev, Yu. N.; Chernyak, S. A.; Arkhipova, E. A.; Savilov, S. V.; Lunin, V. V.

    2017-03-01

    Carbon nanomaterials with the structure of graphene and different compositions of the surface groups are used as catalysts for the conversion of C2-C4 aliphatic alcohols. The conversions of ethanol, propanol- 1, propanol-2, butanol-1, butanol-2, and tert-butanol on carbon nanotubes, nanoflakes, and nanoflakes doped with nitrogen are investigated. Oxidized and nonoxidized multiwalled carbon nanotubes, nanoflakes, and nanoflakes doped with nitrogen are synthesized. X-ray diffraction analysis, X-ray photoelectron spectroscopy, scanning and transmission electronic microscopies, Brunauer-Emmett-Teller method, derivatographic analyses, and the pulsed microcatalytic method are used to characterize comprehensively the prepared catalysts. It was established that all of the investigated carbon nanomaterials (with the exception of nondoped carbon nanoflakes) are bifunctional catalysts for the conversion of aliphatic alcohols, and promote dehydration reactions with the formation of olefins and dehydrogenation reactions with the formation of aldehydes or ketones. Nanoflakes doped with nitrogen are inert with respect to secondary alcohols and tert-butanol. The role of oxygen-containing and nitrogen-containing surface groups, and of the geometrical structure of the carbon matrix of graphene nanocarbon materials in the catalytic conversion of aliphatic alcohols, is revealed. Characteristics of the conversion of aliphatic alcohols that are associated with their structure are identified.

  17. Reconstructive colour X-ray diffraction imaging--a novel TEDDI imaging method.

    PubMed

    Lazzari, Olivier; Jacques, Simon; Sochi, Taha; Barnes, Paul

    2009-09-01

    Tomographic Energy-Dispersive Diffraction Imaging (TEDDI) enables a unique non-destructive mapping of the interior of bulk objects, exploiting the full range of X-ray signals (diffraction, fluorescence, scattering, background) recorded. By analogy to optical imaging, a wide variety of features (structure, composition, orientation, strain) dispersed in X-ray wavelengths can be extracted and colour-coded to aid interpretation. The ultimate aim of this approach is to realise real-time high-definition colour X-ray diffraction imaging, on the timescales of seconds, so that one will be able to 'look inside' optically opaque apparatus and unravel the space/time-evolution of the materials chemistry taking place. This will impact strongly on many fields of science but there are currently two barriers to this goal: speed of data acquisition (a 2D scan currently takes minutes to hours) and loss of image definition through spatial distortion of the X-ray sampling volume. Here we present a data-collection scenario and reconstruction routine which overcomes the latter barrier and which has been successfully applied to a phantom test object and to real materials systems such as a carbonating cement block. These procedures are immediately transferable to the promising technology of multi-energy-dispersive-detector-arrays which are planned to deliver the other breakthrough, that of one-two orders of magnitude improvement in data acquisition rates, that will be needed to realise real-time high-definition colour X-ray diffraction imaging.

  18. 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

  19. Discovery and development of x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Jeong, Yeuncheol; Yin, Ming; Datta, Timir

    2013-03-01

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

  20. High-energy X-ray diffraction using the Pixium 4700 flat-panel detector.

    PubMed

    Daniels, J E; Drakopoulos, M

    2009-07-01

    The Pixium 4700 detector represents a significant step forward in detector technology for high-energy X-ray diffraction. The detector design is based on digital flat-panel technology, combining an amorphous Si panel with a CsI scintillator. The detector has a useful pixel array of 1910 x 2480 pixels with a pixel size of 154 microm x 154 microm, and thus it covers an effective area of 294 mm x 379 mm. Designed for medical imaging, the detector has good efficiency at high X-ray energies. Furthermore, it is capable of acquiring sequences of images at 7.5 frames per second in full image mode, and up to 60 frames per second in binned region of interest modes. Here, the basic properties of this detector applied to high-energy X-ray diffraction are presented. Quantitative comparisons with a widespread high-energy detector, the MAR345 image plate scanner, are shown. Other properties of the Pixium 4700 detector, including a narrow point-spread function and distortion-free image, allows for the acquisition of high-quality diffraction data at high X-ray energies. In addition, high frame rates and shutterless operation open new experimental possibilities. Also provided are the necessary data for the correction of images collected using the Pixium 4700 for diffraction purposes.

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

    PubMed

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

    2007-02-01

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

  2. Nanocrystalline Ce 1- xY xO 2- x/2 (0≤ x≤0.35) Oxides via Carbonate Precipitation: Synthesis and Characterization

    NASA Astrophysics Data System (ADS)

    Li, Ji-Guang; Ikegami, Takayasu; Wang, Yarong; Mori, Toshiyuki

    2002-10-01

    A novel carbonate (co)precipitation method, employing nitrates as the starting salts and ammonium carbonate as the precipitant, has been used to synthesize nanocrystalline CeO 2 and Ce 1- xY xO 2- x/2 ( x≤0.35) solid-solutions. The resultant powders are characterized by elemental analysis, differential thermal analysis/thermogravimetry (DTA/TG), X-ray diffractometry (XRD), Brunauer-Emmett-Teller (BET) analysis, and high-resolution scanning electron microscopy (HRSEM). Due to the direct formation of carbonate solid-solutions during precipitation, Ce 1- xY xO 2- x/2 solid-solution oxides are formed directly during calcination at a very low temperature of ˜300°C for 2 h. The thus-produced oxide nanopowders are essentially non-agglomerated, as revealed by BET in conjunction with XRD analysis. The solubility of YO 1.5 in CeO 2 is determined via XRD to be somewhere in the range from 27 to 35 mol%, from which a Y 2O 3-related type-C phase appears in the final product. Y 3+-doping promotes the formation of spherical nanoparticles, retards thermal decomposition of the precursors, and suppresses significantly crystallite coarsening of the oxides during calcination. The activation energy for crystallite coarsening increases gradually from 68.7 kJ mol -1 for pure CeO 2 to 138.6 kJ mol -1 for CeO 2 doped with 35 mol% YO 1.5. The dopant effects on crystallite coarsening is elaborated from the view point of solid-state chemistry.

  3. Incoherent Diffractive Imaging via Intensity Correlations of Hard X Rays

    NASA Astrophysics Data System (ADS)

    Classen, Anton; Ayyer, Kartik; Chapman, Henry N.; Röhlsberger, Ralf; von Zanthier, Joachim

    2017-08-01

    Established x-ray diffraction methods allow for high-resolution structure determination of crystals, crystallized protein structures, or even single molecules. While these techniques rely on coherent scattering, incoherent processes like fluorescence emission—often the predominant scattering mechanism—are generally considered detrimental for imaging applications. Here, we show that intensity correlations of incoherently scattered x-ray radiation can be used to image the full 3D arrangement of the scattering atoms with significantly higher resolution compared to conventional coherent diffraction imaging and crystallography, including additional three-dimensional information in Fourier space for a single sample orientation. We present a number of properties of incoherent diffractive imaging that are conceptually superior to those of coherent methods.

  4. Combined synchrotron X-ray tomography and X-ray powder diffraction using a fluorescing metal foil.

    PubMed

    Kappen, P; Arhatari, B D; Luu, M B; Balaur, E; Caradoc-Davies, T

    2013-06-01

    This study realizes the concept of simultaneous micro-X-ray computed tomography and X-ray powder diffraction using a synchrotron beamline. A thin zinc metal foil was placed in the primary, monochromatic synchrotron beam to generate a divergent wave to propagate through the samples of interest onto a CCD detector for tomographic imaging, thus removing the need for large beam illumination and high spatial resolution detection. Both low density materials (kapton tubing and a piece of plant) and higher density materials (Egyptian faience) were investigated, and elemental contrast was explored for the example of Cu and Ni meshes. The viability of parallel powder diffraction using the direct beam transmitted through the foil was demonstrated. The outcomes of this study enable further development of the technique towards in situ tomography∕diffraction studies combining micrometer and crystallographic length scales, and towards elemental contrast imaging and reconstruction methods using well defined fluorescence outputs from combinations of known fluorescence targets (elements).

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

    NASA Astrophysics Data System (ADS)

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

    1995-09-01

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

  6. X-ray filter for x-ray powder diffraction

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

    Sinsheimer, John Jay; Conley, Raymond P.; Bouet, Nathalie C. D.

    Technologies are described for apparatus, methods and systems effective for filtering. The filters may comprise a first plate. The first plate may include an x-ray absorbing material and walls defining first slits. The first slits may include arc shaped openings through the first plate. The walls of the first plate may be configured to absorb at least some of first x-rays when the first x-rays are incident on the x-ray absorbing material, and to output second x-rays. The filters may comprise a second plate spaced from the first plate. The second plate may include the x-ray absorbing material and wallsmore » defining second slits. The second slits may include arc shaped openings through the second plate. The walls of the second plate may be configured to absorb at least some of second x-rays and to output third x-rays.« less

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

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

    Jones, Michael W. M.; Phillips, Nicholas W.; van Riessen, Grant A.

    2016-08-11

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

  8. 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

  9. X-ray diffraction from nonuniformly stretched helical molecules

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

    Prodanovic, Momcilo; Irving, Thomas C.; Mijailovich, Srboljub M.

    2016-04-18

    The fibrous proteins in living cells are exposed to mechanical forces interacting with other subcellular structures. X-ray fiber diffraction is often used to assess deformation and movement of these proteins, but the analysis has been limited to the theory for fibrous molecular systems that exhibit helical symmetry. However, this approach cannot adequately interpret X-ray data from fibrous protein assemblies where the local strain varies along the fiber length owing to interactions of its molecular constituents with their binding partners. To resolve this problem a theoretical formulism has been developed for predicting the diffraction from individual helical molecular structures nonuniformly strainedmore » along their lengths. This represents a critical first step towards modeling complex dynamical systems consisting of multiple helical structures using spatially explicit, multi-scale Monte Carlo simulations where predictions are compared with experimental data in a `forward' process to iteratively generate ever more realistic models. Here the effects of nonuniform strains and the helix length on the resulting magnitude and phase of diffraction patterns are quantitatively assessed. Examples of the predicted diffraction patterns of nonuniformly deformed double-stranded DNA and actin filaments in contracting muscle are presented to demonstrate the feasibly of this theoretical approach.« less

  10. Femtosecond X-ray diffraction from an aerosolized beam of protein nanocrystals

    DOE PAGES

    Awel, Salah; Kirian, Richard A.; Wiedorn, Max O.; ...

    2018-02-01

    High-resolution Bragg diffraction from aerosolized single granulovirus nanocrystals using an X-ray free-electron laser is demonstrated. The outer dimensions of the in-vacuum aerosol injector components are identical to conventional liquid-microjet nozzles used in serial diffraction experiments, which allows the injector to be utilized with standard mountings. As compared with liquid-jet injection, the X-ray scattering background is reduced by several orders of magnitude by the use of helium carrier gas rather than liquid. Such reduction is required for diffraction measurements of small macromolecular nanocrystals and single particles. High particle speeds are achieved, making the approach suitable for use at upcoming high-repetition-rate facilities.

  11. 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.

  12. 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.

  13. Buckskin Drill Hole and CheMin X-ray Diffraction

    NASA Image and Video Library

    2015-12-17

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

  14. Radiolytic hydrogen generation at silicon carbide-water interfaces

    NASA Astrophysics Data System (ADS)

    Schofield, Jennifer; Reiff, Sarah C.; Pimblott, Simon M.; LaVerne, Jay A.

    2016-02-01

    While many of the proposed uses of SiC in the nuclear industry involve systems that are assumed to be dry, almost all materials have dissociated chemisorbed water associated with their surface, which can undergo chemistry in radiation fields. Silicon carbide α-phase and β-phase nanoparticles with water were irradiated with γ-rays and 5 MeV 4He ions followed by the determination of the production of molecular hydrogen, H2, and characterization of changes in the particle surface. The yields of H2 from SiC-water slurries were always greater than expected from a simple mixture rule indicating that the presence of SiC was influencing the production of H2 from water, probably through an energy transfer from the solid to liquid phase. Although the increase in H2 yields was modest, a decrease in the water mass percentage led to an increase in H2 yields, especially for very low amounts of water. Surface analysis techniques included diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), nitrogen absorption with the Brunauer - Emmett - Teller (BET) methodology for surface area determination, X-ray diffraction (XRD), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). Little change in the SiC surface was observed following radiolysis except for some conversion of β-phase SiC to the α-phase and the formation of SiO2 with He ion radiolysis.

  15. 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.

  16. Diffraction and Imaging Study of Imperfections of Protein Crystals with Coherent X-rays

    NASA Technical Reports Server (NTRS)

    Hu, Z. W.; Thomas, B. R.; Chernov, A. A.; Chu, Y. S.; Lai, B.

    2004-01-01

    High angular-resolution x-ray diffraction and phase contrast x-ray imaging were combined to study defects and perfection of protein crystals. Imperfections including line defects, inclusions and other microdefects were observed in the diffraction images of a uniformly grown lysozyme crystal. The observed line defects carry distinct dislocation features running approximately along the <110> growth front and have been found to originate mostly in a central growth area and occasionally in outer growth regions. Slow dehydration led to the broadening of a fairly symmetric 4 4 0 rocking curve by a factor of approximately 2.6, which was primarily attributed to the dehydration-induced microscopic effects that are clearly shown in diffraction images. X-ray imaging and diffraction characterization of the quality of apoferritin crystals will also be discussed in the presentation.

  17. Adsorptive Desulfurization of JP-8 Fuel Using Ag+/Silica Based Adsorbents at Room Temperature

    DTIC Science & Technology

    2012-09-01

    promising because it is accomplished at ambient temperature and pressure. Erkey and co-workers used carbon aerogels (CAs) as adsorbents for their sulfur...aluminum oxide ATR auto-thermal reforming BET Brunauer, Emmett and Teller theory BT benzothiophene CAs carbon aerogels CPOX catalytic partial

  18. Enhanced stabilization of Pb, Zn, and Cd in contaminated soils using oxalic acid-activated phosphate rocks.

    PubMed

    Zhang, Zhuo; Guo, Guanlin; Wang, Mei; Zhang, Jia; Wang, Zhixin; Li, Fasheng; Chen, Honghan

    2018-01-01

    Phosphate amendments, especially phosphate rock (PR), are one of the most commonly used materials to stabilize heavy metals in contaminated soils. However, most of PR reserve consists of low-grade ore, which limits the efficiency of PR for stabilizing heavy metals. This study was to enhance the stabilization of heavy metals through improving the available phosphorous (P) release of PR by oxalic acid activation. Raw PR and activated PR (APR) were characterized by scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), X-ray powder diffraction (XRD), Brunauer-Emmett-Teller (BET) surface analysis, and laser diffraction to determine the changes of structure and composition of APR. The stabilization effectiveness of lead (Pb), zinc (Zn), and cadmium (Cd) in soils by APR was investigated through toxicity leaching test and speciation analysis. The results indicated that after treatment by oxalic acid, (1) the crystallinity of the fluorapatite phase of PR transformed into the weddellite phase; (2) the surface area of PR increased by 37%; (3) the particle size of PR became homogenized (20-70 μm); and (4) the available P content in PR increased by 22 times. These changes of physicochemical characteristics of PR induced that APR was more effective to transform soil heavy metals from the non-residual fraction to the residual fraction and enhance the stabilization efficiency of Pb, Zn, and Cd than PR. These results are significant for the future use of low-grade PR to stabilize heavy metals.

  19. Structural and electrical properties of TiO{sub 2}/ZnO core–shell nanoparticles synthesized by hydrothermal method

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

    Vlazan, P.; Ursu, D.H.; Irina-Moisescu, C.

    TiO{sub 2}/ZnO core–shell nanoparticles were successfully synthesized by hydrothermal method in two stages: first stage is the hydrothermal synthesis of ZnO nanoparticles and second stage the obtained ZnO nanoparticles are encapsulated in TiO{sub 2}. The obtained ZnO, TiO{sub 2} and TiO{sub 2}/ZnO core–shell nanoparticles were investigated by means of X-ray diffraction, transmission electron microscopy, Brunauer, Emmett, Teller and resistance measurements. X-ray diffraction analysis revealed the presence of both, TiO{sub 2} and ZnO phases in TiO{sub 2}/ZnO core–shell nanoparticles. According to transmission electron microscopy images, ZnO nanoparticles have hexagonal shapes, TiO{sub 2} nanoparticles have a spherical shape, and TiO{sub 2}/ZnO core–shellmore » nanoparticles present agglomerates and the shape of particles is not well defined. The activation energy of TiO{sub 2}/ZnO core–shell nanoparticles was about 101 meV. - Graphical abstract: Display Omitted - Highlights: • TiO{sub 2}/ZnO core–shell nanoparticles were synthesized by hydrothermal method. • TiO{sub 2}/ZnO core–shell nanoparticles were investigated by means of XRD, TEM and BET. • Electrical properties of TiO{sub 2}/ZnO core–shell nanoparticles were investigated. • The activation energy of TiO{sub 2}/ZnO core–shell nanoparticles was about E{sub a} = 101 meV.« less

  20. Combined X-ray and neutron fibre diffraction studies of biological and synthetic polymers

    NASA Astrophysics Data System (ADS)

    Parrot, I. M.; Urban, V.; Gardner, K. H.; Forsyth, V. T.

    2005-08-01

    The fibrous state is a natural one for polymer molecules which tend to assume regular helical conformations rather than the globular structures characteristic of many proteins. Fibre diffraction therefore has broad application to the study of a wide range of biological and synthetic polymers. The purpose of this paper is to illustrate the general scope of the method and in particular to demonstrate the impact of a combined approach involving both X-ray and neutron diffraction methods. While the flux of modern X-ray synchrotron radiation sources allows high quality datasets to be recorded with good resolution within a very short space of time, neutron studies can provide unique information through the ability to locate hydrogen or deuterium atoms that are often difficult or impossible to locate using X-ray methods. Furthermore, neutron fibre diffraction methods can, through the ability to selectively label specific parts of a structure, be used to highlight novel aspects of polymer structure that can not be studied using X-rays. Two examples are given. The first describes X-ray and neutron diffraction studies of conformational transitions in DNA. The second describes structural studies of the synthetic high-performance polymer poly(p-phenylene terephthalamide) (PPTA), known commercially as Kevlar® or Twaron®.

  1. 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.

  2. X-ray diffraction diagnostic design for the National Ignition Facility

    NASA Astrophysics Data System (ADS)

    Ahmed, Maryum F.; House, Allen; Smith, R. F.; Ayers, Jay; Lamb, Zachary S.; Swift, David W.

    2013-09-01

    This paper describes the design considerations for Target Diffraction In-Situ (TARDIS), an x-ray diffraction diagnostic at the National Ignition Facility. A crystal sample is ramp-compressed to peak pressures between 10 and 30 Mbar and, during a pressure hold period, is probed with quasi-monochromatic x-rays emanating from a backlighter source foil. The crystal spectrography diffraction lines are recorded onto image plates. The crystal sample, filter, and image plates are packaged into one assembly, allowing for accurate and repeatable target to image plate registration. Unconverted laser light impinges upon the device, generating debris, the effects of which have been mitigated. Dimpled blast shields, high strength steel alloy, and high-z tungsten are used to shield and protect the image plates. A tapered opening was designed to provide adequate thickness of shielding materials without blocking the drive beams or x-ray source from reaching the crystal target. The high strength steel unit serves as a mount for the crystal target and x-ray source foil. A tungsten body contains the imaging components. Inside this sub-assembly, there are three image plates: a 160 degree field of view curved plate directly opposite the target opening and two flat plates for the top and bottom. A polycarbonate frame, coated with the appropriate filter material and embedded with registration features for image plate location, is inserted into the diagnostic body. The target assembly is metrologized and then the diagnostic assembly is attached.

  3. Near Edge X-Ray Absorption and X-Ray Photoelectron Diffraction Studies of the Structural Environment of Ge-Si Systems

    NASA Astrophysics Data System (ADS)

    Castrucci, P.; Gunnella, R.; Pinto, N.; Bernardini, R.; de Crescenzi, M.; Sacchi, M.

    Near edge X-ray absorption spectroscopy (XAS), X-ray photoelectron diffraction (XPD) and Auger electron diffraction (AED) are powerful techniques for the qualitative study of the structural and electronic properties of several systems. The recent development of a multiple scattering approach to simulating experimental spectra opened a friendly way to the study of structural environments of solids and surfaces. This article reviews recent X-ray absorption experiments using synchrotron radiation which were performed at Ge L edges and core level electron diffraction measurements obtained using a traditional X-ray source from Ge core levels for ultrathin Ge films deposited on silicon substrates. Thermodynamics and surface reconstruction have been found to play a crucial role in the first stages of Ge growth on Si(001) and Si(111) surfaces. Both techniques show the occurrence of intermixing processes even for room-temperature-grown Ge/Si(001) samples and give a straightforward measurement of the overlayer tetragonal distortion. The effects of Sb as a surfactant on the Ge/Si(001) interface have also been investigated. In this case, evidence of layer-by-layer growth of the fully strained Ge overlayer with a reduced intermixing is obtained when one monolayer of Sb is predeposited on the surface.

  4. THE EFFECT OF SATELLITE LINES FROM THE X-RAY SOURCE ON X-RAY DIFFRACTION PEAKS

    EPA Science Inventory

    The article discusses the development of a method for relating reactivity to crystallite size and strain parameters obtained by the Warren-Averbach technique. EPA has been using crystallite size and strain data obtained from x-ray diffraction (XRD) peak profile analysis to predic...

  5. A portable X-ray diffraction apparatus for in situ analyses of masters' paintings

    NASA Astrophysics Data System (ADS)

    Eveno, Myriam; Duran, Adrian; Castaing, Jacques

    2010-09-01

    It is rare that the analyses of materials in paintings can be carried out by taking micro-samples. Valuable works of art are best studied in situ by non-invasive techniques. For that purpose, a portable X-ray diffraction and fluorescence apparatus has been designed and constructed at the C2RMF. This apparatus has been used for paintings of Rembrandt, Leonardo da Vinci, Van Gogh, Mantegna, etc. Results are given to illustrate the performance of X-ray diffraction, especially when X-ray fluorescence does not bring sufficient information to conclude.

  6. Diffractive X-Ray Telescopes

    NASA Technical Reports Server (NTRS)

    Skinner, Gerald K.

    2010-01-01

    Diffractive X-ray telescopes, using zone plates, phase Fresnel lenses, or related optical elements have the potential to provide astronomers with true imaging capability with resolution many orders of magnitude better than available in any other waveband. Lenses that would be relatively easy to fabricate could have an angular resolution of the order of micro-arc-seconds or even better, that would allow, for example, imaging of the distorted spacetime in the immediate vicinity of the super-massive black holes in the center of active galaxies. What then is precluding their immediate adoption? Extremely long focal lengths, very limited bandwidth, and difficulty stabilizing the image are the main problems. The history, and status of the development of such lenses is reviewed here and the prospects for managing the challenges that they present are discussed.

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

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

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

    2016-07-27

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

  8. In situ and ex situ spectroscopic monitoring of biochar's surface functional groups

    USDA-ARS?s Scientific Manuscript database

    A number of studies described the higher heating temperature (HHT) as the primary pyrolysis parameter dictating the biochar property: surface functional group and fixed carbon contents, O/C, H/C ratios, and Brunauer-Emmett-Teller (BET) surface area. In order to produce desirable biochar properties ...

  9. Time Resolved X-Ray Diffraction Study of Acoustoelectrically Amplified Phonons.

    NASA Astrophysics Data System (ADS)

    Chapman, Leroy Dean

    X-rays diffracted by nearly perfect crystals of n-type InSb have been investigated in the presence of intense acoustoelectrically (A.E.) amplified phonons. The fact that these phonons are nearly monochromatic and have a well defined propagation and polarization direction presents an excellent opportunity to investigate the nature of x -ray photon-phonon scattering in a diffracting crystal. The Debye-Waller factor which accounts for the attenuation of diffracted x-ray intensities due to thermal phonons is reflection dependent owing to its sin (theta)/(lamda) dependence. We have performed experiments comparing the (004) and (008) anomalously transmitted intensities as a function of A.E. amplified flux. The attenuation of both reflections due to the amplified phonons was the same in direct contradiction to an expected sin (theta)/(lamda) dependence. Some possible reasons for this failure are discussed. In a Bragg reflection scattering geometry, the intense monochromatic amplified phonons give rise to satellite peaks symmetrically located about the central elastic Brag peak in a rocking profile. We report in this thesis on the first observation of satellites in a thin crystal Laue transmission geometry. We have theoretically simulated the rocking profiles with some success. The A.E. amplification process in InSb is strongly favored for {110} propagation fast transverse (FT) phonons. In earlier experiments it was found that non-{110} FT phonons were also produced during the amplification process. We have developed a time resolved x-ray counting system which, in conjunction with a spatially resolved x-ray beam and a localized, traveling A.E. phonon distribution, allow the time evolution of the amplified distribution to be followed. We report on time resolved measurements for both the symmetric Bragg and Laue geometries from which we can determine when and where non-{110 } FT flux is generated and restrict the possible mechanisms for its generation.

  10. Unconventional Synthesis of γ-Fe2O3: Excellent Low-Concentration Ethanol Sensing Performance

    NASA Astrophysics Data System (ADS)

    Naskar, Atanu; Narjinary, Mousumi; Kundu, Susmita

    2017-01-01

    This study reports on a simple unconventional procedure for synthesis of γ-Fe2O3 nanopowder and its fabrication as a resistive ethanol sensor. γ-Fe2O3 powder having an average particle size of ˜15 nm was prepared by thermal decomposition of iron(III) acetylacetonate. Platinum incorporation (0.5-1.5 wt.%) was also carried out for enhancing sensing performance. The powders were characterized using an x-ray diffractometer, x-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface area, field area scanning electron microscopy, transmission electron microscopy along with energy dispersion x-ray analyses. Sensor fabricated from pure γ-Fe2O3 exhibited excellent ethanol sensing performance at concentrations down to 1 ppm, having a great demand in medical diagnosis and food-processing industries. The response observed for pure γ-Fe2O3 (˜75% for 1 ppm ethanol) was enhanced ˜10% after 1 wt.% Pt impregnation. Sensors were quite stable and selective towards ethanol vapour detection. A possible mechanism for high sensing performance has been discussed.

  11. 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.

  12. 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.

  13. Single-pulse coherent diffraction imaging using soft x-ray laser.

    PubMed

    Kang, Hyon Chol; Kim, Hyung Taek; Kim, Sang Soo; Kim, Chan; Yu, Tae Jun; Lee, Seong Ku; Kim, Chul Min; Kim, I Jong; Sung, Jae Hee; Janulewicz, Karol A; Lee, Jongmin; Noh, Do Young

    2012-05-15

    We report a coherent diffraction imaging (CDI) using a single 8 ps soft x-ray laser pulse at a wavelength of 13.9 nm. The soft x-ray pulse was generated by a laboratory-scale intense pumping laser providing coherent x-ray pulses up to the level of 10(11) photons/pulse. A spatial resolution below 194 nm was achieved with a single pulse, and it was shown that a resolution below 55 nm is feasible with improved detector capability. The single-pulse CDI might provide a way to investigate dynamics of nanoscale molecules or particles.

  14. Experimental Approaches for Solution X-Ray Scattering and Fiber Diffraction

    PubMed Central

    Irving, T. C.

    2008-01-01

    X-ray scattering and diffraction from non-crystalline systems have gained renewed interest in recent years, as focus shifts from the structural chemistry information gained by high-resolution studies to the context of structural physiology at larger length scales. Such techniques permit the study of isolated macromolecules as well as highly organized macromolecular assemblies as a whole under near-physiological conditions. Time-resolved approaches, made possible by advanced synchrotron instrumentation, add a critical dimension to many of these investigations. This article reviews experimental approaches in non-crystalline x-ray scattering and diffraction that may be used to illuminate important scientific questions such as protein/nucleic acid folding and structure-function relationships in large macromolecular assemblies. PMID:18801437

  15. 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

  16. Neutron and X-Ray Diffraction Studies of Advanced Materials

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

    Barabash, Rozaliya; Tiley, Jaimie; Wang, Yandong

    2010-01-01

    The selection of articles in the special topic 'Neutron and X-Ray Studies of Advanced Materials' is based on the materials presented during the TMS 2009 annual meeting in San Francisco, CA, February 15-19, 2009. The development of ultrabrilliant third-generation synchrotron X-ray sources, together with advances in X-ray optics, has created intense X-ray microbeams, which provide the best opportunities for in-depth understanding of mechanical behavior in a broad spectrum of materials. Important applications include ultrasensitive elemental detection by X-ray fluorescence/absorption and microdiffraction to identify phase and strain with submicrometer spatial resolution. X-ray microdiffraction is a particularly exciting application compared with alternativemore » probes of crystalline structure, orientation, and strain. X-ray microdiffraction is nondestructive with good strain resolution, competitive or superior spatial resolution in thick samples, and with the ability to probe below the sample surface. Moreover, the high-energy X-ray diffraction technique provides an effective tool for characterizing the mechanical and functional behavior in various environments (temperature, stress, and magnetic field). At the same time, some neutron diffraction instruments constructed mainly for the purpose of engineering applications can be found at nearly all neutron facilities. The first generation-dedicated instruments designed for studying in-situ mechanical behavior have been commissioned and used, and industrial standards for reliable and repeatable measurements have been developed. Furthermore, higher penetration of neutron beams into most engineering materials provides direct measurements on the distribution of various stresses (i.e., types I, II, and III) beneath the surface up to several millimeters, even tens of millimeters for important industrial components. With X-ray and neutron measurements, it is possible to characterize material behavior at different length

  17. Efficient solar light-driven degradation of Congo red with novel Cu-loaded Fe3O4@TiO2 nanoparticles.

    PubMed

    Arora, Priya; Fermah, Alisha; Rajput, Jaspreet Kaur; Singh, Harminder; Badhan, Jigyasa

    2017-08-01

    In this work, Cu-loaded Fe 3 O 4 @TiO 2 core shell nanoparticles were prepared in a single pot by coating of TiO 2 on Fe 3 O 4 nanoparticles followed by Cu loading. X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HR-TEM), thermogravimetric analysis (TGA), Brunauer-Emmett- Teller (BET), vibrating sample magnetometry (VSM), X-ray photoelectron spectroscopy (XPS), and valence band X-ray photoelectron spectroscopy (VB XPS) techniques were used for characterization of as prepared nanoparticles. Synergism between copper and titania was evaluated by studying the solar light-driven photodegradation of Congo red dye solution in the presence of Fe 3 O 4 @TiO 2 nanoparticles on one side and Cu-loaded Fe 3 O 4 @TiO 2 nanoparticles on the other side. The latter performed better than the former catalyst, indicating the enhanced activity of copper-loaded catalyst. Further photodegradation was studied by three means, i.e., under ultraviolet (UV), refluxing, and solar radiations. Cu-loaded Fe 3 O 4 @TiO 2 enhanced the degradation efficiency of Congo red dye. Thus, Cu act possibly by reducing the band gap of TiO 2 and widening the optical response of semiconductor, as a result of which solar light could be used to carry out photocatalysis. Graphical abstract Photodegradation of congo red over Cu-loaded Fe 3 O 4 @TiO 2 nanoparticles.

  18. In Situ 3D Coherent X-ray Diffraction Imaging of Shock Experiments: Possible?

    NASA Astrophysics Data System (ADS)

    Barber, John

    2011-03-01

    In traditional coherent X-ray diffraction imaging (CXDI), a 2D or quasi-2D object is illuminated by a beam of coherent X-rays to produce a diffraction pattern, which is then manipulated via a process known as iterative phase retrieval to reconstruct an image of the original 2D sample. Recently, there have been dramatic advances in methods for performing fully 3D CXDI of a sample from a single diffraction pattern [Raines et al, Nature 463 214-7 (2010)], and these methods have been used to image samples tens of microns in size using soft X-rays. In this work, I explore the theoretical possibility of applying 3D CXDI techniques to the in situ imaging of the interaction between a shock front and a polycrystal, a far more stringent problem. A delicate trade-off is required between photon energy, spot size, imaging resolution, and the dimensions of the experimental setup. In this talk, I will outline the experimental and computational requirements for performing such an experiment, and I will present images and movies from simulations of one such hypothetical experiment, including both the time-resolved X-ray diffraction patterns and the time-resolved sample imagery.

  19. Compact ultrahigh vacuum sample environments for x-ray nanobeam diffraction and imaging.

    PubMed

    Evans, P G; Chahine, G; Grifone, R; Jacques, V L R; Spalenka, J W; Schülli, T U

    2013-11-01

    X-ray nanobeams present the opportunity to obtain structural insight in materials with small volumes or nanoscale heterogeneity. The effective spatial resolution of the information derived from nanobeam techniques depends on the stability and precision with which the relative position of the x-ray optics and sample can be controlled. Nanobeam techniques include diffraction, imaging, and coherent scattering, with applications throughout materials science and condensed matter physics. Sample positioning is a significant mechanical challenge for x-ray instrumentation providing vacuum or controlled gas environments at elevated temperatures. Such environments often have masses that are too large for nanopositioners capable of the required positional accuracy of the order of a small fraction of the x-ray spot size. Similarly, the need to place x-ray optics as close as 1 cm to the sample places a constraint on the overall size of the sample environment. We illustrate a solution to the mechanical challenge in which compact ion-pumped ultrahigh vacuum chambers with masses of 1-2 kg are integrated with nanopositioners. The overall size of the environment is sufficiently small to allow their use with zone-plate focusing optics. We describe the design of sample environments for elevated-temperature nanobeam diffraction experiments demonstrate in situ diffraction, reflectivity, and scanning nanobeam imaging of the ripening of Au crystallites on Si substrates.

  20. Compact ultrahigh vacuum sample environments for x-ray nanobeam diffraction and imaging

    NASA Astrophysics Data System (ADS)

    Evans, P. G.; Chahine, G.; Grifone, R.; Jacques, V. L. R.; Spalenka, J. W.; Schülli, T. U.

    2013-11-01

    X-ray nanobeams present the opportunity to obtain structural insight in materials with small volumes or nanoscale heterogeneity. The effective spatial resolution of the information derived from nanobeam techniques depends on the stability and precision with which the relative position of the x-ray optics and sample can be controlled. Nanobeam techniques include diffraction, imaging, and coherent scattering, with applications throughout materials science and condensed matter physics. Sample positioning is a significant mechanical challenge for x-ray instrumentation providing vacuum or controlled gas environments at elevated temperatures. Such environments often have masses that are too large for nanopositioners capable of the required positional accuracy of the order of a small fraction of the x-ray spot size. Similarly, the need to place x-ray optics as close as 1 cm to the sample places a constraint on the overall size of the sample environment. We illustrate a solution to the mechanical challenge in which compact ion-pumped ultrahigh vacuum chambers with masses of 1-2 kg are integrated with nanopositioners. The overall size of the environment is sufficiently small to allow their use with zone-plate focusing optics. We describe the design of sample environments for elevated-temperature nanobeam diffraction experiments demonstrate in situ diffraction, reflectivity, and scanning nanobeam imaging of the ripening of Au crystallites on Si substrates.

  1. Titration of a Solid Acid Monitored by X-Ray Diffraction

    ERIC Educational Resources Information Center

    Dungey, Keenan E.; Epstein, Paul

    2007-01-01

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

  2. Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA.

    PubMed

    Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

    2014-05-01

    Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the `diffraction before destruction' scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles.

  3. Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA

    PubMed Central

    Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

    2014-01-01

    Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the ‘diffraction before destruction’ scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles. PMID:24763651

  4. Preparation of MoO2/g-C3N4 composites with a high surface area and its application in deep desulfurization from model oil

    NASA Astrophysics Data System (ADS)

    Hou, Liang-pei; Zhao, Rong-xiang; Li, Xiu-ping; Gao, Xiao-han

    2018-03-01

    A series of catalysts of composition X-MoO2/g-C3N4 (X = 0, 0.5, 1, 3, 5 wt.%) were successfully synthesized by calcination of a mixture of (NH4)6Mo7O24·4H2O and g-C3N4. Oxidative desulfurization experiments were conducted using X-MoO2/g-C3N4 as a catalyst, H2O2 as an oxidant, and ionic liquids (ILs) as extraction agents. Catalysts were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared (FT-IR), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), and Brunauer-Emmett-Teller analysis (BET). Characterization results suggested that MoO2 was present in the catalyst and its crystallinity improved with increased Mo-loading. The catalysts had a larger specific surface area due to the presence of MoO2 dispersed on g-C3N4. Experimental results showed that 3%-MoO2/g-C3N4 had the highest catalytic activity among all the catalysts tested. A desulfurization rate of 96.0% was achieved under optimal conditions. Through gas chromatography-mass spectrometry (GC-MS) analysis, it was shown that dibenzothoiphene sulfone was the sole product of the oxidation desulfurization reaction. An apparent activation energy of 61.1 kJ/mol was estimated based on Arrhenius equation. The activity of 3%-MoO2/g-C3N4 slightly decreased after six runs. A possible mechanism for the reaction has been proposed.

  5. 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

  6. High spatial resolution X-ray and gamma ray imaging system using diffraction crystals

    DOEpatents

    Smither, Robert K [Hinsdale, IL

    2011-05-17

    A method and a device for high spatial resolution imaging of a plurality of sources of x-ray and gamma-ray radiation are provided. The device comprises a plurality of arrays, with each array comprising a plurality of elements comprising a first collimator, a diffracting crystal, a second collimator, and a detector.

  7. 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

  8. X-ray diffraction patterns and diffracted intensity of Kα spectral lines of He-like ions

    NASA Astrophysics Data System (ADS)

    Goyal, Arun; Khatri, Indu; Singh, A. K.; Sharma, Rinku; Mohan, Man

    2017-09-01

    In the present paper, we have calculated fine-structure energy levels related to the configurations 1s2s, 1s2p, 1s3s and 1s3p by employing GRASP2K code. We have also computed radiative data for transitions from 1s2p 1 P1o, 1s2p 3 P2o, 1s2p 3 P1o and 1s2s 3S1 to the ground state 1s2. We have made comparisons of our presented energy levels and transition wavelengths with available results compiled by NIST and good agreement is achieved. We have also provided X-ray diffraction (XRD) patterns of Kα spectral lines, namely w, x, y and z of Cu XXVIII, Kr XXXV and Mo with diffraction angle and maximum diffracted intensity which is not published elsewhere in the literature. We believe that our presented results may be beneficial in determination of the order parameter, X-ray crystallography, solid-state drug analysis, forensic science, geological and medical applications.

  9. 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.

  10. Spread spectrum phase modulation for coherent X-ray diffraction imaging.

    PubMed

    Zhang, Xuesong; Jiang, Jing; Xiangli, Bin; Arce, Gonzalo R

    2015-09-21

    High dynamic range, phase ambiguity and radiation limited resolution are three challenging issues in coherent X-ray diffraction imaging (CXDI), which limit the achievable imaging resolution. This paper proposes a spread spectrum phase modulation (SSPM) method to address the aforementioned problems in a single strobe. The requirements on phase modulator parameters are presented, and a practical implementation of SSPM is discussed via ray optics analysis. Numerical experiments demonstrate the performance of SSPM under the constraint of available X-ray optics fabrication accuracy, showing its potential to real CXDI applications.

  11. Analytical characterization of a new mobile X-ray fluorescence and X-ray diffraction instrument combined with a pigment identification case study

    NASA Astrophysics Data System (ADS)

    Van de Voorde, Lien; Vekemans, Bart; Verhaeven, Eddy; Tack, Pieter; De Wolf, Robin; Garrevoet, Jan; Vandenabeele, Peter; Vincze, Laszlo

    2015-08-01

    A new, commercially available, mobile system combining X-ray diffraction and X-ray fluorescence has been evaluated which enables both elemental analysis and phase identification simultaneously. The instrument makes use of a copper or molybdenum based miniature X-ray tube and a silicon-Pin diode energy-dispersive detector to count the photons originating from the samples. The X-ray tube and detector are both mounted on an X-ray diffraction protractor in a Bragg-Brentano θ:θ geometry. The mobile instrument is one of the lightest and most compact instruments of its kind (3.5 kg) and it is thus very useful for in situ purposes such as the direct (non-destructive) analysis of cultural heritage objects which need to be analyzed on site without any displacement. The supplied software allows both the operation of the instrument for data collection and in-depth data analysis using the International Centre for Diffraction Data database. This paper focuses on the characterization of the instrument, combined with a case study on pigment identification and an illustrative example for the analysis of lead alloyed printing letters. The results show that this commercially available light-weight instrument is able to identify the main crystalline phases non-destructively, present in a variety of samples, with a high degree of flexibility regarding sample size and position.

  12. Structural investigation of porcine stomach mucin by X-ray fiber diffraction and homology modeling

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

    Veluraja, K., E-mail: veluraja@msuniv.ac.in; Vennila, K.N.; Umamakeshvari, K.

    Research highlights: {yields} Techniques to get oriented mucin fibre. {yields} X-ray fibre diffraction pattern for mucin. {yields} Molecular modeling of mucin based on X-ray fibre diffraction pattern. -- Abstract: The basic understanding of the three dimensional structure of mucin is essential to understand its physiological function. Technology has been developed to achieve orientated porcine stomach mucin molecules. X-ray fiber diffraction of partially orientated porcine stomach mucin molecules show d-spacing signals at 2.99, 4.06, 4.22, 4.7, 5.37 and 6.5 A. The high intense d-spacing signal at 4.22 A is attributed to the antiparallel {beta}-sheet structure identified in the fraction of themore » homology modeled mucin molecule (amino acid residues 800-980) using Nidogen-Laminin complex structure as a template. The X-ray fiber diffraction signal at 6.5 A reveals partial organization of oligosaccharides in porcine stomach mucin. This partial structure of mucin will be helpful in establishing a three dimensional structure for the whole mucin molecule.« less

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

    DOE PAGES

    Beetz, T.; Howells, M. R.; Jacobsen, C.; ...

    2005-03-14

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

  14. 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

  15. Retention of barium and europium radionuclides from aqueous solutions on ash-based sorbents by application of radiochemical techniques.

    PubMed

    Noli, Fotini; Kapnisti, Maria; Buema, Gabriela; Harja, Maria

    2016-10-01

    New materials were synthesized for application in sorption of radionuclides from aqueous solutions. The elaboration was performed by conversion of power plant ash using the hydrothermal method under optimum experimental conditions. Sodalite, Na-Y, and analcime were formed from ash precursor during the treatment, exhibiting thermal stability as revealed by the characterization by X-ray diffraction (XRD) and thermogravimetric differential thermal analysis (TG-DTA). The Brunauer-Emmett-Teller (BET) surface area and pore volume were determined and they presented higher values than plant ash. The ability of the new products to retain Ba and Eu radionuclides was studied in aqueous solutions using (133)Ba and (152)Eu as tracers and γ-ray spectroscopy under batch experiments. The experimental data were modeled by the Langmuir and Freundlich equations, whereas sorption kinetics measurements were performed at 293, 308, and 323K and thermodynamic parameters were calculated. The release of the sorbed ions into the environment was also tested by leaching experiments. The results of these tests indicated that the synthesized materials are very efficient in removing the aforementioned metals from aqueous solutions and can be considered as potential low-cost sorbents in nuclear waste management. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Photo-degradation of basic green 1 and basic red 46 dyes in their binary solution by La2O3-Al2O3nanocomposite using first-order derivative spectra and experimental design methodology.

    PubMed

    Fahimirad, Bahareh; Asghari, Alireza; Rajabi, Maryam

    2017-05-15

    In this work, the lanthanum oxide-aluminum oxide (La 2 O 3 -Al 2 O 3 ) nanocomposite is introduced as an efficient photocatalyst for the photo-degradation of the dyes basic green 1 (BG1) and basic red 46 (BR46) in their binary aqueous solution under the UV light irradiation. The properties of this catalyst are determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), Brunauer-Emmett-Teller (BET), and UV-visible spectrophotometry. The first-order derivative spectra are used for the simultaneous analysis of the dyes in their binary solution. The screening investigations indicate that five parameters including the catalyst dosage, concentration of the dyes, irradiation time, and solution pH have significant effects on the photo-degradation of the dyes. The effects of these variables together with their interactions in the photo-degradation of the dyes are studied using the Box-Behnken design (BBD). Under the optimum experimental conditions, obtained via the desirability function, the photo-catalytic activities of La 2 O 3 -Al 2 O 3 and pure Al 2 O 3 are also investigated. The results obtained show an enhancement in the photo-catalytic activity when La 2 O 3 nanoparticles are loaded on the surface of Al 2 O 3 nanoparticles. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Decoration of nitrogen-doped reduced graphene oxide with cobalt tungstate nanoparticles for use in high-performance supercapacitors

    NASA Astrophysics Data System (ADS)

    Naderi, Hamid Reza; Sobhani-Nasab, Ali; Rahimi-Nasrabadi, Mehdi; Ganjali, Mohammad Reza

    2017-11-01

    A composite of cobalt tungstate nanoparticles coated on nitrogen-doped reduced graphene oxide (CoWO4/NRGO) was prepared through an in situ sonochemical approach. The composite was next evaluated as an electrode material for use supercapacitors electrodes. The characterization of the various CoWO4/NRGO nanocomposite samples was carried out through field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), X-ray photoemission spectroscopy (XPS), Brunauer-Emmett-Teller (BET) method and Raman spectroscopy. Complementary studies were also performed through cyclic voltammetry (CV), galvanostatic charge/discharge, electrochemical impedance spectroscopy (EIS), and continues cyclic voltammetry (CCV). The electrochemical evaluations were carried out in a 2 M H2SO4 solution as the electrolyte. The electrochemical evaluations on the nano-composite samples indicated that CoWO4/NRGO-based electrodes reveal enhanced supercapacitive characteristics (i.e. a high specific capacitance (SC) of 597 F g-1 at a scan rate of 5 mV s-1, an energy density (ED) value of 67.9 W h kg-1, and high rate capability). CCV studies indicated that CoWO4/NRGO-based electrodes keep 97.1% of their original capacitance after 4000 cycles. The results led to the conclusion that CoWO4/NRGO effectively merge the merits of CoWO4 and CoWO4/RGO in one new nanocomposite material.

  18. Multi-applicative tetragonal TiO2/SnO2 nanocomposites for photocatalysis and gas sensing

    NASA Astrophysics Data System (ADS)

    Patil, S. M.; Dhodamani, A. G.; Vanalakar, S. A.; Deshmukh, S. P.; Delekar, S. D.

    2018-04-01

    TiO2-based mixed metal oxide heteronanostructures have multiple applications in photocatalysis and gas sensing because of their charge transport properties. In this study, we prepared tetragonal TiO2/SnO2 nanocomposites (NCs) with different weight percentages using a simple wet impregnation method. The physicochemical properties of the NCs were investigated using X-ray diffraction, Fourier transform-infrared spectroscopy, ultraviolet-visible spectroscopy, field-emission scanning electron microscopy, energy dispersive X-ray spectroscopy, transmission electron microscopy, and Brunauer-Emmett-Teller surface area analysis. The results showed that the surface area of the NCs increased significantly and the anatase TiO2 was sensitized after the addition of a small amount of cassiterite SnO2 NPs. We systematically studied the as-prepared NCs during the photocatalytic degradation of Congo Red dye under visible light irradiation (λ > 420 nm) and NH3 gas sensing, which demonstrated the efficient photocatalytic performance and the superior sensing response of the catalyst with a weight composition of 25% SnO2 in TiO2 (4:1) compared with the other NCs or the bare individual nanoparticles. The improved photocatalytic and gas sensing performance of the TiO2/SnO2 (4:1) NCs may be attributed to the increased active surface area, the increased adsorption of the dye and target gas molecules, as well as efficient electron-hole charge separation and transfer.

  19. One-step electrospinning synthesis of TiO2/g-C3N4 nanofibers with enhanced photocatalytic properties

    NASA Astrophysics Data System (ADS)

    Tang, Qian; Meng, Xianfeng; Wang, Zhiying; Zhou, Jianwei; Tang, Hua

    2018-02-01

    TiO2/g-C3N4 composite nanofibers have been successfully synthesized by one-step electrospinning method, using titanium (IV) n-butoxide (TNBT) and urea as raw materials. The structure and compositions of TiO2/g-C3N4 samples are characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Diffuse reflectance spectroscopy (DRS), Scanning electron microscopy (SEM), Transmission electron microscope (TEM), X-ray photoelectron spectrometer (XPS) and Brunauer-Emmett-Teller (BET), respectively. The results show that the porous uniform TiO2/g-C3N4 composite nanofibers, with diameter of 100-150 nm, can be successfully prepared through electrospinning method combining 550 °C calcination process. The photocatalytic activity is evaluated by the degradation of rhodamine B (RhB) under simulated solar light. The enhanced catalytic activity is attributed predominantly to the heterojunction between TiO2 and g-C3N4, which promotes the transferring of carriers and prohibits their recombination. With the optimal doping amount of 0.6 g urea (corresponding to 3 g TNBT), the TiO2/g-C3N4 composite nanofibers exhibit the highest rate towards the photocatalytic degradation of RhB. A diagram is presented to explicate the mechanism of the whole catalytic experiment. This study might provide a promising future of applying green catalysts to solving water pollution problems.

  20. Comparison of the solar photocatalytic activity of ZnO-Fe2O3 and ZnO-Fe(0) on 2,4-D degradation in a CPC reactor.

    PubMed

    Maya-Treviño, M L; Villanueva-Rodríguez, M; Guzmán-Mar, J L; Hinojosa-Reyes, L; Hernández-Ramírez, A

    2015-03-01

    In this work a comparative study of the catalytic activity of ZnO-Fe2O3 and ZnO-Fe(0) 0.5 wt% materials was carried out in the degradation of 2,4-dichlorophenoxyacetic acid (2,4-D) as a commercial formulation Hierbamina®, using a compound parabolic collector (CPC) reactor. The catalysts were synthesized by the sol-gel method and characterized by X-ray diffraction, UV-Vis diffuse reflectance spectroscopy, Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy. The textural properties of solids were determined from N2 adsorption isotherms using the Brunauer-Emmett-Teller (BET) method. The incorporation of Fe(0) onto ZnO was demonstrated by X-ray photoelectron spectroscopy analysis. The photocatalytic tests were performed at pH 7, using 10 mg L(-1) of herbicide and 0.5 g L(-1) of catalyst loading. The decay in herbicide concentration was followed by reversed-phase chromatography. A complete degradation of 2,4-D was achieved using ZnO-Fe(0) while 47% of herbicide removal was attained with ZnO-Fe2O3 mixed oxide for an accumulated energy QUV ≈ 2 kJ L(-1). The removal percentage of total organic carbon (TOC) during the solar photocatalytic process was superior using ZnO-Fe(0), achieving 45% compared to the 15% obtained with the mixed oxide catalyst.

  1. Development of CdS Nanostructures by Thermal Decomposition of Aminocaproic Acid-Mixed Cd-Thiourea Complex Precursor: Structural, Optical and Photocatalytic Characterization.

    PubMed

    Patel, Jayesh D; Mighri, Frej; Ajji, Abdellah; Chaudhuri, Tapas K

    2015-04-01

    The present work deals with two different CdS nanostructures produced via hydrothermal and solvothermal decompositions of aminocaproic acid (ACA)-mixed Cd-thiourea complex precursor at 175 °C. Both nanostructures were extensively characterized for their structural, morphological and optical properties. The powder X-ray diffraction characterization showed that the two CdS nanostructures present a wurtzite morphology. Scanning electron microscopy and energy-dispersive X-ray characterizations revealed that the hydrothermal decomposition produced well-shaped CdS flowers composed of six dendritic petals, and the solvothermal decomposition produced CdS microspheres with close stoichiometric chemical composition. The UV-vis absorption and photoluminescence spectra of CdS dendritic flowers and microsphere nanostructures showed that both nanostructures present a broad absorption between 200 and 700 nm and exhibit strong green emissions at 576 and 520 nm upon excitations at 290 nm and 260 nm, respectively. The transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) characterizations confirmed that CdS microspheres were mesoporous and were composed of small nanocrystals. A possible growth mechanism in the formation of the CdS nanostructures was proposed based on morphology evolution as a function of the reaction time. Furthermore, the as-synthesized CdS nanostructures were found to exhibit highly efficient photocatalytic activities for the degradation of methyl orange (MeO) and rhodamine B (RhB) dyes.

  2. Synthesis of cerium and nickel doped titanium nanofibers for hydrolysis of sodium borohydride.

    PubMed

    Tamboli, Ashif H; Gosavi, S W; Terashima, Chiaki; Fujishima, Akira; Pawar, Atul A; Kim, Hern

    2018-07-01

    A recyclable titanium nanofibers, doped with cerium and nickel doped was successfully synthesized by using sol-gel and electrospinning method for hydrogen generation from alkali free hydrolysis of NaBH 4 . The resultant nanocomposite was characterized to find out the structural and physical-chemical properties by a series of analytical techniques such as FT-IR (Fourier transform infrared spectroscopy), XRD (X-ray diffraction), SEM (scanning electron microscope), EDX (energy-dispersive X-ray spectroscopy),N 2 adsorption-desorption and BET (Brunauer-Emmett-Teller), etc. The results revealed that cerium and nickel nanoparticles were homogeneously distributed on the surface of the TiO 2 nanofibers due to having similar oxidation state and atomic radium of TiO 2 nanofibers with CeO 2 and NiO for the effective immobilization of metal ions. The NiO doped catalyst showed superior catalytic performance towards the hydrolysis reaction of NaBH 4 at room temperature. These catalysts have ability to produce 305 mL of H 2 within the time of 160 min at room temperature. Additionally, reusability test revealed that the catalyst is active even after five runs of hydrolytic reaction, implying the as-prepared NiO doped TiO 2 nanofibers could be considered as a potential candidate catalyst for portable hydrogen fuel system such as PEMFC (proton exchange membrane fuel cells). Copyright © 2018 Elsevier Ltd. All rights reserved.

  3. Dechlorination of disinfection by-product monochloroacetic acid in drinking water by nanoscale palladized iron bimetallic particle.

    PubMed

    Chen, Chao; Wang, Xiangyu; Chang, Ying; Liu, Huiling

    2008-01-01

    Nanoscale palladized iron (Pd/Fe) bimetallic particles were prepared by reductive deposition method. The particles were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscope (SEM), transmission electron microscope (TEM), and Brunauer-Emmett-Teller-nitrogen (BET-N2) method. Data obtained from those methods indicated that nanoscale Pd/Fe bimetallic particles contained alpha-Fe0. Detected Pd to Fe ratio by weight (Pd/Fe ratio) was close to theoretical value. Spherical granules with diameter of 47 +/- 11.5 nm connected with one another to form chains and the chains composed nanoscale Pd/Fe bimetallic particles. Specific surface area of particles was 51 m2/g. The factors, such as species of reductants, Pd/Fe ratio, dose of nanoscale Pd/Fe bimetallic particles added into solutions, solution initial pH, and a variety of solvents were studied. Dechlorination effect of monochloroacetic acid by different reductants followed the trend: nanoscale Pd/Fe bimetallic particles of 0.182% Pd/Fe > nanoscale Fe > reductive Fe. When the Pd/Fe ratio was lower than 0.083%, increasing Pd/Fe ratio would increase dechlorination efficiency (DE) of MCAA. When the Pd/Fe ratio was higher than 0.083%, increasing Pd/Fe ratio caused a decrease in DE. Adding more nanoscale Pd/Fe bimetallic particles to solution would enhance DE. The DE of MCAA decreased as initial pH of solution increased.

  4. Synthesis of graphene supported Li2SiO3 as a high performance anode material for lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Yang, Shuai; Wang, Qiufen; Miao, Juan; Zhang, Jingyang; Zhang, Dafeng; Chen, Yumei; Yang, Hong

    2018-06-01

    The Li2SiO3-graphene composite is successfully synthesized through an easy hydrothermal method. The structures and morphologies of the produced samples are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectrum, Brunauer-Emmett-Teller formalism, scanning electron microscope, transmission electron microscope, and electrochemistry methods. The result shows a well crystalline of the Li2SiO3-GE composite. The existence of graphene doesn't change the crystalline of Li2SiO3. In addition, the Li2SiO3 compound with an average diameter of 20 nm can be seen on the surface of graphene with uniform distribution. After the composite with graphene, the composite displays large surface area which ensures the well electrochemistry of the composite. Finally, the Li2SiO3-graphene composite delivers a high initial capacity of 878.3 mAh g-1 at 1C as well as a high recovery capacity of 400 mAh g-1 after 200 cycles. When charged and discharged at high rate, the Li2SiO3-doping graphene composite still exhibits a high specific capacity of 748.3 mAh g-1 (at 2C, and 576 mAh g-1 at 5C) and well cycling performance. The well synthesized composite possesses well structure and well electrochemistry performance.

  5. Bi-template assisted synthesis of mesoporous manganese oxide nanostructures: Tuning properties for efficient CO oxidation.

    PubMed

    Roy, Mouni; Basak, Somjyoti; Naskar, Milan Kanti

    2016-02-21

    A simple soft bi-templating process was used for the synthesis of mesoporous manganese oxide nanostructures using KMnO4 as a precursor and polyethylene glycol and cetyltrimethylammonium bromide as templates in the presence of benzaldehyde as an organic additive in alkaline media, followed by calcination at 400 °C. X-ray diffraction and Raman spectroscopic analysis of the calcined products confirmed the existence of stoichiometric (MnO2 and Mn5O8) and non-stoichiometric mixed phases (MnO2 + Mn5O8) of Mn oxides obtained by tuning the concentration of the additive and the synthesis time. The surface properties of the prepared Mn oxides were determined by X-ray photoelectron spectroscopy. The mesoporosity of the samples was confirmed by N2 adsorption-desorption. Different synthetic conditions resulted in the formation of different morphologies of the Mn oxides (α-MnO2, Mn5O8, and α-MnO2 + Mn5O8), such as nanoparticles, nanorods, and nanowires. The synthesized mesoporous Mn oxide nanostructures were used for the catalytic oxidation of the harmful air pollutant carbon monoxide. The Mn5O8 nanoparticles with the highest Brunauer-Emmett-Teller surface area and the non-stoichiometric manganese oxide (α-MnO2 + Mn5O8) nanorods with a higher Mn(3+) concentration had the best catalytic efficiency.

  6. Modifying surface properties of KIT-6 zeolite with Ni and V for enhancing catalytic CO methanation

    NASA Astrophysics Data System (ADS)

    Cao, Hong-Xia; Zhang, Jun; Guo, Cheng-Long; Chen, Jingguang G.; Ren, Xiang-Kun

    2017-12-01

    The surface of the KIT-6 zeolite was modified with different amounts of Ni and V to promote the catalytic properties for CO methanation. A series of xNi-yV/KIT-6 with various Ni and V contents were prepared by the incipient-wetness impregnation method. The modified surfaces were characterized using N2 adsorption-desorption, Brunauer-Emmett-Teller (BET), X-ray diffraction (XRD), hydrogen temperature-programmed reduction (H2-TPR), Fourier transformed infrared spectroscopy (FT-IR), Raman, X-ray photoelectron spectroscopy (XPS), transmission electron microscope (TEM), and energy-dispersive X-ray spectroscopy (EDX), respectively. The characterization results illustrated that the modification of V species was able to significantly promote low-temperature catalytic performance below 350 °C compared to that of unmodified Ni/KIT-6, which was likely due to an increase in the H2 uptake accompanied by enhanced CO dissociation derived from stronger electron transfer from V species to Ni0. Correspondingly, the xNi-yV/KIT-6 catalysts exhibited a distinct enhancement in CO conversion, CH4 selectivity and CH4 yield over unmodified Ni/KIT-6. Among all catalysts, 20Ni-2V/KIT-6 showed the best catalytic performance, corresponding to nearly 100% CO conversion and 85% CH4 yield at a low temperature of 300 °C. Furthermore, 20Ni-2V/KIT-6 presented enhanced coking-resistant and anti-sintering properties during a 60h-lifetime test at 500 °C and 1 atm with a high weight hourly space velocity (WHSV) of 60000 ml/g/h.

  7. Quantitative determination of mineral composition by powder x-ray diffraction

    DOEpatents

    Pawloski, G.A.

    1984-08-10

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

  8. Quantitative determination of mineral composition by powder X-ray diffraction

    DOEpatents

    Pawloski, Gayle A.

    1986-01-01

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

  9. Crystallographic Characterization of Extraterrestrial Materials by Energy-Scanning X-ray Diffraction

    NASA Technical Reports Server (NTRS)

    Hagiya, Kenji; Mikouchi, Takashi; Ohsumi, Kazumasa; Terada, Yasuko; Yagi, Naoto; Komatsu, Mutsumi; Yamaguchi, Shoki; Hirata, Arashi; Kurokawa, Ayaka; Zolensky, Michael E. (Principal Investigator)

    2016-01-01

    We have continued our long-term project using X-ray diffraction to characterize a wide range of extraterrestrial samples. The stationary sample method with polychromatic X-rays is advantageous because the irradiated area of the sample is always same and fixed, meaning that all diffraction spots occur from the same area of the sample, however, unit cell parameters cannot be directly obtained by this method though they are very important for identification of mineral and for determination of crystal structures. In order to obtain the cell parameters even in the case of the sample stationary method, we apply energy scanning of a micro-beam of monochromatic SR at SPring-8.

  10. 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

  11. 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.

  12. Femtosecond X-ray Diffraction: Applications for Laser-Irradiated Materials

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

    Wark, Justin S.

    2009-09-10

    Over the past few years short pulse x-ray diffraction at the nanosecond and picosecond level has become an established technique in many high-power laser laboratories for interrogating the lattice response of laser-perturbed and shocked matter, and is now finding applications in diagnosing the state of crystalline materials subject to quasi-isentropic compression. We review some of the previous results obtained in this area, for example the direct observation of coherent phonons, the first direct confirmation of the alpha-epsilon transition in shocked iron, and recent measurements indicating that the strength of matter can be measured at shock pressures exceeding a Mbar. Themore » majority of sources used to date have been laser-plasma based, with some work being performed using 3{sup rd} generation synchrotron sources. However, the development of 4{sup th} generation x-ray free-electron lasers, such as LCLS, afford many new opportunities, with pulse lengths in the femtosecond regime. The extremely low divergence and monochromatic nature of the LCLS beam make it well suited to study compressed polycrystalline matter, especially samples with small grain sizes. At extremely short pulse lengths, such that the pulse is shorter than an x-ray extinction depth traversal time, the diffraction process itself becomes time-dependent, and in certain cases the full wave-field solution will be required, particularly if the matter itself is being rapidly perturbed, as will occur if the intense x-ray radiation is used to create warm dense matter, as in recent experiments on FLASH at DESY.« less

  13. 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

  14. Ultrasound-assisted facile synthesis of a new tantalum(V) metal-organic framework nanostructure: Design, characterization, systematic study, and CO2 adsorption performance

    NASA Astrophysics Data System (ADS)

    Sargazi, Ghasem; Afzali, Daryoush; Mostafavi, Ali; Ebrahimipour, S. Yousef

    2017-06-01

    This work presents a fast route for the preparation of a new Ta(V) metal-organic framework nanostructure with high surface area, significant porosity, and small size distribution. X-ray diffraction (XRD), scanning electron microscopy (SEM), Transition electron microscopy (TEM), energy dispersive spectrometer (EDS), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), CHNS/O elemental analyser, and Brunauer-Emmett-Teller (BET) surface area analysis were applied to characterize the synthesized product. Moreover, the influences of ultrasonic irradiation including temperature, time, and power on different features of the final products were systematically studied using 2k-1 factorial design experiments, and the response surface optimization was used for determining the best welding parameter combination. The results obtained from analyses of variances showed that ultrasonic parameters affected the size distribution, thermal behaviour, and surface area of Ta-MOF samples. Based on response surface methodology, Ta-MOF could be obtained with mean diameter of 55 nm, thermal stability of 228 °C, and high surface area of 2100 m2/g. The results revealed that the synthesized products could be utilized in various applications such as a novel candidate for CO2 adsorption.

  15. Selective determination of caffeine in foods with 3D-graphene based ultrasound-assisted magnetic solid phase extraction.

    PubMed

    Rahimi, Afshin; Zanjanchi, Mohammad Ali; Bakhtiari, Sadjad; Dehsaraei, Mohammad

    2018-10-01

    An efficient method was applied for extraction of caffeine in food samples. Three-dimensional graphene-Fe 3 O 4 (3D-G-Fe 3 O 4 ) nanoparticles was successfully synthesized and used as adsorbent in magnetic solid phase extraction (MSPE) step. The properties of synthesized adsorbent were characterized by fourier-transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), vibrating sample magnetometer (VSM), X-ray diffraction (XRD), Raman spectroscopy, Brunauer-Emmett-Teller (BET) and Barrett-Joyner-Halenda (BJH) methods. The influence of main parameters of extraction procedure such as ultrasound parameter, amount of nanoparticles, pH, salt concentration and desorption condition were investigated and optimized. Under the optimized experimental conditions, the figure of merit results showed excellent linear dynamic range (LDR) of 0.5-500 µg mL -1 , with determination coefficient (R 2 ) higher than 0.996 and limit of detection (LOD) of 0.1 µg mL -1 . Intra- and inter-day relative standard deviations (RSDs) were less than 5.9 and 7.1%, respectively. The method was successfully applied for determination of caffeine in different food samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

  16. Electrical, thermal and electrochemical properties of disordered carbon prepared from palygorskite and cane molasses

    NASA Astrophysics Data System (ADS)

    Alvarez, Edelio Danguillecourt; Laffita, Yodalgis Mosqueda; Montoro, Luciano Andrey; Della Santina Mohallem, Nelcy; Cabrera, Humberto; Pérez, Guillermo Mesa; Frutis, Miguel Aguilar; Cappe, Eduardo Pérez

    2017-02-01

    We have synthesized and electrochemically tested a carbon sample that was suitable as anode for lithium secondary battery. The synthesis was based on the use of the palygorskite clay as template and sugar cane molasses as carbon source. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Brunauer-Emmett-Teller (BET) measurements and High Resolution Transmission Electron Microscope (HRTEM) analysis showed that the nanometric carbon material has a highly disordered graphene-like wrinkled structure and large specific surface area (467 m2 g-1). The compositional characterization revealed a 14% of heteroatoms-containing groups (O, H, N, S) doping the as-prepared carbon. Thermophysical measurements revealed the good thermal stability and an acceptable thermal diffusivity (9·10-7 m2 s-1) and conductivity (1.1 W m-1 K-1) of this carbon. The electrical properties showed an electronic conductivity of hole-like carriers of approximately one S/cm in a 173-293 K range. The testing of this material as anodes in a secondary lithium battery displayed a high specific capacity and excellent performance in terms of number of cycles. A high reversible capacity of 356 mA h g-1 was reached.

  17. Synthesis and characterization of different MnO2 morphologies for lithium-air batteries

    NASA Astrophysics Data System (ADS)

    Choi, Hyun-A.; Jang, Hyuk; Hwang, Hyein; Choi, Mincheol; Lim, Dongwook; Shim, Sang Eun; Baeck, Sung-Hyeon

    2014-09-01

    Manganese dioxide (MnO2) was synthesized in the forms of nanorods, nanoparticles, and mesoporous structures and the characteristics of these materials were investigated. Crystallinities were studied by x-ray diffraction and morphologies by scanning and transmission electron microscopy. Average pore sizes and specific surface areas were analyzed using the Barret-Joyner-Halenda and Brunauer-Emmett-Teller methods, respectively. Samples were also studied by cyclic voltammetry using 1M aqueous KOH solution saturated with either O2 or N2 as electrolytes to investigate their ORR (oxygen reduction reaction) and OER (oxygen evolution reaction) activities. Of the samples produced, mesoporous MnO2 exhibited the highest ORR and OER catalytic activities. Mesoporous MnO2 supported on a gas diffusion layer was also used as a catalyst on the air electrode (cathode) of a lithium-air battery in organic electrolyte. The charge-discharge behavior of mesoporous MnO2 was investigated at a current density 0.2 mAcm-2 in a pure oxygen environment. Mesoporous MnO2 electrodes showed stable cycleability up to 65 cycles at a cell capacity of 700 mAhg-1.

  18. Chiral monolithic absorbent constructed by optically active helical-substituted polyacetylene and graphene oxide: preparation and chiral absorption capacity.

    PubMed

    Li, Weifei; Wang, Bo; Yang, Wantai; Deng, Jianping

    2015-02-01

    Chiral monolithic absorbent is successfully constructed for the first time by using optically active helical-substituted polyacetylene and graphene oxide (GO). The preparative strategy is facile and straightforward, in which chiral-substituted acetylene monomer (Ma), cross-linker (Mb), and alkynylated GO (Mc) undergo copolymerization to form the desired monolithic absorbent in quantitative yield. The resulting monoliths are characterized by circular dichroism, UV-vis absorption, scanning electron microscopy (SEM), FT-IR, Raman, energy-dispersive spectrometer (EDS), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), XPS, and thermogravimetric analysis (TGA) techniques. The polymer chains derived from Ma form chiral helical structures and thus provide optical activity to the monoliths, while GO sheets contribute to the formation of porous structures. The porous structure enables the monolithic absorbents to demonstrate a large swelling ratio in organic solvents, and more remarkably, the helical polymer chains provide optical activity and further enantio-differentiating absorption ability. The present study establishes an efficient and versatile methodology for preparing novel functional materials, in particular monolithic chiral materials based on substituted polyacetylene and GO. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Effect of cetyl trimethyl ammonium bromide concentration on structure, morphology and carbon dioxide adsorption capacity of calcium hydroxide based sorbents

    NASA Astrophysics Data System (ADS)

    Hlaing, Nwe Ni; Vignesh, K.; Sreekantan, Srimala; Pung, Swee-Yong; Hinode, Hirofumi; Kurniawan, Winarto; Othman, Radzali; Thant, Aye Aye; Mohamed, Abdul Rahman; Salim, Chris

    2016-02-01

    Calcium hydroxide (Ca(OH)2) has been proposed as an important material for industrial, architectural, and environmental applications. In this study, calcium acetate was used as a precursor and cetyl trimethyl ammonium bromide (CTAB) was used as a surfactant to synthesize Ca(OH)2 based adsorbents for carbon dioxide (CO2) capture. The effect of CTAB concentration (0.2-0.8 M) on the structure, morphology and CO2 adsorption performance of Ca(OH)2 was studied in detail. The synthesized samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), BET surfaced area and thermogravimetry-differential thermal analysis (TG-DTA) techniques. The phase purity, crystallite size, Brunauer-Emmett-Teller (BET) surface area and CO2 adsorption performance of Ca(OH)2 precursor adsorbents were significantly increased when the concentration of CTAB was increased. XRD results showed that pure Ca(OH)2 phase was obtained at the CTAB concentration of 0.8 M. TGA results exhibited that 0.8 M of CTAB-assisted Ca(OH)2 precursor adsorbent possessed a residual carbonation conversion of ∼56% after 10 cycles.

  20. Synthesis of graphene aerogel for adsorption of bisphenol A

    NASA Astrophysics Data System (ADS)

    Trinh, Truong Thi Phuong Nguyet Xuan; Long, Nguyen Huynh Bach Son; Quang, Dong Thanh; Hieu, Nguyen Huu

    2018-04-01

    In this research, graphene aerogel (GA) was synthesized by chemical reduction method using ethylene diamine as a reducing agent. The morphology and properties of GA were characterized by calculating apparent density, Fourier transform infrared spectroscopy, X-ray diffraction, Raman spectroscopy, field emission scanning electron microscopy, and Brunauer-Emmett-Teller (BET) specific surface area. High-performance liquid chromatography (HPLC) was used to quantify the amount of the residual bisphenol A (BPA) concentration. The analysis results showed that GA exhibited low density ranging from 4-8 mg/cm3, hydrophobicity, high porosity, and specific surface area of 1883 m2/g according to BET. The obtained GA was used as an adsorbent for BPA. The effects of pH, contact time, and initial BPA concentration on the adsorption were investigated. The adsorption equilibrium time could be reached within 240 minutes. The adsorption data were well-fitted to pseudo-second-order kinetic equation and Langmuir isotherm model. The maximum adsorption capacity of GA for BPA calculated by the Langmuir model was 185.185 mg/g at pH 7. Accordingly, GA could be considered as promising adsorbents for BPA in water.

  1. Application of Box-Behnken design for modeling of lead adsorption onto unmodified and NaCl-modified zeolite NaA obtained from biosilica.

    PubMed

    Terzioğlu, Pinar; Yücel, Sevil; Öztürk, Mehmet

    2017-01-01

    The main objective of the present study was to optimize lead adsorption onto zeolite NaA. For this purpose, to synthesize zeolite NaA under hydrothermal conditions, local wheat husk was precleaned with chemical treatment using hydrochloric acid solution. The unmodified (ZU) and NaCl-modified (ZN) zeolites were characterized by Brunauer-Emmett-Teller, scanning electron microscopy coupled with energy dispersive spectroscopy and X-ray diffraction. The optimization of adsorption process was examined using Box-Behnken Experimental Design in response surface methodology by Design Expert Version 7.0.0 (Stat-Ease, USA). The effects of initial lead (II) concentration, temperature, and time were selected as independent variables. Lack of fit test indicates that the quadratic regression model was significant with the high coefficients of determination values for both adsorbents. Optimum process conditions for lead (II) adsorption onto ZU and ZN were found to be 64.40°C and 64.80°C, respectively, and 90.80 min, and 350 mg L -1 initial lead(II) concentration for both adsorbents. Under these conditions, maximum adsorption capacities of ZU and ZN for lead (II) were 293.38 mg g -1 and 321.85 mg g -1 , respectively.

  2. In-situ Polymerization of Polyaniline/Polypyrrole Copolymer using Different Techniques

    NASA Astrophysics Data System (ADS)

    Hammad, A. S.; Noby, H.; Elkady, M. F.; El-Shazly, A. H.

    2018-01-01

    The morphology and surface area of the poly(aniline-co-pyrrole) copolymer (PANPY) are important properties which improve the efficiency of the copolymer in various applications. In this investigation, different techniques were employed to produce PANPY in different morphologies. Aniline and pyrrole were used as monomers, and ammonium peroxydisulfate (APS) was used as an oxidizer with uniform molar ratio. Rapid mixing, drop-wise mixing, and supercritical carbon dioxide (ScCO2) polymerization techniques were appointed. The chemical structure, crystallinity, porosity, and morphology of the composite were distinguished by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Brunauer, Emmett and Teller (BET) analysis, and transmission electron microscopy (TEM) respectively. The characterization tests indicated that the polyaniline/polypyrrole copolymer was successfully prepared with different morphologies. Based on the obtained TEM, hollow nanospheres were formed using rapid mixing technique with acetic acid that have a diameter of 75 nm and thickness 26 nm approximately. Also, according to the XRD, the produced structures have a semi- crystalline structure. The synthesized copolymer with ScCO2-assisted polymerization technique showed improved surface area (38.1 m2/g) with HCl as dopant.

  3. Highly Sensitive and Selective Hydrogen Gas Sensor Using the Mesoporous SnO₂ Modified Layers.

    PubMed

    Xue, Niuzi; Zhang, Qinyi; Zhang, Shunping; Zong, Pan; Yang, Feng

    2017-10-14

    It is important to improve the sensitivities and selectivities of metal oxide semiconductor (MOS) gas sensors when they are used to monitor the state of hydrogen in aerospace industry and electronic field. In this paper, the ordered mesoporous SnO₂ (m-SnO₂) powders were prepared by sol-gel method, and the morphology and structure were characterized by X-ray diffraction analysis (XRD), transmission electron microscope (TEM) and Brunauer-Emmett-Teller (BET). The gas sensors were fabricated using m-SnO₂ as the modified layers on the surface of commercial SnO₂ (c-SnO₂) by screen printing technology, and tested for gas sensing towards ethanol, benzene and hydrogen with operating temperatures ranging from 200 °C to 400 °C. Higher sensitivity was achieved by using the modified m-SnO₂ layers on the c-SnO₂ gas sensor, and it was found that the S(c/m2) sensor exhibited the highest response (Ra/Rg = 22.2) to 1000 ppm hydrogen at 400 °C. In this paper, the mechanism of the sensitivity and selectivity improvement of the gas sensors is also discussed.

  4. Fabrication and characterization of akaganeite/graphene oxide nanocomposite for arsenic removal from water

    NASA Astrophysics Data System (ADS)

    Trang, Nguyen Thi Thuy; Thy, Lu Thi Mong; Cuong, Pham Mai; Tu, Tran Hoang; Hieu, Nguyen Huu

    2018-04-01

    In this study, akageneite/graphene oxide (β-FeOOH/GO) nanocomposite was fabricated by in situ forced hydrolysis of iron (III) chloride. The structure and morphology of β-FeOOH/GO were characterized by Fourier Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), and Brunauer-Emmett- Teller (BET) specific surface area. XRD, FTIR, and TEM results indicated that β-FeOOH nanoparticles were successfully decorated on the surface of GO nanosheets. The BET specific surface area of β-FeOOH/GO was observed of 97.94 m2/g. The nanocomposite was used as an adsorbent for removal of arsenic (As5+) from water. Adsorption experiments were carried out to investigate contact time, pH values, and As5+ initial concentrations. The adsorption equilibrium time was reached within 180 minutes. The adsorption was well-fitted by a pseudo-second-order kinetic and Langmuir isotherm model. The maximum adsorption capacity of β-FeOOH/GO for As5+ ions of 94.34 mg/g that was calculated from the Langmuir model at pH 3. Accordingly, the nanocomposite β-FeOOH/GO could be considered as a highly efficient adsorbent for removing arsenic from water.

  5. Characterization and activity of visible-light-driven TiO 2 photocatalyst codoped with lanthanum and iodine

    NASA Astrophysics Data System (ADS)

    Li, Ling; Zhuang, Huisheng; Bu, Dan

    2011-08-01

    The novel visible-light-activated La/I/TiO 2 nanocomposition photocatalyst was successfully synthesized using precipitation-dipping method, and characterized by X-ray powder diffraction (XRD), the Brunauer-Emmett-Teller (BET) method, transmission electron microscopy (TEM), thermogravimetry-differential scanning calorimetry (TG-DSC) and UV-vis diffuse reflectance spectroscopy (UV-vis DRS). The photocatalytic activity of La/I/TiO 2 was evaluated by studying photodegradation of reactive blue 19 as a probe reaction under simulated sunlight irradiation. Photocatalytic experiment results showed that the maximum specific photocatalytic activity of the La/I/TiO 2 photocatalyst appeared when the molar ratio of La/Ti was 2.0 at%, calcined at 350 °C for 2 h, due to the sample with good crystallization, high BET surface area and small crystal size. Under simulated sunlight irradiation, the degradation of reactive blue 19 aqueous solution reached 98.6% in 80 min, which showed La/I/TiO 2 photocatalyst to be much higher photocatalytic activity compared to standard Degussa P25 photocatalyst. The higher visible light activity is due to the codoping of lanthanum and iodine.

  6. Li-cycling properties of molten salt method prepared nano/submicrometer and micrometer-sized CuO for lithium batteries.

    PubMed

    Reddy, M V; Yu, Cai; Jiahuan, Fan; Loh, Kian Ping; Chowdari, B V R

    2013-05-22

    We report the synthesis of CuO material by molten salt method at a temperature range, 280 to 950 °C for 3 h in air. This report includes studies on the effect of morphology, crystal structure and electrochemical properties of CuO prepared at different temperatures. Obtained CuO was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) surface area methods. Samples prepared at ≥410 °C showed a single-phase material with a lattice parameter value of a = 4.69 Å, b = 3.43 Å, c = 5.13 Å and surface area values are in the range 1.0-17.0 m(2) g(-1). Electrochemical properties were evaluated via cyclic voltammetry (CV) and galvanostatic cycling studies. CV studies showed a minor difference in the peak potentials depending on preparation temperature and all compounds exhibit a main anodic peak at ~2.45 V and cathodic peaks at ~0.85 V and ~1.25 V vs Li. CuO prepared at 750 °C showed high and stable capacity of ~620 mA h g(-1) at the end of 40th cycle.

  7. High-pressure homogenization associated hydrothermal process of palygorskite for enhanced adsorption of Methylene blue

    NASA Astrophysics Data System (ADS)

    Zhang, Zhifang; Wang, Wenbo; Wang, Aiqin

    2015-02-01

    Palygorskite (PAL) was modified by a high-pressure homogenization assisted hydrothermal process. The effects of modification on the morphology, structure and physicochemical properties of PAL were systematically investigated by Field-emission scanning electron microscopy (FESEM), Transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FTIR), Brunauer-Emmett-Teller (BET) analysis, X-ray diffraction (XRD) and Zeta potential analysis techniques, and the adsorption properties were systematically evaluated using Methylene blue (MB) as the model dye. The results revealed that the crystal bundles were disaggregated and the PAL nanorods became more even after treated via associated high-pressure homogenization and hydrothermal process, and the crystal bundles were dispersed as nanorods. The intrinsic crystal structure of PAL was remained after hydrothermal treatment, and the pore size calculated by the BET method was increased. The adsorption properties of PAL for MB were evidently improved (from 119 mg/g to 171 mg/g) after modification, and the dispersion of PAL before hydrothermal reaction is favorable to the adsorption. The desorption evaluation confirms that the modified PAL has stronger affinity with MB, which is benefit to fabricate a stable organic-inorganic hybrid pigment.

  8. Relation between the conditions of preparation and the polarization characteristics of spongy Raney nickel electrodes used as anodes for fuel cells

    NASA Astrophysics Data System (ADS)

    Tomida, Tahei; Okamura, Kazuhiro; Ashida, Toshifumi; Nakabayashi, Ichiro

    1992-04-01

    Spongy Raney nickel electrodes were prepared from substrates of spongy nickel plate coated with aluminum. Influences of the temperature for alloying and the weight ratio of aluminum to nickel (Al/Ni) in the substrate on polarization characteristics were studied in connection with the alloy compositions formed, and the surface microstructure of the catalysts. For this, the ratio Al/Ni in the substrate was varied ranging from 0.1 to 2.5. Electrode performance was improved, with increases in both the temperature for alloying and the Al/Ni ratio of the substrates. However, the higher the temperature used for alloying, the lower were the effects of the Al/Ni ratio. The activated Raney nickel was prepared from an alloy whose components were NiAl3 and/or Ni2Al3. It was also shown that a good polarization performance resulted from the increase in activated nickel grains, which were observed by scanning electron microscopy, and an increase in the Brunauer, Emmett, and Teller (BET) surface area of the electrode-catalyst. The broad peaks observed in X-ray diffraction of Raney nickel catalysts implied crystal distortions, which should be closely related to an increase in the BET surface area.

  9. Ultrasonic degradation of aqueous phenolsulfonphthalein (PSP) in the presence of nano-Fe/H2O2.

    PubMed

    Ayanda, Olushola S; Nelana, Simphiwe M; Naidoo, Eliazer B

    2018-10-01

    In this study, nano iron (nano-Fe) was successfully synthesized by sodium borohydride reduction of ferric chloride solution to enhance the ultrasonic degradation of phenolsulfonphthalein (PSP). The nano-Fe was characterized by scanning electron microscopy - energy dispersive spectroscopy (SEM-EDX), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), attenuated total reflection - Fourier transform infrared spectroscopy (ATR-FTIR), and Brunauer, Emmett and Teller (BET) surface area determination. Experimental results demonstrated that a combined ultrasonic/nano-Fe/H 2 O 2 system was more effective for PSP removal in combination than they were individually and there was a significant difference between the combined and single processes. The ultrasonic/nano-Fe/H 2 O 2 degradation follows the Langmuir-Hinshelwood (L-H) kinetic model. The addition of nano-Fe and H 2 O 2 to the ultrasonic reactor greatly accelerated the degradation of PSP (25 mg/L) from 12.5% up to 96.5%. These findings indicated that ultrasonic degradation in the presence of nano-Fe and H 2 O 2 is a promising and efficient technique for the elimination of emerging micropollutants from aqueous solution. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Spectrophotometric determination of basic fuchsin from various water samples after vortex assisted solid phase extraction using reduced graphene oxide as an adsorbent.

    PubMed

    Tokalıoğlu, Şerife; Yavuz, Emre; Aslantaş, Ayşe; Şahan, Halil; Taşkın, Ferhat; Patat, Şaban

    2015-01-01

    In this study, a fast and simple vortex assisted solid phase extraction method was developed for the separation/preconcentration of basic fuchsin in various water samples. The determination of basic fuchsin was carried out at a wavelength of 554 nm by spectrophotometry. Reduced graphene oxide which was used as a solid phase extractor was synthesized and characterized by X-ray diffraction, scanning electron microscopy and the Brunauer, Emmett and Teller. The optimum conditions are as follows: pH 2, contact times for adsorption and elution of 30 s and 90 s, respectively, 10 mg adsorbent, and eluent (ethanol) volume of 1 mL. The effects of some interfering ions and dyes were investigated. The method was linear in the concentration range of 50-250 μg L(-1). The adsorption capacity was 34.1 mg g(-1). The preconcentration factor, limit of detection and precision (RSD, %) of the method were found to be 400, 0.07 μg L(-1) and 1.2%, respectively. The described method was validated by analyzing basic fuchsin spiked certified reference material (SPS-WW1 Batch 114-Wastewater) and spiked real water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Liquefied petroleum gas sensor based on manganese (III) oxide and zinc manganese (III) oxide nanoparticles

    NASA Astrophysics Data System (ADS)

    Sharma, Shiva; Chauhan, Pratima; Husain, Shahid

    2018-01-01

    In this paper, {{{Mn}}}2{{{O}}}3 and {{{ZnMn}}}2{{{O}}}4 nanoparticles (NPs) are successfully synthesized using chemical co-precipitation method at room temperature and further annealed at 450 °C. The structure, crystallite size, morphology, specific surface area (SSA) and band gap energy have been determined by x-ray diffraction, transmission electron microscopy, Brunauer-Emmett-Teller surface area analysis, scanning electron microscopy (SEM-EDS) and UV-visible spectrophotometer. The sensor films of the {{{Mn}}}2{{{O}}}3 NPs and {{{ZnMn}}}2{{{O}}}4 NPs have been fabricated onto glass substrate using spin coater system separately. These sensor films are investigated for different concentrations (200-1200 ppm) of liquefied petroleum gas (LPG) at different operating temperatures ranging from 100 °C to 400 °C. A comparative study of gas sensing properties shows that spinel {{{ZnMn}}}2{{{O}}}4 sensor film exhibit excellent response (≈ 80 % ) towards 1000 ppm LPG at 300 °C in comparison to {{{Mn}}}2{{{O}}}3 sensor films. The enhancement in the gas sensing characteristics of {{{ZnMn}}}2{{{O}}}4 sensor film is attributed to the reduced crystallite size, greater SSA, and modification in structure as well as morphology.

  12. Template-free fabrication of hierarchical In2O3 hollow microspheres with superior HCHO-sensing properties

    NASA Astrophysics Data System (ADS)

    Zhang, Su; Song, Peng; Tian, Zhebin; Wang, Qi

    2018-05-01

    Hierarchical In2O3 hollow microspheres were successfully prepared via a facile and low-cost hydrothermal method. Their morphology and structure were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and the Brunauer-Emmett-Teller (BET) approach. The SEM and TEM results revealed that the as-obtained hollow In2O3 microspheres is composed of In2O3 nanospheres with 200-400 nm in diameter, and the size of In2O3 microspheres is about 2-4 μm. The specific surface area of the as-prepared In2O3 is about 40.94 m2/g. The sensor based on hierarchical In2O3 hollow microspheres displays excellent sensing properties to 10 ppm HCHO, and the optimum operating temperature is relatively low (200 °C). The response value of the as-fabricated sensor to 10 ppm HCHO is about 20. Due to the sensor based on hierarchical In2O3 hollow microspheres has many advantages, such as facile preparation and excellent gas-sensing properties, it has a wide range of prospects in practical applications.

  13. One Step Assembly of Thin Films of Carbon Nanotubes on Screen Printed Interface for Electrochemical Aptasensing of Breast Cancer Biomarker.

    PubMed

    Nawaz, Muhammad Azhar Hayat; Rauf, Sajid; Catanante, Gaelle; Nawaz, Mian Hasnain; Nunes, Gilvanda; Marty, Jean Louis; Hayat, Akhtar

    2016-10-06

    Thin films of organic moiety functionalized carbon nanotubes (CNTs) from a very well-dispersed aqueous solution were designed on a screen printed transducer surface through a single step directed assembly methodology. Very high density of CNTs was obtained on the screen printed electrode surface, with the formation of a thin and uniform layer on transducer substrate. Functionalized CNTs were characterized by X-ray diffraction spectroscopy (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and Brunauer-Emmett- Teller (BET) surface area analyzer methodologies, while CNT coated screen printed transducer platform was analyzed by scanning electron microscopy (SEM), atomic force microscopy (AFM), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The proposed methodology makes use of a minimum amount of CNTs and toxic solvents, and is successfully demonstrated to form thin films over macroscopic areas of screen printed carbon transducer surface. The CNT coated screen printed transducer surface was integrated in the fabrication of electrochemical aptasensors for breast cancer biomarker analysis. This CNT coated platform can be applied to immobilize enzymes, antibodies and DNA in the construction of biosensor for a broad spectrum of applications.

  14. Sono-assisted adsorption of a textile dye on milk vetch-derived charcoal supported by silica nanopowder.

    PubMed

    Jorfi, Sahand; Darvishi Cheshmeh Soltani, Reza; Ahmadi, Mehdi; Khataee, Alireza; Safari, Mahdi

    2017-02-01

    This study was performed to assess the efficiency of silica nanopowder (SNP)/milk vetch-derived charcoal (MVDC) nanocomposite coupled with the ultrasonic irradiation named sono-adsorption process for treating water-contained Basic Red 46 (BR46) dye. Field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) and Fourier transform infrared spectroscopy (FT-IR) were performed for the characterization of as-prepared adsorbent. The sono-assisted adsorption process was optimized using response surface optimization on the basis of central composite design by the application of quadratic model. Accordingly, the color removal can be retained more than 93% by an initial BR46 concentration of 8 mg/L, sonication time of 31 min, adsorbent dosage of 1.2 g/L and initial pH of 9. The pseudo-second order kinetic model described the sono-assisted adsorption of BR46 reasonably well (R 2  > 0.99). The intra-particular diffusion kinetic model pointed out that the sono-assisted adsorption of BR46 onto SNP/MVDC nanocomposite was diffusion controlled as well as that ultrasonication enhanced the diffusion rate. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. Fabrication of hierarchical flower-like porous ZnO nanostructures from layered ZnC2O4·3Zn(OH)2 and gas sensing properties

    NASA Astrophysics Data System (ADS)

    Cui, Jiashan; Sun, Jianbo; Liu, Xin; Li, Jinwei; Ma, Xinzhi; Chen, Tingting

    2014-07-01

    ZnO materials with porous and hierarchical flower-like structure were synthesized through mild hydrothermal and simple calcination approach, in which the flower-like layered zinc oxalate hydroxide (ZnC2O4·3Zn(OH)2) precursor was first synthesized and then calcined at 600 °C. The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopic (TEM), Brunauer-Emmett-Teller (BET) and thermogravimetric (TG) analysis. We proposed the possible growth mechanism of the material via studying the time evolution experiment results. In the process of reaction, oxalic acid as a structure-directing agent hydrolyzed and then formed primarily sheets-like intermediate ZnC2O4·2H2O. Hexamethylenetetramine (HMT) as surfactant, with directional adsorption, leads to the formation of layered zinc oxalate hydroxide precursor. Furthermore, the gas sensitivity also can be characterized, whose results indicated that the synthesized materials had a preferable selectivity to ethanol gas. The fast response rate and reversible performance can be attributed to the produced greater specific surface area produced, which was caused by the porous and hierarchical flower-like structure.

  16. TiO2-graphene oxide nanocomposite as advanced photocatalytic materials.

    PubMed

    Stengl, Václav; Bakardjieva, Snejana; Grygar, Tomáš Matys; Bludská, Jana; Kormunda, Martin

    2013-02-27

    Graphene oxide composites with photocatalysts may exhibit better properties than pure photocatalysts via improvement of their textural and electronic properties. TiO2-Graphene Oxide (TiO2 - GO) nanocomposite was prepared by thermal hydrolysis of suspension with graphene oxide (GO) nanosheets and titania peroxo-complex. The characterization of graphene oxide nanosheets was provided by using an atomic force microscope and Raman spectroscopy. The prepared nanocomposites samples were characterized by Brunauer-Emmett-Teller surface area and Barrett-Joiner-Halenda porosity, X-ray Diffraction, Infrared Spectroscopy, Raman Spectroscopy and Transmission Electron Microscopy. UV/VIS diffuse reflectance spectroscopy was employed to estimate band-gap energies. From the TiO2 - GO samples, a 300 μm thin layer on a piece of glass 10×15 cm was created. The photocatalytic activity of the prepared layers was assessed from the kinetics of the photocatalytic degradation of butane in the gas phase. The best photocatalytic activity under UV was observed for sample denoted TiGO_100 (k = 0.03012 h-1), while sample labeled TiGO_075 (k = 0.00774 h-1) demonstrated the best activity under visible light.

  17. Zn₂SnO₄-Reduced Graphene Oxide Nanohybrids for Visible-Light-Driven Photocatalysis.

    PubMed

    Li, Hui; Wu, Xiang-Feng; Sun, Yang; Zhao, Ze-Hua; Zhang, Chen-Xu; Jia, Fan-Fan; Zhang, Han; Yu, Mai-Tuo; Yang, Xin-Yue

    2018-02-01

    Zn2SnO4-reduced graphene oxide photocatalysts were synthesized by using SnCl4 5H2O, Zn(NO3)2 · 6H2O and graphene oxide via hydrothermal process. The structure, morphology, specific surface area and photo response of the as-prepared nanocomposites were characterized by X-ray diffraction, Transmission electron microscopy, UV-vis diffuse reflectance spectra, Brunauer-emmett-teller surface area measurement and Photoluminescence emission spectra. Experimental results showed that the Zn2SnO4 nanoparticles, with 20-30 nm a size range, were uniformly dispersed on the surfaces of reduced graphene oxide. Moreover, the as-prepared Zn2SnO4-reduced graphene oxide photocatalysts exhibited enhanced photocatalytic activities for degradation of Rhodamine B compared to those of pure Zn2SnO4. When the amount of reduced graphene oxide was 4 wt%, it showed the highest photocatalytic efficiency of 99.7% for 240 min, and the photocatalytic efficiency was still 98.5% after it was recycled 4 times. It also possessed the band gap of 2.48 eV and specific surface area of 58.1 m2 g-1.

  18. [Study on bamboo treated with gamma rays by X-ray diffraction].

    PubMed

    Sun, Feng-Bo; Fei, Ben-Hua; Jiang, Ze-Hui; Yu, Zi-Xuan; Tian, Gen-Lin; Yang, Quan-Wen

    2011-06-01

    The microfibril angle and crystallinity of bamboo treated with gamma rays were tested by X-ray diffraction (XRD). The result indicated that crystallinity in bamboo increased when irradiation dose was less than 100 kGy, while the irradiation dose was raised to about 100 kGy, crystallinity in bamboo reduced. But during the whole irradiation process, the influence on microfibril angle was not obvious, so it was not the dominant factors on variation in physical-mechanical properties of bamboo during the process of irradiation.

  19. Observation of sagittal X-ray diffraction by surface acoustic waves in Bragg geometry.

    PubMed

    Vadilonga, Simone; Zizak, Ivo; Roshchupkin, Dmitry; Evgenii, Emelin; Petsiuk, Andrei; Leitenberger, Wolfram; Erko, Alexei

    2017-04-01

    X-ray Bragg diffraction in sagittal geometry on a Y-cut langasite crystal (La 3 Ga 5 SiO 14 ) modulated by Λ = 3 µm Rayleigh surface acoustic waves was studied at the BESSY II synchrotron radiation facility. Owing to the crystal lattice modulation by the surface acoustic wave diffraction, satellites appear. Their intensity and angular separation depend on the amplitude and wavelength of the ultrasonic superlattice. Experimental results are compared with the corresponding theoretical model that exploits the kinematical diffraction theory. This experiment shows that the propagation of the surface acoustic waves creates a dynamical diffraction grating on the crystal surface, and this can be used for space-time modulation of an X-ray beam.

  20. Coded diffraction system in X-ray crystallography using a boolean phase coded aperture approximation

    NASA Astrophysics Data System (ADS)

    Pinilla, Samuel; Poveda, Juan; Arguello, Henry

    2018-03-01

    Phase retrieval is a problem present in many applications such as optics, astronomical imaging, computational biology and X-ray crystallography. Recent work has shown that the phase can be better recovered when the acquisition architecture includes a coded aperture, which modulates the signal before diffraction, such that the underlying signal is recovered from coded diffraction patterns. Moreover, this type of modulation effect, before the diffraction operation, can be obtained using a phase coded aperture, just after the sample under study. However, a practical implementation of a phase coded aperture in an X-ray application is not feasible, because it is computationally modeled as a matrix with complex entries which requires changing the phase of the diffracted beams. In fact, changing the phase implies finding a material that allows to deviate the direction of an X-ray beam, which can considerably increase the implementation costs. Hence, this paper describes a low cost coded X-ray diffraction system based on block-unblock coded apertures that enables phase reconstruction. The proposed system approximates the phase coded aperture with a block-unblock coded aperture by using the detour-phase method. Moreover, the SAXS/WAXS X-ray crystallography software was used to simulate the diffraction patterns of a real crystal structure called Rhombic Dodecahedron. Additionally, several simulations were carried out to analyze the performance of block-unblock approximations in recovering the phase, using the simulated diffraction patterns. Furthermore, the quality of the reconstructions was measured in terms of the Peak Signal to Noise Ratio (PSNR). Results show that the performance of the block-unblock phase coded apertures approximation decreases at most 12.5% compared with the phase coded apertures. Moreover, the quality of the reconstructions using the boolean approximations is up to 2.5 dB of PSNR less with respect to the phase coded aperture reconstructions.

  1. Ultrahigh vacuum/high pressure chamber for surface x-ray diffraction experiments

    NASA Astrophysics Data System (ADS)

    Bernard, P.; Peters, K.; Alvarez, J.; Ferrer, S.

    1999-02-01

    We describe an ultrahigh vacuum chamber that can be internally pressurized to several bars and that is designed to perform surface x-ray diffraction experiments on solid-gas interfaces. The chamber has a cylindrical beryllium window that serves as the entrance and exit for the x rays. The sample surface can be ion bombarded with an ancillary ion gun and annealed to 1200 K.

  2. Borman effect in resonant diffraction of X-rays

    NASA Astrophysics Data System (ADS)

    Oreshko, A. P.

    2013-08-01

    A dynamic theory of resonant diffraction (occurring when the energy of incident radiation is close to the energy of the absorption edge of an element in the composition of a given substance) of synchronous X-rays is developed in the two-wave approximation in the coplanar Laue geometry for large grazing angles in perfect crystals. A sharp decrease in the absorption coefficient in the substance with simultaneously satisfied diffraction conditions (Borman effect) is demonstrated, and the theoretical and first experimental results are compared. The calculations reveal the possibility of applying this approach in analyzing the quadrupole-quadrupole contribution to the absorption coefficient.

  3. KOTOBUKI-1 apparatus for cryogenic coherent X-ray diffraction imaging.

    PubMed

    Nakasako, Masayoshi; Takayama, Yuki; Oroguchi, Tomotaka; Sekiguchi, Yuki; Kobayashi, Amane; Shirahama, Keiya; Yamamoto, Masaki; Hikima, Takaaki; Yonekura, Koji; Maki-Yonekura, Saori; Kohmura, Yoshiki; Inubushi, Yuichi; Takahashi, Yukio; Suzuki, Akihiro; Matsunaga, Sachihiro; Inui, Yayoi; Tono, Kensuke; Kameshima, Takashi; Joti, Yasumasa; Hoshi, Takahiko

    2013-09-01

    We have developed an experimental apparatus named KOTOBUKI-1 for use in coherent X-ray diffraction imaging experiments of frozen-hydrated non-crystalline particles at cryogenic temperature. For cryogenic specimen stage with small positional fluctuation for a long exposure time of more than several minutes, we here use a cryogenic pot cooled by the evaporation cooling effect for liquid nitrogen. In addition, a loading device is developed to bring specimens stored in liquid nitrogen to the specimen stage in vacuum. The apparatus allows diffraction data collection for frozen-hydrated specimens at 66 K with a positional fluctuation of less than 0.4 μm and provides an experimental environment to easily exchange specimens from liquid nitrogen storage to the specimen stage. The apparatus was developed and utilized in diffraction data collection of non-crystalline particles with dimensions of μm from material and biological sciences, such as metal colloid particles and chloroplast, at BL29XU of SPring-8. Recently, it has been applied for single-shot diffraction data collection of non-crystalline particles with dimensions of sub-μm using X-ray free electron laser at BL3 of SACLA.

  4. Diamond-anvil cell for radial x-ray diffraction.

    PubMed

    Chesnut, G N; Schiferl, D; Streetman, B D; Anderson, W W

    2006-06-28

    We have designed a new diamond-anvil cell capable of radial x-ray diffraction to pressures of a few hundred GPa. The diffraction geometry allows access to multiple angles of Ψ, which is the angle between each reciprocal lattice vector g(hkl) and the compression axis of the cell. At the 'magic angle', Ψ≈54.7°, the effects of deviatoric stresses on the interplanar spacings, d(hkl), are significantly reduced. Because the systematic errors, which are different for each d(hkl), are significantly reduced, the crystal structures and the derived equations of state can be determined reliably. At other values of Ψ, the effects of deviatoric stresses on the diffraction pattern could eventually be used to determine elastic constants.

  5. 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.

  6. The Use of Spray-Dried Mn₃O₄/C Composites as Electrocatalysts for Li-O₂ Batteries.

    PubMed

    Yang, Hong-Kai; Chin, Chih-Chun; Chen, Jenn-Shing

    2016-11-07

    The electrocatalytic activities of Mn₃O₄/C composites are studied in lithium-oxygen (Li-O₂) batteries as cathode catalysts. The Mn₃O₄/C composites are fabricated using ultrasonic spray pyrolysis (USP) with organic surfactants as the carbon sources. The physical and electrochemical performance of the composites is characterized by X-ray diffraction, scanning electron microscopy, particle size analysis, Brunauer-Emmett-Teller (BET) measurements, elemental analysis, galvanostatic charge-discharge methods and rotating ring-disk electrode (RRDE) measurements. The electrochemical tests demonstrate that the Mn₃O₄/C composite that is prepared using Trition X-114 (TX114) surfactant has higher activity as a bi-functional catalyst and delivers better oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) catalytic performance in Li-O₂ batteries because there is a larger surface area and particles are homogeneous with a meso/macro porous structure. The rate constant ( k f ) for the production of superoxide radical (O₂ • - ) and the propylene carbonate (PC)-electrolyte decomposition rate constant ( k ) for M₃O₄/C and Super P electrodes are measured using RRDE experiments and analysis in the 0.1 M tetrabutylammonium hexafluorophosphate (TBAPF₆)/PC electrolyte. The results show that TX114 has higher electrocatalytic activity for the first step of ORR to generate O₂ • - and produces a faster PC-electrolyte decomposition rate.

  7. 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.

  8. New software to model energy dispersive X-ray diffraction in polycrystalline materials

    NASA Astrophysics Data System (ADS)

    Ghammraoui, B.; Tabary, J.; Pouget, S.; Paulus, C.; Moulin, V.; Verger, L.; Duvauchelle, Ph.

    2012-02-01

    Detection of illicit materials, such as explosives or drugs, within mixed samples is a major issue, both for general security and as part of forensic analyses. In this paper, we describe a new code simulating energy dispersive X-ray diffraction patterns in polycrystalline materials. This program, SinFullscat, models diffraction of any object in any diffractometer system taking all physical phenomena, including amorphous background, into account. Many system parameters can be tuned: geometry, collimators (slit and cylindrical), sample properties, X-ray source and detector energy resolution. Good agreement between simulations and experimental data was obtained. Simulations using explosive materials indicated that parameters such as the diffraction angle or the energy resolution of the detector have a significant impact on the diffraction signature of the material inspected. This software will be a convenient tool to test many diffractometer configurations, providing information on the one that best restores the spectral diffraction signature of the materials of interest.

  9. 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).

  10. Method for improve x-ray diffraction determinations of residual stress in nickel-base alloys

    DOEpatents

    Berman, Robert M.; Cohen, Isadore

    1990-01-01

    A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys which comprises covering part of a predetermined area of the surface of a nickel-base alloy with a dispersion, exposing the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample.

  11. 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

  12. Structural studies of homoisoflavonoids: NMR spectroscopy, X-ray diffraction, and theoretical calculations

    NASA Astrophysics Data System (ADS)

    Sievänen, Elina; Toušek, Jaromír; Lunerová, Kamila; Marek, Jaromír; Jankovská, Dagmar; Dvorská, Margita; Marek, Radek

    2010-08-01

    In this article we present a detailed structural investigation for five homoisoflavonoids, molecules important from the pharmacological point of view. For studying the electron distribution as well as its influence on the physicochemical properties, NMR spectroscopy, X-ray diffraction, and theoretical calculations have been used. Nuclear magnetic shieldings obtained by using DFT calculations for optimized molecular geometries are correlated with the experimentally determined chemical shifts. The theoretical data are well in agreement with the experimental values. The single crystal X-ray structures of homoisoflavonoid derivatives 1, 3, and 4 have been solved. The molecular geometries and crystal packing determined by X-ray diffraction are used for characterizing the intermolecular interactions. Electron distribution is crucial for the stability of radicals and hence the antioxidant efficiency of flavonoid structures. The hydrogen bonding governs the formation of complexes of homoisoflavonoids with biological targets.

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

    DOE PAGES

    Huang, Xiaojing; Miao, Huijie; Steinbrener, Jan; ...

    2009-01-01

    Using a signal-to-noise ratio estimation based on correlations between multiple simulated images, we compare the dose efficiency of two soft x-ray imaging systems: incoherent brightfield imaging using zone plate optics in a transmission x-ray microscope (TXM), and x-ray diffraction microscopy (XDM) where an image is reconstructed from the far-field coherent diffraction pattern. In XDM one must computationally phase weak diffraction signals; in TXM one suffers signal losses due to the finite numerical aperture and efficiency of the optics. In simulations with objects representing isolated cells such as yeast, we find that XDM has the potential for delivering equivalent resolution imagesmore » using fewer photons. As a result, this can be an important advantage for studying radiation-sensitive biological and soft matter specimens.« less

  14. 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.

  15. Rosalind Franklin's X-ray photo of DNA as an undergraduate optical diffraction experiment

    NASA Astrophysics Data System (ADS)

    Thompson, J.; Braun, G.; Tierney, D.; Wessels, L.; Schmitzer, H.; Rossa, B.; Wagner, H. P.; Dultz, W.

    2018-02-01

    Rosalind Franklin's X-ray diffraction patterns of DNA molecules rendered the important clue that DNA has the structure of a double helix. The most famous X-ray photograph, Photo 51, is still printed in most Biology textbooks. We suggest two optical experiments for undergraduates that make this historic achievement comprehensible for students by using macromodels of DNA and visible light to recreate a diffraction pattern similar to Photo 51. In these macromodels, we replace the double helix both mathematically and experimentally with its two-dimensional (flat) projection and explain why this is permissible. Basic optical concepts are used to infer certain well-known characteristics of DNA from the diffraction pattern.

  16. 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.

  17. 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.

  18. Peculiarities of section topograms for the multiple diffraction of X rays

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

    Kohn, V. G., E-mail: kohnvict@yandex.ru; Smirnova, I. A.

    The distortion of interference fringes on the section topograms of single crystal due to the multiple diffraction of X rays has been investigated. The cases of the 220 and 400 reflections in a silicon crystal in the form of a plate with a surface oriented normally to the [001] direction are considered both theoretically and experimentally. The same section topogram exhibits five cases of multiple diffraction at small azimuthal angles for the 400 reflection and MoK{sub α} radiation, while the topogram for the 220 reflection demonstrates two cases of multiple diffraction. All these cases correspond to different combinations of reciprocalmore » lattice vectors. Exact theoretical calculations of section topograms for the aforementioned cases of multiple diffraction have been performed for the first time. The section topograms exhibit two different distortion regions. The distortions in the central region of the structure are fairly complex and depend strongly on the azimuthal angle. In the tails of the multiple diffraction region, there is a shift of two-beam interference fringes, which can be observed even with a laboratory X-ray source.« less

  19. Serial femtosecond X-ray diffraction of enveloped virus microcrystals

    DOE PAGES

    Lawrence, Robert M.; Conrad, Chelsie E.; Zatsepin, Nadia A.; ...

    2015-08-20

    Serial femtosecond crystallography (SFX) using X-ray free-electron lasers has produced high-resolution, room temperature, time-resolved protein structures. We report preliminary SFX of Sindbis virus, an enveloped icosahedral RNA virus with ~700 Å diameter. Microcrystals delivered in viscous agarose medium diffracted to ~40 Å resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is a pertinent step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

  20. Diffraction effects on angular response of X-ray collimators

    NASA Technical Reports Server (NTRS)

    Blake, R. L.; Barrus, D. M.; Fenimore, E.

    1976-01-01

    Angular responses have been measured for X-ray collimators with half-widths ranging from minutes of arc down to 10 arcsec. In the seconds-of-arc range, diffraction peaks at off-axis angles can masquerade as side lobes of the collimator angular response. Measurements and qualitative physical arguments lead to a rule of thumb for collimator design; namely, the angle of first minimum in the Fraunhofer single-slit diffraction pattern should be less than one-fourth of the collimator geometrical full-width at half-maximum intensity.

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

    DOE PAGES

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

    2016-08-09

    In this paper, we present a novel methodology based on machine learning to extract lattice variations in crystalline materials, at the nanoscale, from an x-ray Bragg diffraction-based imaging technique. By employing a full-field microscopy setup, we capture real space images of materials, with imaging contrast determined solely by the x-ray diffracted signal. The data sets that emanate from this imaging technique are a hybrid of real space information (image spatial support) and reciprocal lattice space information (image contrast), and are intrinsically multidimensional (5D). By a judicious application of established unsupervised machine learning techniques and multivariate analysis to this multidimensional datamore » cube, we show how to extract features that can be ascribed physical interpretations in terms of common structural distortions, such as lattice tilts and dislocation arrays. Finally, we demonstrate this 'big data' approach to x-ray diffraction microscopy by identifying structural defects present in an epitaxial ferroelectric thin-film of lead zirconate titanate.« less

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

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

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

    In this paper, we present a novel methodology based on machine learning to extract lattice variations in crystalline materials, at the nanoscale, from an x-ray Bragg diffraction-based imaging technique. By employing a full-field microscopy setup, we capture real space images of materials, with imaging contrast determined solely by the x-ray diffracted signal. The data sets that emanate from this imaging technique are a hybrid of real space information (image spatial support) and reciprocal lattice space information (image contrast), and are intrinsically multidimensional (5D). By a judicious application of established unsupervised machine learning techniques and multivariate analysis to this multidimensional datamore » cube, we show how to extract features that can be ascribed physical interpretations in terms of common structural distortions, such as lattice tilts and dislocation arrays. Finally, we demonstrate this 'big data' approach to x-ray diffraction microscopy by identifying structural defects present in an epitaxial ferroelectric thin-film of lead zirconate titanate.« less

  3. Conceptual Design for Time-Resolved X-ray Diffraction in a Single Laser-Driven Compression Experiment

    NASA Astrophysics Data System (ADS)

    Benedetti, Laura Robin; Eggert, J. H.; Kilkenny, J. D.; Bradley, D. K.; Bell, P. M.; Palmer, N. E.; Rygg, J. R.; Boehly, T. R.; Collins, G. W.; Sorce, C.

    2017-06-01

    Since X-ray diffraction is the most definitive method for identifying crystalline phases of a material, it is an important technique for probing high-energy-density materials during laser-driven compression experiments. We are developing a design for collecting several x-ray diffraction datasets during a single laser-driven experiment, with a goal of achieving temporal resolution better than 1ns. The design combines x-ray streak cameras, for a continuous temporal record of diffraction, with fast x-ray imagers, to collect several diffraction patterns with sufficient solid angle range and resolution to identify crystalline texture. Preliminary experiments will be conducted at the Omega laser and then implemented at the National Ignition Facility. We will describe the status of the conceptual design, highlighting tradeoffs in the design process. We will also discuss the technical issues that must be addressed in order to develop a successful experimental platform. These include: Facility-specific geometric constraints such as unconverted laser light and target alignment; EMP issues when electronic diagnostics are close to the target; X-ray source requirements; and detector capabilities. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344, LLNL-ABS-725146.

  4. Synthesis of TiO2-loaded Co0.85Se thin films with heterostructure and their enhanced catalytic activity for p-nitrophenol reduction and hydrazine hydrate decomposition

    NASA Astrophysics Data System (ADS)

    Zuo, Yong; Song, Ji-Ming; Niu, He-Lin; Mao, Chang-Jie; Zhang, Sheng-Yi; Shen, Yu-Hua

    2016-04-01

    P-nitrophenol (4-NP) and hydrazine hydrate are considered to be highly toxic pollutants in wastewater, and it is of great importance to remove them. Herein, TiO2-loaded Co0.85Se thin films with heterostructure were successfully synthesized by a hydrothermal route. The as-synthesized samples were characterized by x-ray diffraction, x-ray photoelectron spectroscopy, transmission electron microscopy and selective-area electron diffraction. The results demonstrate that TiO2 nanoparticles with a size of about 10 nm are easily loaded on the surface of graphene-like Co0.85Se nanofilms, and the NH3 · H2O plays an important role in the generation and crystallization of TiO2 nanoparticles. Brunauer-Emmett-Teller measurement shows that the obtained nanocomposites have a larger specific surface area (199.3 m2 g-1) than that of Co0.85Se nanofilms (55.17 m2 g-1) and TiO2 nanoparticles (19.49 m2 g-1). The catalytic tests indicate Co0.85Se-TiO2 nanofilms have the highest activity for 4-NP reduction and hydrazine hydrate decomposition within 10 min and 8 min, respectively, compared with the corresponding precursor Co0.85Se nanofilms and TiO2 nanoparticles. The enhanced catalytic performance can be attributed to the larger specific surface area and higher rate of interfacial charge transfer in the heterojunction than that of the single components. In addition, recycling tests show that the as-synthesized sample presents stable conversion efficiency for 4-NP reduction.

  5. Synthesis of TiO₂-loaded Co0.85Se thin films with heterostructure and their enhanced catalytic activity for p-nitrophenol reduction and hydrazine hydrate decomposition.

    PubMed

    Zuo, Yong; Song, Ji-Ming; Niu, He-Lin; Mao, Chang-Jie; Zhang, Sheng-Yi; Shen, Yu-Hua

    2016-04-08

    P-nitrophenol (4-NP) and hydrazine hydrate are considered to be highly toxic pollutants in wastewater, and it is of great importance to remove them. Herein, TiO2-loaded Co0.85Se thin films with heterostructure were successfully synthesized by a hydrothermal route. The as-synthesized samples were characterized by x-ray diffraction, x-ray photoelectron spectroscopy, transmission electron microscopy and selective-area electron diffraction. The results demonstrate that TiO2 nanoparticles with a size of about 10 nm are easily loaded on the surface of graphene-like Co0.85Se nanofilms, and the NH3 · H2O plays an important role in the generation and crystallization of TiO2 nanoparticles. Brunauer-Emmett-Teller measurement shows that the obtained nanocomposites have a larger specific surface area (199.3 m(2) g(-1)) than that of Co0.85Se nanofilms (55.17 m(2) g(-1)) and TiO2 nanoparticles (19.49 m(2) g(-1)). The catalytic tests indicate Co0.85Se-TiO2 nanofilms have the highest activity for 4-NP reduction and hydrazine hydrate decomposition within 10 min and 8 min, respectively, compared with the corresponding precursor Co0.85Se nanofilms and TiO2 nanoparticles. The enhanced catalytic performance can be attributed to the larger specific surface area and higher rate of interfacial charge transfer in the heterojunction than that of the single components. In addition, recycling tests show that the as-synthesized sample presents stable conversion efficiency for 4-NP reduction.

  6. Absolute x-ray energy calibration and monitoring using a diffraction-based method

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

    Hong, Xinguo, E-mail: xhong@bnl.gov; Weidner, Donald J.; Duffy, Thomas S.

    2016-07-27

    In this paper, we report some recent developments of the diffraction-based absolute X-ray energy calibration method. In this calibration method, high spatial resolution of the measured detector offset is essential. To this end, a remotely controlled long-translation motorized stage was employed instead of the less convenient gauge blocks. It is found that the precision of absolute X-ray energy calibration (ΔE/E) is readily achieved down to the level of 10{sup −4} for high-energy monochromatic X-rays (e.g. 80 keV). Examples of applications to pair distribution function (PDF) measurements and energy monitoring for high-energy X-rays are presented.

  7. Surface modified mesostructured iron oxyhydroxide: synthesis, ecotoxicity, and application.

    PubMed

    Choi, Jae-Woo; Mahendran, Basuvaraj; Chung, Seung-Gun; Kim, Song-Bae; Lee, Sang-Hyup

    2014-12-01

    Mesoporous iron oxide, particularly amine-functionalized FeO(x) and FeO(x), was investigated for the removal of toxic heavy metal anions of arsenic and chromium from an aqueous solution. As a control experiment for these toxic compounds, adsorption tests were also performed on Fe3O4 as their counterpart bulk chemical. The mesostructures were confirmed by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) and transmission electron microscopy (TEM). In addition, we prepared stock suspensions of meso-FeO(x), amine-functionalized meso-FeO(x) and Fe3O4 particles, and compared their acute toxicity against Daphnia magna. The 24 h-EC50 values of the amine-functionalized meso-FeO(x), meso-FeO(x) and Fe particle suspensions used in this study were 1682, 2549 and 95 mg/L, respectively. Organism toxicity caused by spills of adsorbents can be negated when the amine-functionalized meso-FeO(x), up to 1500 mg/L, is used as the adsorbent for heavy metal treatment. The adsorption of arsenic and chromium by the three adsorbents were examined, and different adsorption models were used to describe the equilibrium and kinetic data. The amine-functionalized meso-FeO(x) adsorbent was found to give the maximum adsorption capacities for arsenic and chromium (33.51 and 25.05 mg/g, respectively). This research gives promising results for the application of modified meso-FeO(x) as an adsorbent of toxic heavy metal anions from aqueous solutions.

  8. Nondestructive strain depth profiling with high energy X-ray diffraction: System capabilities and limitations

    NASA Astrophysics Data System (ADS)

    Zhang, Zhan; Wendt, Scott; Cosentino, Nicholas; Bond, Leonard J.

    2018-04-01

    Limited by photon energy, and penetration capability, traditional X-ray diffraction (XRD) strain measurements are only capable of achieving a few microns depth due to the use of copper (Cu Kα1) or molybdenum (Mo Kα1) characteristic radiation. For deeper strain depth profiling, destructive methods are commonly necessary to access layers of interest by removing material. To investigate deeper depth profiles nondestructively, a laboratory bench-top high-energy X-ray diffraction (HEXRD) system was previously developed. This HEXRD method uses an industrial 320 kVp X-Ray tube and the Kα1 characteristic peak of tungsten, to produces a higher intensity X-ray beam which enables depth profiling measurement of lattice strain. An aluminum sample was investigated with deformation/load provided using a bending rig. It was shown that the HEXRD method is capable of strain depth profiling to 2.5 mm. The method was validated using an aluminum sample where both the HEXRD method and the traditional X-ray diffraction method gave data compared with that obtained using destructive etching layer removal, performed by a commercial provider. The results demonstrate comparable accuracy up to 0.8 mm depth. Nevertheless, higher attenuation capabilities in heavier metals limit the applications in other materials. Simulations predict that HEXRD works for steel and nickel in material up to 200 µm, but experiment results indicate that the HEXRD strain profile is not practical for steel and nickel material, and the measured diffraction signals are undetectable when compared to the noise.

  9. Resonance energy shifts during nuclear Bragg diffraction of x rays

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

    Arthur, J.; Brown, G.S.; Brown, D.E.

    1989-10-09

    We have observed dramatic changes in the time distribution of synchrotron x rays resonantly scattered from {sup 57}Fe nuclei in a crystal of yttrium iron garnet, which depend on the deviation angle of the incident radiation from the Bragg angle. These changes are caused by small shifts in the effective energies of the hyperfine-split nuclear resonances, an effect of dynamical diffraction for the coherently excited nuclei in the crystal. The very high brightness of the synchro- tron x-ray source allows this effect to be observed in a 15-min measurement.

  10. X-ray diffraction study of elemental thulium to 86 GPa

    NASA Astrophysics Data System (ADS)

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

    2006-03-01

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

  11. Surface Area Analysis Using the Brunauer-Emmett-Teller (BET) Method: Standard Operating Procedure Series: SOP-C

    DTIC Science & Technology

    2016-09-01

    Method Scientific Operating Procedure Series : SOP-C En vi ro nm en ta l L ab or at or y Jonathon Brame and Chris Griggs September 2016...BET) Method Scientific Operating Procedure Series : SOP-C Jonathon Brame and Chris Griggs Environmental Laboratory U.S. Army Engineer Research and...response, including the time for reviewing instructions, searching existing data sources, gathering and maintaining the data needed, and completing

  12. Method for improving x-ray diffraction determinations of residual stress in nickel-base alloys

    DOEpatents

    Berman, R.M.; Cohen, I.

    1988-04-26

    A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys is discussed. Part of a predetermined area of the surface of a nickel-base alloy is covered with a dispersion. This exposes the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose, since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample. 2 figs.

  13. Preliminary small-angle X-ray scattering and X-ray diffraction studies of the BTB domain of lola protein from Drosophila melanogaster

    NASA Astrophysics Data System (ADS)

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

    2017-11-01

    The Drosophila genome has several dozens of transcription factors (TTK group) containing BTB domains assembled into octamers. The LOLA protein belongs to this family. The purification, crystallization, and preliminary X-ray diffraction and small-angle X-ray scattering (SAXS) studies of the BTB domain of this protein are reported. The crystallization conditions were found by the vapor-diffusion technique. A very low diffraction resolution (8.7 Å resolution) of the crystals was insufficient for the determination of the threedimensional structure of the BTB domain. The SAXS study demonstrated that the BTB domain of the LOLA protein exists as an octamer in solution.

  14. X-ray laser–induced electron dynamics observed by femtosecond diffraction from nanocrystals of Buckminsterfullerene

    PubMed Central

    Abbey, Brian; Dilanian, Ruben A.; Darmanin, Connie; Ryan, Rebecca A.; Putkunz, Corey T.; Martin, Andrew V.; Wood, David; Streltsov, Victor; Jones, Michael W. M.; Gaffney, Naylyn; Hofmann, Felix; Williams, Garth J.; Boutet, Sébastien; Messerschmidt, Marc; Seibert, M. Marvin; Williams, Sophie; Curwood, Evan; Balaur, Eugeniu; Peele, Andrew G.; Nugent, Keith A.; Quiney, Harry M.

    2016-01-01

    X-ray free-electron lasers (XFELs) deliver x-ray pulses with a coherent flux that is approximately eight orders of magnitude greater than that available from a modern third-generation synchrotron source. The power density of an XFEL pulse may be so high that it can modify the electronic properties of a sample on a femtosecond time scale. Exploration of the interaction of intense coherent x-ray pulses and matter is both of intrinsic scientific interest and of critical importance to the interpretation of experiments that probe the structures of materials using high-brightness femtosecond XFEL pulses. We report observations of the diffraction of extremely intense 32-fs nanofocused x-ray pulses by a powder sample of crystalline C60. We find that the diffraction pattern at the highest available incident power significantly differs from the one obtained using either third-generation synchrotron sources or XFEL sources operating at low output power and does not correspond to the diffraction pattern expected from any known phase of crystalline C60. We interpret these data as evidence of a long-range, coherent dynamic electronic distortion that is driven by the interaction of the periodic array of C60 molecular targets with intense x-ray pulses of femtosecond duration. PMID:27626076

  15. MSL Chemistry and Mineralogy X-Ray Diffraction X-Ray Fluorescence (CheMin) Instrument

    NASA Technical Reports Server (NTRS)

    Zimmerman, Wayne; Blake, Dave; Harris, William; Morookian, John Michael; Randall, Dave; Reder, Leonard J.; Sarrazin, Phillipe

    2013-01-01

    This paper provides an overview of the Mars Science Laboratory (MSL) Chemistry and Mineralogy Xray Diffraction (XRD), X-ray Fluorescence (XRF) (CheMin) Instrument, an element of the landed Curiosity rover payload, which landed on Mars in August of 2012. The scientific goal of the MSL mission is to explore and quantitatively assess regions in Gale Crater as a potential habitat for life - past or present. The CheMin instrument will receive Martian rock and soil samples from the MSL Sample Acquisition/Sample Processing and Handling (SA/SPaH) system, and process it utilizing X-Ray spectroscopy methods to determine mineral composition. The Chemin instrument will analyze Martian soil and rocks to enable scientists to investigate geophysical processes occurring on Mars. The CheMin science objectives and proposed surface operations are described along with the CheMin hardware with an emphasis on the system engineering challenges associated with developing such a complex instrument.

  16. Submicron x-ray diffraction and its applications to problems in materials and environmental science

    NASA Astrophysics Data System (ADS)

    Tamura, N.; Celestre, R. S.; MacDowell, A. A.; Padmore, H. A.; Spolenak, R.; Valek, B. C.; Meier Chang, N.; Manceau, A.; Patel, J. R.

    2002-03-01

    The availability of high brilliance third generation synchrotron sources together with progress in achromatic focusing optics allows us to add submicron spatial resolution to the conventional century-old x-ray diffraction technique. The new capabilities include the possibility to map in situ, grain orientations, crystalline phase distribution, and full strain/stress tensors at a very local level, by combining white and monochromatic x-ray microbeam diffraction. This is particularly relevant for high technology industry where the understanding of material properties at a microstructural level becomes increasingly important. After describing the latest advances in the submicron x-ray diffraction techniques at the Advanced Light Source, we will give some examples of its application in material science for the measurement of strain/stress in metallic thin films and interconnects. Its use in the field of environmental science will also be discussed.

  17. Investigation of Renal Stones by X-ray and Neutron Diffraction

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

    Baeva, M.; Boianova, A.; Beskrovnyi, A. I.

    2007-04-23

    Renal stones were investigated by X-ray diffraction. The obtained results showed only one crystal phase in every sample. With the aim to verify eventual availability of second phase (under 3 volume %) the same renal stones were investigated by neutron diffraction. The neutron spectra proved that additional crystal phase was absent in the renal stones. The obtained results are scientific-practical, in aid of the medicine, especially in the case of renal stone disease.

  18. X-Ray Diffraction and Fluorescence Measurements for In Situ Planetary Instruments

    NASA Astrophysics Data System (ADS)

    Hansford, G.; Hill, K. S.; Talboys, D.; Vernon, D.; Ambrosi, R.; Bridges, J.; Hutchinson, I.; Marinangeli, L.

    2011-12-01

    The ESA/NASA ExoMars mission, due for launch in 2018, has a combined X-ray fluorescence/diffraction instrument, Mars-XRD, as part of the onboard analytical laboratory. The results of some XRF (X-ray fluorescence) and XRD (X-ray diffraction) tests using a laboratory chamber with representative performance are reported. A range of standard geological reference materials and analogues were used in these tests. The XRD instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA ExoMars missions and will provide the first demonstrations of the capabilities of combined XRD/XRF instrumentation in situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-ray diffraction instrument, Mars-XRD [1,2]. Mars-XRD incorporates an Fe-55 radioisotope source and three fixed-position charge-coupled devices (CCDs) to simultaneously acquire an X-ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition. The CCDs cover an angular range of 2θ = 6° to 73° enabling the analysis of a wide range of geologically important minerals including phyllosilicates, feldspars, oxides, carbonates and evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an Fe-55 source and X-ray sensitive CCD. The XRF/XRD test system consists of a single CCD on a motorised arm, an Fe-55 X-ray source, a collimator and a sample table which approximately replicate the reflection geometry of the Mars-XRD instrument. It was used to test geological reference standard materials and Martian analogues. This work was funded by the Science and Technology Facilities Council, UK. References [1] Marinangeli, L., Hutchinson, I

  19. Structure of rare-earth chalcogenide glasses by neutron and x-ray diffraction

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

    Drewitt, James W. E.; Salmon, Philip S.; Zeidler, Anita

    The method of neutron diffraction with isomorphic substitution was used to measure the structure of the rare-earth chalcogenide glasses (R 2X 3) 0.07(Ga 2X 3) 0.33(GeX 2) 0.60 with R = La or Ce and X = S or Se. X-ray diffraction was also used to measure the structure of the sulphide glass. The results are consistent with networks that are built from GeX 4 and GaX 4 tetrahedra, and give R-S and R-Se coordination numbers of 8.0(2) and 8.5(4), respectively. The minimum nearest-neighbour R-R distance associated with rare-earth clustering is discussed.

  20. Structure of rare-earth chalcogenide glasses by neutron and x-ray diffraction

    DOE PAGES

    Drewitt, James W. E.; Salmon, Philip S.; Zeidler, Anita; ...

    2017-04-28

    The method of neutron diffraction with isomorphic substitution was used to measure the structure of the rare-earth chalcogenide glasses (R 2X 3) 0.07(Ga 2X 3) 0.33(GeX 2) 0.60 with R = La or Ce and X = S or Se. X-ray diffraction was also used to measure the structure of the sulphide glass. The results are consistent with networks that are built from GeX 4 and GaX 4 tetrahedra, and give R-S and R-Se coordination numbers of 8.0(2) and 8.5(4), respectively. The minimum nearest-neighbour R-R distance associated with rare-earth clustering is discussed.

  1. Solution to the Phase Problem Using Multibeam X-Ray Diffraction.

    NASA Astrophysics Data System (ADS)

    Shen, Qun

    Multi-beam x-ray diffraction, especially the asymmetry effect in the virtual Bragg scattering case, has been proved to provide useful phase information on the structure factors that are involved in the scattering process. A perturbation theory has been developed to provide an analytical expression for the diffracted wave field in virtual Bragg scattering situations, which explains the physical origin of the asymmetry effect. Two experiments on the (202) reflection of benzil, using 3.5 keV x-rays, have shown that the asymmetry effect is visible in a mosaic non-centrosymmetric organic crystal. The results do not depend on the shape of the crystal, hence proving that the method is universally applicable. A practical method to obtain arbitrary values of the phase triplet, based on the perturbation theory, has been developed and shown to work in the case of non-centrosymmetric crystals like benzil.

  2. Femtosecond X-ray coherent diffraction of aligned amyloid fibrils on low background graphene.

    PubMed

    Seuring, Carolin; Ayyer, Kartik; Filippaki, Eleftheria; Barthelmess, Miriam; Longchamp, Jean-Nicolas; Ringler, Philippe; Pardini, Tommaso; Wojtas, David H; Coleman, Matthew A; Dörner, Katerina; Fuglerud, Silje; Hammarin, Greger; Habenstein, Birgit; Langkilde, Annette E; Loquet, Antoine; Meents, Alke; Riek, Roland; Stahlberg, Henning; Boutet, Sébastien; Hunter, Mark S; Koglin, Jason; Liang, Mengning; Ginn, Helen M; Millane, Rick P; Frank, Matthias; Barty, Anton; Chapman, Henry N

    2018-05-09

    Here we present a new approach to diffraction imaging of amyloid fibrils, combining a free-standing graphene support and single nanofocused X-ray pulses of femtosecond duration from an X-ray free-electron laser. Due to the very low background scattering from the graphene support and mutual alignment of filaments, diffraction from tobacco mosaic virus (TMV) filaments and amyloid protofibrils is obtained to 2.7 Å and 2.4 Å resolution in single diffraction patterns, respectively. Some TMV diffraction patterns exhibit asymmetry that indicates the presence of a limited number of axial rotations in the XFEL focus. Signal-to-noise levels from individual diffraction patterns are enhanced using computational alignment and merging, giving patterns that are superior to those obtainable from synchrotron radiation sources. We anticipate that our approach will be a starting point for further investigations into unsolved structures of filaments and other weakly scattering objects.

  3. 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.

  4. Observation of sagittal X-ray diffraction by surface acoustic waves in Bragg geometry1

    PubMed Central

    Vadilonga, Simone; Zizak, Ivo; Roshchupkin, Dmitry; Evgenii, Emelin; Petsiuk, Andrei; Leitenberger, Wolfram; Erko, Alexei

    2017-01-01

    X-ray Bragg diffraction in sagittal geometry on a Y-cut langasite crystal (La3Ga5SiO14) modulated by Λ = 3 µm Rayleigh surface acoustic waves was studied at the BESSY II synchrotron radiation facility. Owing to the crystal lattice modulation by the surface acoustic wave diffraction, satellites appear. Their intensity and angular separation depend on the amplitude and wavelength of the ultrasonic superlattice. Experimental results are compared with the corresponding theoretical model that exploits the kinematical diffraction theory. This experiment shows that the propagation of the surface acoustic waves creates a dynamical diffraction grating on the crystal surface, and this can be used for space–time modulation of an X-ray beam. PMID:28381976

  5. 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

  6. 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

  7. 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

  8. 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

  9. 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.

  10. 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.

  11. In situ electrochemical high-energy X-ray diffraction using a capillary working electrode cell geometry

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

    Young, Matthias J.; Bedford, Nicholas M.; Jiang, Naisheng

    The ability to generate new electrochemically active materials for energy generation and storage with improved properties will likely be derived from an understanding of atomic-scale structure/function relationships during electrochemical events. Here, the design and implementation of a new capillary electrochemical cell designed specifically forin situhigh-energy X-ray diffraction measurements is described. By increasing the amount of electrochemically active material in the X-ray path while implementing low-Zcell materials with anisotropic scattering profiles, an order of magnitude enhancement in diffracted X-ray signal over traditional cell geometries for multiple electrochemically active materials is demonstrated. This signal improvement is crucial for high-energy X-ray diffraction measurementsmore » and subsequent Fourier transformation into atomic pair distribution functions for atomic-scale structural analysis. As an example, clear structural changes in LiCoO 2under reductive and oxidative conditions using the capillary cell are demonstrated, which agree with prior studies. Accurate modeling of the LiCoO 2diffraction data using reverse Monte Carlo simulations further verifies accurate background subtraction and strong signal from the electrochemically active material, enabled by the capillary working electrode geometry.« less

  12. Enhanced activity and stability of copper oxide/γ-alumina catalyst in catalytic wet-air oxidation: Critical roles of cerium incorporation

    NASA Astrophysics Data System (ADS)

    Zhang, Yongli; Zhou, Yanbo; Peng, Chao; Shi, Junjun; Wang, Qingyu; He, Lingfeng; Shi, Liang

    2018-04-01

    By successive impregnation method, the Ce-modified Cu-O/γ-Al2O3 catalyst was prepared and characterized using nitrogen adsorption-desorption, scanning electron microscopy energy dispersive X-ray analysis (SEM-EDS), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman, and H2-Temperature programming reduction (H2-TPR). In catalytic wet-air oxidation (CWAO) process for the printing and dyeing wastewater (PDW), the effects of Ce addition on performance, mechanism and kinetics of the catalyst were investigated. The Ce addition increases the Brunauer-Emmett-Teller (BET) surface area and pore volume of the catalyst and makes the active components uniformly distributed on the catalyst surface. Formation of a stable CuAl2O4 solid solution by anchoring Cu onto the γ-Al2O3 crystal lattice leads to a significant decrease in metal leaching of the Ce-modified catalyst. The proportion of lattice oxygen in the catalyst substantially increases and the apparent activation energy of Cu-O/γ-Al2O3 catalyst decreases owing to Ce addition. Therefore, the catalytic activity and stability of the Ce-modified catalyst are considerably improved. The scavengers experiments identify the active species existed in the CWAO reaction system, with the order of reactivity: h+ > O2•- > H2O2 > HO•. This novel Cu-Ce-O/γ-Al2O3 catalyst has great potential in applications for treatment of concentrated organic wastewater due to its superior catalytic activity and improved stability.

  13. Activated carbon-supported CuO nanoparticles: a hybrid material for carbon dioxide adsorption

    NASA Astrophysics Data System (ADS)

    Boruban, Cansu; Esenturk, Emren Nalbant

    2018-03-01

    Activated carbon-supported copper(II) oxide (CuO) nanoparticles were synthesized by simple impregnation method to improve carbon dioxide (CO2) adsorption capacity of the support. The structural and chemical properties of the hybrid material were characterized by scanning electron microscopy (SEM), energy dispersive X-ray (EDX), X-ray diffraction (https://www.google.com.tr/url?sa=t&rct=j&q=&esrc=s&source=web&cd=3&cad=rja&uact=8&ved=0CCsQFjAC&url=http%3A%2F%2Fwww.intertek.com%2Fanalytical-laboratories%2Fxrd%2F&ei=-5WZVYSCHISz7Aatqq-IAw&usg=AFQjCNFBlk-9wqy49foh8tskmbD-GGbG9g&sig2=eKrhYjO75rl_Id2sLGpq4w&bvm=bv.96952980,d.bGg) (XRD), X-ray photoelectron spectroscopy (XPS), atomic absorption spectroscopy (AAS), and Brunauer-Emmett-Teller (BET) analyses. The analyses showed that CuO nanoparticles are well-distributed on the activated carbon surface. The CO2 adsorption behavior of the activated carbon-supported CuO nanoparticles was observed by thermogravimetric analysis (TGA), temperature programmed desorption (TPD), Fourier transform infrared (FTIR), and BET analyses. The results showed that CuO nanoparticle loading on activated carbon led to about 70% increase in CO2 adsorption capacity of activated carbon under standard conditions (1 atm and 298 K). The main contributor to the observed increase is an improvement in chemical adsorption of CO2 due to the presence of CuO nanoparticles on activated carbon.

  14. Sonochemical surface functionalization of exfoliated LDH: Effect on textural properties, CO2 adsorption, cyclic regeneration capacities and subsequent gas uptake for simultaneous methanol synthesis.

    PubMed

    Ezeh, Collins I; Huang, Xiani; Yang, Xiaogang; Sun, Cheng-Gong; Wang, Jiawei

    2017-11-01

    To improve CO 2 adsorption, amine modified Layered double hydroxide (LDH) were prepared via a two stage process, SDS/APTS intercalation was supported by ultrasonic irradiation and then followed by MEA extraction. The prepared samples were characterised using Scanning electron microscope-Energy dispersive X-ray spectroscopy (SEM-EDX), X-ray Photoelectron Spectroscopy (XPS), X-ray diffraction (XRD), Temperature Programmed Desorption (TPD), Brunauer-Emmett-Teller (BET), and Thermogravimetric analysis (TGA), respectively. The characterisation results were compared with those obtained using the conventional preparation method with consideration to the effect of sonochemical functionalization on textural properties, adsorption capacity, regeneration and lifetime of the LDH adsorbent. It is found that LDHs prepared by sonochemical modification had improved pore structure and CO 2 adsorption capacity, depending on sonic intensity. This is attributed to the enhanced deprotonation of activated amino functional groups via the sonochemical process. Subsequently, this improved the amine loading and effective amine efficiency by 60% of the conventional. In addition, the sonochemical process improved the thermal stability of the adsorbent and also, reduced the irreversible CO 2 uptake, CUirrev, from 0.18mmol/g to 0.03mmol/g. Subsequently, improving the lifetime and ease of regenerating the adsorbent respectively. This is authenticated by subjecting the prepared adsorbents to series of thermal swing adsorption (TSA) cycles until its adsorption capacity goes below 60% of the original CO 2 uptake. While the conventional adsorbent underwent a 10 TSA cycles before breaking down, the sonochemically functionalized LDH went further than 30 TSA cycles. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Amorphous mesoporous GeO x anode for Na-ion batteries with high capacity and long lifespan.

    PubMed

    Shen, Kangze; Lin, Ning; Xu, Tianjun; Han, Ying; Qian, Yitai

    2018-01-01

    It is recently demonstrated that amorphous Ge anode shows higher reversible Na-ion storage capacity (590 mA h g -1 ) than crystallized Ge anode (369 mA h g -1 ). Here, amorphous GeO x anode is prepared by a simple wet-chemistry reduction route at room temperature. The obtained amorphous GeO x shows a porous hierarchical architecture, accompanied with a Brunauer-Emmett-Teller surface area of 159 m 2  g -1 and an average pore diameter of 14 nm. This unique structure enables the GeO x anode to enhance the Na-ion/electron diffusion rate, and buffer the volume change. As anode for Na-ion battery, high reversible capacity over 400 mA h g -1 , fine rate capability with a capacity of 200 mA h g -1 maintained at 3.0 A g -1 and long-term cycling stability with 270 mA h g -1 even over 1000 cycles at 1.0 A g -1 are obtained.

  16. Evaluation of Aluminium Dross as Adsorbent for Removal of Carcinogenic Congo Red Dye in Wastewater

    NASA Astrophysics Data System (ADS)

    Zakaria, Mohamad Zulfika Hazielim b.; Zauzi, Nur Syuhada Ahmad; Baini, Rubiyah; Sutan, Norsuzailina Mohamed; Rezaur Rahman, Md

    2017-06-01

    In this study, aluminium dross waste generated from aluminium smelting industries was employed as adsorbent in removing of congo red dye in aqueous solution. The raw aluminium dross as adsorbent was characterized using Scanning Electron Microscope (SEM), Brunauer-Emmett-Teller (BET) for surface area and X-Ray Fluorescence (XRF) Spectroscopy. Adsorption experiments were carried out by batch system at different adsorbent mass, pH, and initial dye concentration. The results showed that the per cent removal of dye increased as adsorbent mass increased. It was found that 0.4 gram of adsorbent can remove approximately 100 % of dye at pH 9 for dye concentration 20 and 40 ppm. Therefore, it can be concluded that raw aluminium dross without undergone any treatment can be effectively used for the adsorption of congo red in textile wastewater related industries.

  17. Manganese porphyrin immobilized on magnetic MCM-41 nanoparticles as an efficient and reusable catalyst for alkene oxidations with sodium periodate

    NASA Astrophysics Data System (ADS)

    Hajian, Robabeh; Ehsanikhah, Amin

    2018-01-01

    This study describes the immobilization of tetraphenylporphyrinatomanganese(III) chloride, (MnPor), onto imidazole functionalized MCM-41 with magnetite nanoparticle core (Fe3O4@MCM-41-Im). The resultant material (Fe3O4@MCM-41-Im@MnPor) was characterized by X-ray diffractometry (XRD), Fourier transform infra-red (FT-IR), diffuse reflectance UV-Vis spectrophotometry (DR UV-Vis), field emission scanning electron microscopy (FESEM), Inductively coupled plasma (ICP), analyzer transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) surface area. This new heterogenized catalyst was applied as an efficient catalyst for the epoxidation of a variety of cyclic and linear olefins with NaIO4 under mild conditions. The prepared catalyst can be easily recovered through the application of an external magnet, and reused several times without any significant decrease in activity and magnetic properties.

  18. Risk and benefit of diffraction in Energy Dispersive X-ray fluorescence mapping

    NASA Astrophysics Data System (ADS)

    Nikonow, Wilhelm; Rammlmair, Dieter

    2016-11-01

    Energy dispersive X-ray fluorescence mapping (μ-EDXRF) is a fast and non-destructive method for chemical quantification and therefore used in many scientific fields. The combination of spatial and chemical information is highly valuable for understanding geological processes. Problems occur with crystalline samples due to diffraction, which appears according to Bragg's law, depending on the energy of the X-ray beam, the incident angle and the crystal parameters. In the spectra these peaks can overlap with element peaks suggesting higher element concentrations. The aim of this study is to investigate the effect of diffraction, the possibility of diffraction removal and potential geoscientific applications for X-ray mapping. In this work the μ-EDXRF M4 Tornado from Bruker was operated with a Rh-tube and polychromatic beam with two SDD detectors mounted each at ± 90° to the tube. Due to the polychromatic beam the Bragg condition fits for several mineral lattice planes. Since diffraction depends on the angle, it is shown that a novel correction approach can be applied by measuring from two different angles and calculating the minimum spectrum of both detectors gaining a better limit of quantification for this method. Furthermore, it is possible to use the diffraction information for separation of differently oriented crystallites within a monomineralic aggregate and obtain parameters like particle size distribution for the sample, as it is done by thin section image analysis in cross-polarized light. Only with μ-EDXRF this can be made on larger samples without preparation of thin sections.

  19. Correct interpretation of diffraction properties of quartz crystals for X-ray optics applications

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

    Huang, Xian-Rong; Gog, Thomas; Kim, Jungho

    Quartz has hundreds of strong Bragg reflections that may offer a great number of choices for making fixed-angle X-ray analyzers and polarizers at virtually any hard X-ray energies with selectable resolution. However, quartz crystals, unlike silicon and germanium, are chiral and may thus appear in two different forms of handedness that are mirror images. Furthermore, because of the threefold rotational symmetry along thecaxis, the {h 1h 2h 3L} and {h 2h 1h 3L} Bragg reflections may have quite different Darwin bandwidth, reflectivity and angular acceptance, although they have the same Bragg angle. The design of X-ray optics from quartz crystalsmore » therefore requires unambiguous determination of the orientation, handedness and polarity of the crystals. The Laue method and single-axis diffraction technique can provide such information, but the variety of conventions used in the literature to describe quartz structures has caused widespread confusion. The current studies give detailed guidelines for design and fabrication of quartz X-ray optics, with special emphasis on the correct interpretation of Laue patterns in terms of the crystallography and diffraction properties of quartz. Meanwhile, the quartz crystals examined were confirmed by X-ray topography to have acceptably low densities of dislocations and other defects, which is the foundation for developing high-resolution quartz-based X-ray optics.« less

  20. Influence of neutron irradiation on the microstructure of nuclear graphite: An X-ray diffraction study

    NASA Astrophysics Data System (ADS)

    Zhou, Z.; Bouwman, W. G.; Schut, H.; van Staveren, T. O.; Heijna, M. C. R.; Pappas, C.

    2017-04-01

    Neutron irradiation effects on the microstructure of nuclear graphite have been investigated by X-ray diffraction on virgin and low doses (∼ 1.3 and ∼ 2.2 dpa), high temperature (750° C) irradiated samples. The diffraction patterns were interpreted using a model, which takes into account the turbostratic disorder. Besides the lattice constants, the model introduces two distinct coherent lengths in the c-axis and the basal plane, that characterise the volumes from which X-rays are scattered coherently. The methodology used in this work allows to quantify the effect of irradiation damage on the microstructure of nuclear graphite seen by X-ray diffraction. The results show that the changes of the deduced structural parameters are in agreement with previous observations from electron microscopy, but not directly related to macroscopic changes.

  1. X-Ray Diffractive Optics

    NASA Technical Reports Server (NTRS)

    Dennis, Brian; Li, Mary; Skinner, Gerald

    2013-01-01

    X-ray optics were fabricated with the capability of imaging solar x-ray sources with better than 0.1 arcsecond angular resolution, over an order of magnitude finer than is currently possible. Such images would provide a new window into the little-understood energy release and particle acceleration regions in solar flares. They constitute one of the most promising ways to probe these regions in the solar atmosphere with the sensitivity and angular resolution needed to better understand the physical processes involved. A circular slit structure with widths as fine as 0.85 micron etched in a silicon wafer 8 microns thick forms a phase zone plate version of a Fresnel lens capable of focusing approx. =.6 keV x-rays. The focal length of the 3-cm diameter lenses is 100 microns, and the angular resolution capability is better than 0.1 arcsecond. Such phase zone plates were fabricated in Goddard fs Detector Development Lab. (DDL) and tested at the Goddard 600-microns x-ray test facility. The test data verified that the desired angular resolution and throughput efficiency were achieved.

  2. A Curved Image-Plate Detector System for High-Resolution Synchrotron X-ray Diffraction

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

    Sarin, P.; Haggerty, R; Yoon, W

    2009-01-01

    The developed curved image plate (CIP) is a one-dimensional detector which simultaneously records high-resolution X-ray diffraction (XRD) patterns over a 38.7 2{theta} range. In addition, an on-site reader enables rapid extraction, transfer and storage of X-ray intensity information in {le}30 s, and further qualifies this detector to study kinetic processes in materials science. The CIP detector can detect and store X-ray intensity information linearly proportional to the incident photon flux over a dynamical range of about five orders of magnitude. The linearity and uniformity of the CIP detector response is not compromised in the unsaturated regions of the image plate,more » regardless of saturation in another region. The speed of XRD data acquisition together with excellent resolution afforded by the CIP detector is unique and opens up wide possibilities in materials research accessible through X-ray diffraction. This article presents details of the basic features, operation and performance of the CIP detector along with some examples of applications, including high-temperature XRD.« less

  3. Framework for three-dimensional coherent diffraction imaging by focused beam x-ray Bragg ptychography.

    PubMed

    Hruszkewycz, Stephan O; Holt, Martin V; Tripathi, Ash; Maser, Jörg; Fuoss, Paul H

    2011-06-15

    We present the framework for convergent beam Bragg ptychography, and, using simulations, we demonstrate that nanocrystals can be ptychographically reconstructed from highly convergent x-ray Bragg diffraction. The ptychographic iterative engine is extended to three dimensions and shown to successfully reconstruct a simulated nanocrystal using overlapping raster scans with a defocused curved beam, the diameter of which matches the crystal size. This object reconstruction strategy can serve as the basis for coherent diffraction imaging experiments at coherent scanning nanoprobe x-ray sources.

  4. Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals

    DOE PAGES

    Dao, E. Han; Sierra, Raymond G.; Laksmono, Hartawan; ...

    2015-04-30

    In this work, we collected radiation-damage-free data from a set of cryo-cooled crystals for a novel 30S ribosomal subunit mutant using goniometer-based femtosecond crystallography. Crystal quality assessment for these samples was conducted at the X-ray Pump Probe end-station of the Linac Coherent Light Source (LCLS) using recently introduced goniometer-based instrumentation. These 30S subunit crystals were genetically engineered to omit a 26-residue protein, Thx, which is present in the wild-type Thermus thermophilus 30S ribosomal subunit. We are primarily interested in elucidating the contribution of this ribosomal protein to the overall 30S subunit structure. To assess the viability of this study, femtosecondmore » X-ray diffraction patterns from these crystals were recorded at the LCLS during a protein crystal screening beam time. During our data collection, we successfully observed diffraction from these difficult-to-grow 30S ribosomal subunit crystals. Most of our crystals were found to diffract to low resolution, while one crystal diffracted to 3.2 Å resolution. These data suggest the feasibility of pursuing high-resolution data collection as well as the need to improve sample preparation and handling in order to collect a complete radiation-damage-free data set using an X-ray Free Electron Laser.« less

  5. 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.

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

    DOE PAGES

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

    2016-06-24

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

  7. Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

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

    McGonegle, David, E-mail: d.mcgonegle1@physics.ox.ac.uk; Wark, Justin S.; Higginbotham, Andrew

    2015-08-14

    A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as maymore » occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. The simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.« less

  8. Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

    DOE PAGES

    McGonegle, David; Milathianaki, Despina; Remington, Bruce A.; ...

    2015-08-11

    A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as maymore » occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. In conclusion, the simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.« less

  9. 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...

  10. A study of X-ray multiple diffraction by means of section topography.

    PubMed

    Kohn, V G; Smirnova, I A

    2015-09-01

    The results of theoretical and experimental study are presented for the question of how the X-ray multiple diffraction in a silicon single crystal influences the interference fringes of section topography for the 400 reflection in the Laue case. Two different cases of multiple diffraction are discovered for zero and very small values of the azimuthal angle for the sample in the form of a plate with the surface normal to the 001 direction. The cases are seen on the same topogram without rotation of the crystal. Accurate computer simulations of the section topogram for the case of X-ray multiple diffraction are performed for the first time. It is shown that the structure of interference fringes on the section topogram in the region of multiple diffraction becomes more complicated. It has a very sharp dependence on the azimuthal angle. The experiment is carried out using a laboratory source under conditions of low resolution over the azimuthal angle. Nevertheless, the characteristic inclination of the interference fringes on the tails of the multiple diffraction region is easily seen. This phenomenon corresponds completely to the computer simulations.

  11. Synchrotron X-ray powder diffraction data of LASSBio-1515: A new N-acylhydrazone derivative compound

    NASA Astrophysics Data System (ADS)

    Costa, F. N.; Braz, D.; Ferreira, F. F.; da Silva, T. F.; Barreiro, E. J.; Lima, L. M.; Colaço, M. V.; Kuplich, L.; Barroso, R. C.

    2014-02-01

    In this work, synchrotron X-ray powder diffraction data allowed for a successful indexing of LASSBio-1515 compound, candidate to analgesic and anti-inflammatory activity. X-ray powder diffraction data collected in transmission and high-throughput geometries were used to analyze this compound. The X-ray wavelength of the synchrotron radiation used in this study was determined to be λ=1.55054 Å. LASSBio-1515 was found to be monoclinic with space group P21/c and unit cell parameters a=11.26255(16) Å, b=12.59785(16) Å, c=8.8540(1) Å, β=90.5972(7)° and V=1256.17(3) Å3.

  12. 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).

  13. Observation of divergent-beam X-ray diffraction from a crystal of diamond using synchrotron radiation.

    PubMed

    Glazer, A M; Collins, S P; Zekria, D; Liu, J; Golshan, M

    2004-03-01

    In 1947 Kathleen Lonsdale conducted a series of experiments on X-ray diffraction using a divergent beam external to a crystal sample. Unlike the Kossel technique, where divergent X-rays are excited by the presence of fluorescing atoms within the crystal, the use of an external divergent source made it possible to study non-fluorescing crystals. The resulting photographs not only illustrated the complexity of X-ray diffraction from crystals in a truly beautiful way, but also demonstrated unprecedented experimental precision. This long-forgotten work is repeated here using a synchrotron radiation source and, once again, considerable merit is found in Lonsdale's technique. The results of this experiment suggest that, through the use of modern 'third-generation' synchrotron sources, divergent-beam diffraction could soon enjoy a renaissance for high-precision lattice-parameter determination and the study of crystal perfection.

  14. Characterization of ion beam sputtered deposited W/Si multilayers by grazing incidence x-ray diffraction and x-ray reflectivity technique

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

    Dhawan, Rajnish, E-mail: rajnish@rrcat.gov.in; Rai, Sanjay

    2016-05-23

    W/Si multilayers four samples have been deposited on silicon substrate using ion beam sputtering system. Thickness of tungsten (W) varies from around 10 Å to 40 Å while the silicon (Si) thickness remains constant at around 30 Å in multilayers [W-Si]{sub x4}. The samples have been characterized by grazing incidence X-ray diffraction (GIXRD) and X-ray reflectivity technique (XRR). GIXRD study shows the crystalline behaviour of W/Si multilayer by varying W thickness and it is found that above 20 Å the W film transform from amorphous to crystalline phase and X-ray reflectivity data shows that the roughnesses of W increases onmore » increasing the W thicknesses in W/Si multilayers.« less

  15. High resolution X-ray diffraction imaging of lead tin telluride

    NASA Technical Reports Server (NTRS)

    Steiner, Bruce; Dobbyn, Ronald C.; Black, David; Burdette, Harold; Kuriyama, Masao; Spal, Richard; Simchick, Richard; Fripp, Archibald

    1991-01-01

    High resolution X-ray diffraction images of two directly comparable crystals of lead tin telluride, one Bridgman-grown on Space Shuttle STS 61A and the other terrestrially Bridgman-grown under similar conditions from identical material, present different subgrain structure. In the terrestrial, sample 1 the appearance of an elaborate array of subgrains is closely associated with the intrusion of regions that are out of diffraction in all of the various images. The formation of this elaborate subgrain structure is inhibited by growth in microgravity.

  16. Roosevelt Hot Springs, Utah FORGE X-Ray Diffraction Data

    DOE Data Explorer

    Nash, Greg; Jones, Clay

    2018-02-07

    This dataset contains X-ray diffraction (XRD) data taken from wells and outcrops as part of the DOE GTO supported Utah FORGE project located near Roosevelt Hot Springs. It contains an Excel spreadsheet with the XRD data, a text file with sample site names, types, and locations in UTM, Zone 12, NAD83 coordinates, and a GIS shapefile of the sample locations with attributes.

  17. Nanomodulated electron beams via electron diffraction and emittance exchange for coherent x-ray generation

    DOE PAGES

    Nanni, E. A.; Graves, W. S.; Moncton, D. E.

    2018-01-19

    We present a new method for generation of relativistic electron beams with current modulation on the nanometer scale and below. The current modulation is produced by diffracting relativistic electrons in single crystal Si, accelerating the diffracted beam and imaging the crystal structure, then transferring the image into the temporal dimension via emittance exchange. The modulation period can be tuned by adjusting electron optics after diffraction. This tunable longitudinal modulation can have a period as short as a few angstroms, enabling production of coherent hard x-rays from a source based on inverse Compton scattering with total accelerator length of approximately tenmore » meters. Electron beam simulations from cathode emission through diffraction, acceleration, and image formation with variable magnification are presented along with estimates of the coherent x-ray output properties.« less

  18. Nanomodulated electron beams via electron diffraction and emittance exchange for coherent x-ray generation

    NASA Astrophysics Data System (ADS)

    Nanni, E. A.; Graves, W. S.; Moncton, D. E.

    2018-01-01

    We present a new method for generation of relativistic electron beams with current modulation on the nanometer scale and below. The current modulation is produced by diffracting relativistic electrons in single crystal Si, accelerating the diffracted beam and imaging the crystal structure, then transferring the image into the temporal dimension via emittance exchange. The modulation period can be tuned by adjusting electron optics after diffraction. This tunable longitudinal modulation can have a period as short as a few angstroms, enabling production of coherent hard x-rays from a source based on inverse Compton scattering with total accelerator length of approximately ten meters. Electron beam simulations from cathode emission through diffraction, acceleration, and image formation with variable magnification are presented along with estimates of the coherent x-ray output properties.

  19. Nanomodulated electron beams via electron diffraction and emittance exchange for coherent x-ray generation

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

    Nanni, E. A.; Graves, W. S.; Moncton, D. E.

    We present a new method for generation of relativistic electron beams with current modulation on the nanometer scale and below. The current modulation is produced by diffracting relativistic electrons in single crystal Si, accelerating the diffracted beam and imaging the crystal structure, then transferring the image into the temporal dimension via emittance exchange. The modulation period can be tuned by adjusting electron optics after diffraction. This tunable longitudinal modulation can have a period as short as a few angstroms, enabling production of coherent hard x-rays from a source based on inverse Compton scattering with total accelerator length of approximately tenmore » meters. Electron beam simulations from cathode emission through diffraction, acceleration, and image formation with variable magnification are presented along with estimates of the coherent x-ray output properties.« less

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

    PubMed

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

    2015-03-01

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

  1. X-ray absorption microtomography (microCT) and small beam diffraction mapping of sea urchin teeth.

    PubMed

    Stock, S R; Barss, J; Dahl, T; Veis, A; Almer, J D

    2002-07-01

    Two noninvasive X-ray techniques, laboratory X-ray absorption microtomography (microCT) and X-ray diffraction mapping, were used to study teeth of the sea urchin Lytechinus variegatus. MicroCT revealed low attenuation regions at near the tooth's stone part and along the carinar process-central prism boundary; this latter observation appears to be novel. The expected variation of Mg fraction x in the mineral phase (calcite, Ca(1-x)Mg(x)CO(3)) cannot account for all of the linear attenuation coefficient decrease in the two zones: this suggested that soft tissue is localized there. Transmission diffraction mapping (synchrotron X-radiation, 80.8 keV, 0.1 x 0.1mm(2) beam area, 0.1mm translation grid, image plate area detector) simultaneously probed variations in 3-D and showed that the crystal elements of the "T"-shaped tooth were very highly aligned. Diffraction patterns from the keel (adaxial web) and from the abaxial flange (containing primary plates and the stone part) differed markedly. The flange contained two populations of identically oriented crystal elements with lattice parameters corresponding to x=0.13 and x=0.32. The keel produced one set of diffraction spots corresponding to the lower x. The compositions were more or less equivalent to those determined by others for camarodont teeth, and the high Mg phase is expected to be disks of secondary mineral epitaxially related to the underlying primary mineral element. Lattice parameter gradients were not noted in the keel or flange. Taken together, the microCT and diffraction results indicated that there was a band of relatively high protein content, of up to approximately 0.25 volume fraction, in the central part of the flange and paralleling its adaxial and abaxial faces. X-ray microCT and microdiffraction data used in conjunction with protein distribution data will be crucial for understanding the properties of various biocomposites and their mechanical functions.

  2. The effect of laser radiation on the diffraction of X-rays in crystals

    NASA Astrophysics Data System (ADS)

    Trushin, V. N.; Chuprunov, E. V.; Khokhlov, A. F.

    1988-10-01

    The effect of laser radiation on the intensity of the X-ray diffraction peaks of KDP, ADP, and CuSO4-5H2O crystals was studied experimentally. This intensity was found to increase as a function of the laser beam power. This result suggests that it is possible to use laser beams to control X-ray intensity in the crystals considered.

  3. Anomalous x-ray diffraction on InAs/GaAs quantum dot systems

    NASA Astrophysics Data System (ADS)

    Schulli, T. U.; Sztucki, M.; Chamard, V.; Metzger, T. H.; Schuh, D.

    2002-07-01

    Free-standing InAs quantum dots on a GaAs (001) substrate have been investigated using grazing incidence x-ray diffraction. To suppress the strong scattering contribution from the GaAs substrate, we performed anomalous diffraction experiments at the superstructure (200) reflection, showing that the relative intensities from the dots and the substrate undergo a significant change with the x-ray energy below and above the As K edge. Since the signal from the substrate material can essentially be suppressed, this method is ideally suited for the investigation of strain, shape, and interdiffusion of buried quantum dots and quantum dots embedded in heteroepitaxial multilayers. In addition, we show that it can be used as a tool for studying wetting layers.

  4. 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., E-mail: haughmj@nv.doe.gov; Jacoby, K. D.; Wu, M.

    2014-11-15

    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 in Albuquerque, New Mexico. 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 double crystal diffractometer 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

  5. 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

  6. Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystalsa)

    NASA Astrophysics Data System (ADS)

    Haugh, M. J.; Wu, M.; Jacoby, K. D.; Loisel, G. P.

    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 that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. 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 double crystal diffractometer 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.

  7. Preparation of nanocrystalline forsterite by combustion of different fuels and their comparative in-vitro bioactivity, dissolution behaviour and antibacterial studies.

    PubMed

    Choudhary, Rajan; Manohar, Prasanth; Vecstaudza, Jana; Yáñez-Gascón, Maria Josefa; Sánchez, Horacio Pérez; Nachimuthu, Ramesh; Locs, Janis; Swamiappan, Sasikumar

    2017-08-01

    This study presents different fuels (Glycine and Urea) that can be used to synthesize nanocrystalline forsterite by the sol-gel combustion method. The weight change of precursor during thermal treatment was studied by thermo-gravimetric analysis (TGA). Pure forsterite was characterized by heating microscopy, Fourier transform infrared spectroscopy, X-ray Diffraction, Brunauer-Emmett-Teller, Scanning Electron Microscopy, and Energy dispersive X-ray spectroscopy. The HAP (hydroxyapatite) deposition ability, degradation and dissolution behaviour of forsterite was examined in simulated body fluid (SBF). The combusted forsterite precursor showed distinct thermal behaviour for each fuel when analyzed by heating microscopy. BET analysis showed that the particle size of forsterite synthesized using glycine was 28nm, specific surface area 65.11m 2 /g and average pore diameter 16.4nm while using urea 1.951μm, 0.939m 2 /g, and 30.5nm are the respective parameters. The dissolution of forsterite pointed to the consumption of Ca and P ions from SBF, the negligible release of Si ion into the SBF and these ionic interactions with SBF can be altered as per the material properties. The forsterite showed good antibacterial activity against S. aureus but lower activity against E. coli. The bactericidal activity of forsterite indicated that it can be used to inhibit biofilm formation in dental, bone implants and bacterial infection during surgical operations. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Zirconium doped nano-dispersed oxides of Fe, Al and Zn for destruction of warfare agents

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

    Stengl, Vaclav, E-mail: stengl@uach.cz; Houskova, Vendula; Bakardjieva, Snejana

    2010-11-15

    Zirconium doped nano dispersive oxides of Fe, Al and Zn were prepared by a homogeneous hydrolysis of the respective sulfate salts with urea in aqueous solutions. Synthesized metal oxide hydroxides were characterized using Brunauer-Emmett-Teller (BET) surface area and Barrett-Joiner-Halenda porosity (BJH), X-ray diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM) and energy-dispersive X-ray microanalysis (EDX). These oxides were taken for an experimental evaluation of their reactivity with sulfur mustard (HD or bis(2-chloroethyl)sulfide), soman (GD or (3,3'-Dimethylbutan-2-yl)-methylphosphonofluoridate) and VX agent (S-[2-(diisopropylamino)ethyl]-O-ethyl-methylphosphonothionate). The presence of Zr{sup 4+} dopant can increase both the surface area and the surface hydroxylation of the resultingmore » doped oxides, decreases their crystallites' sizes thereby it may contribute in enabling the substrate adsorption at the oxide surface thus it can accelerate the rate of degradation of warfare agents. Addition of Zr{sup 4+} converts the product of the reaction of ferric sulphate with urea from ferrihydrite to goethite. We found out that doped oxo-hydroxides Zr-FeO(OH) - being prepared by a homogeneous hydrolysis of ferric and zirconium oxo-sulfates mixture in aqueous solutions - exhibit a comparatively higher degradation activity towards chemical warfare agents (CWAs). Degradation of soman or VX agent on Zr-doped FeO(OH) containing ca. 8.3 wt.% of zirconium proceeded to completion within 30 min.« less

  9. Design and synthesis of hierarchical mesoporous WO3-MnO2 composite nanostructures on carbon cloth for high-performance supercapacitors

    NASA Astrophysics Data System (ADS)

    Shinde, Pragati A.; Lokhande, Vaibhav C.; Patil, Amar M.; Ji, Taeksoo; Lokhande, Chandrakant D.

    2017-12-01

    To enhance the energy density and power performance of supercapacitors, the rational design and synthesis of active electrode materials with hierarchical mesoporous structure is highly desired. In the present work, fabrication of high-performance hierarchical mesoporous WO3-MnO2 composite nanostructures on carbon cloth substrate via a facile hydrothermal method is reported. By varying the content of MnO2 in the composite, different WO3-MnO2 composite thin films are obtained. The formation of composite is confirmed by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analyses. The Brunauer-Emmett-Teller (BET) analysis reveals maximum specific surface area of 153 m2 g-1. The optimized WO3-MnO2 composite electrode demonstrates remarkable electrochemical performance with high specific capacitance of 657 F g-1 at a scan rate of 5 mV s-1 and superior longterm cycling stability (92% capacity retention over 2000 CV cycles). Furthermore, symmetric flexible solid-state supercapacitor based on WO3-MnO2 electrodes has been fabricated. The device exhibits good electrochemical performance with maximum specific capacitance of 78 F g-1 at a scan rate of 5 mV s-1 and specific energy of 10.8 Wh kg-1 at a specific power of 0.65 kW kg-1. The improved electrochemical performance could be ascribed to the unique combination of multivalence WO3 and MnO2 nanostructures and synergistic effect between them

  10. Room-temperature CO Thermoelectric Gas Sensor based on Au/Co3O4 Catalyst Tablet.

    PubMed

    Sun, L; Luan, W L; Wang, T C; Su, W X; Zhang, L X

    2017-02-17

    A carbon monoxide (CO) thermoelectric (TE) gas sensor was fabricated by affixing a Au/Co 3 O 4 catalyst tablet on a TE film layer. The Au/Co 3 O 4 catalyst tablet was prepared by a co-precipitation and tablet compression method and its possible catalytic mechanism was discussed by means of x-ray diffraction, field emission scanning electron microscopy, high resolution transmission electron microscopy, x-ray photoelectron spectroscopy, temperature-programmed reduction of hydrogen, Fourier transform infrared spectroscopy and Brunauer-Emmett-Teller analysis. The optimal catalyst, with a Au content of 10 wt%, was obtained at a calcination temperature between 200 and 300 °C. The small size of the Au nanoparticles, high specific surface, the existence of Co 3+ and water-derived species contributed to  high catalytic activity. Based on the optimal Au/Co 3 O 4 catalyst tablet, the CO TE gas sensor worked at room temperature and showed a response voltage signal (ΔV) of 23 mV, high selectivity among hydrogen and methane, high stability, and a fast response time of 106 s for 30 000 ppm CO/air. In addition, a CO concentration in the range of 5000-30 000 ppm could obviously be detected and exhibited a linear relationship with ΔV. The CO TE gas sensor provides a promising option for the detection of CO gas at room temperature.

  11. Effective sorption of atrazine by biochar colloids and residues derived from different pyrolysis temperatures.

    PubMed

    Yang, Fan; Gao, Yan; Sun, Lili; Zhang, Shuaishuai; Li, Jiaojiao; Zhang, Ying

    2018-04-26

    Biochar has attracted much attention, which owns many environmental and agronomic benefits, including carbon sequestration, improvement of soil quality, and immobilization of environmental contaminants. Biochar has been also investigated as an effective sorbent in recent publications. Generally, biochar particles can be divided into colloids and residues according to particle sizes, while understanding of adsorption capacities towards organic pollutants in each section is largely unknown, representing a critical knowledge gap in evaluations on the effectiveness of biochar for water treatment application. Scanning electron microscopy (SEM) images, X-ray diffraction (XRD), Raman spectra, Fourier-transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and Brunauer-Emmett-Teller (BET) method are used to examine the structures and surface properties of biochar colloids and residues derived from corn straws prepared at different pyrolysis temperatures. Also, their roles in atrazine (a typical organic pollutant) removal are investigated by batch adsorption experiments and fitted by different kinetic and thermodynamic models, respectively. The adsorption capacities of biochar colloids are much more than those of residues, resulting from the colloids containing abundant oxygen functional groups and mineral substances, and the adsorption capacities of biochar colloids and residues increase with the increase of pyrolysis temperatures. The highest adsorption performance of 139.33 mg g -1 can be obtained in biochar colloids prepared at 700 °C, suggesting the important functions of biochar colloids in the application of atrazine removal by biochar.

  12. Natural fiber templated TiO2 microtubes via a double soaking sol-gel route and their photocatalytic performance

    NASA Astrophysics Data System (ADS)

    Yang, Li; Li, Xu; Wang, Ziru; Shen, Yun; Liu, Ming

    2017-10-01

    TiO2 microtubes with a yam-like surface were prepared for the first time through a simple and efficient double soaking sol-gel route by utilizing Platanus acerifolia seed fibers as bio-templates. The physicochemical properties of the samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), Brunauer Emmett Teller (BET) surface analysis and Ultraviolet-visible absorption spectroscopy (UV-vis). The results showed that the obtained TiO2 microtubes had an anatase phase and were composed of a smooth internal wall and a rough yam-like external wall with an average diameter of 24 μm and the wall thickness of 2 μm. The surface area and pore volume of the as-prepared TiO2 microtubes reached 128.271 m2/g and 0.149 cm3/g, respectively. The UV-vis analysis displayed a favorable extension of light absorption capacity of TiO2 microtubes. The synthetic mechanism was preliminarily discussed as well. The moisture in the natural fiber templates facilitated the mild hydrolysis of titanium sol, leaving a prime layer on the surface of the fibers, and subsequently assisted in the successful preparation of TiO2 microtubes with a yam-like surface without requiring specific control of hydrolysis. Photocatalytic experiments indicated that the as-obtained TiO2 microtubes exhibited a higher efficiency than commercial P25 in the degradation of tetracycline hydrochloride.

  13. Finely Tuned SnO2 Nanoparticles for Efficient Detection of Reducing and Oxidizing Gases: The Influence of Alkali Metal Cation on Gas-Sensing Properties.

    PubMed

    Lee, Szu-Hsuan; Galstyan, Vardan; Ponzoni, Andrea; Gonzalo-Juan, Isabel; Riedel, Ralf; Dourges, Marie-Anne; Nicolas, Yohann; Toupance, Thierry

    2018-03-28

    Tin dioxide (SnO 2 ) nanoparticles were straightforwardly synthesized using an easily scaled-up liquid route that involves the hydrothermal treatment, either under acidic or basic conditions, of a commercial tin dioxide particle suspension including potassium counterions. After further thermal post-treatment, the nanomaterials have been thoroughly characterized by Fourier transform infrared and Raman spectroscopy, powder X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, and nitrogen sorption porosimetry. Varying pH conditions and temperature of the thermal treatment provided cassiterite SnO 2 nanoparticles with crystallite sizes ranging from 7.3 to 9.7 nm and Brunauer-Emmett-Teller surface areas ranging from 61 to 106 m 2 ·g -1 , acidic conditions favoring potassium cation removal. Upon exposure to a reducing gas (H 2 , CO, and volatile organic compounds such as ethanol and acetone) or oxidizing gas (NO 2 ), layers of these SnO 2 nanoparticles led to highly sensitive, reversible, and reproducible responses. The sensing results were discussed in regard to the crystallite size, specific area, valence band energy, Debye length, and chemical composition. Results highlight the impact of the counterion residuals, which affect the gas-sensing performance to an extent much higher than that of size and surface area effects. Tin dioxide nanoparticles prepared under acidic conditions and calcined in air showed the best sensing performances because of lower amount of potassium cations and higher crystallinity, despite the lower surface area.

  14. Multi-metals column adsorption of lead(II), cadmium(II) and manganese(II) onto natural bentonite clay.

    PubMed

    Alexander, Jock Asanja; Surajudeen, Abdulsalam; Aliyu, El-Nafaty Usman; Omeiza, Aroke Umar; Zaini, Muhammad Abbas Ahmad

    2017-10-01

    The present work was aimed at evaluating the multi-metals column adsorption of lead(II), cadmium(II) and manganese(II) ions onto natural bentonite. The bentonite clay adsorbent was characterized for physical and chemical properties using X-ray diffraction, X-ray fluorescence, Brunauer-Emmett-Teller surface area and cation exchange capacity. The column performance was evaluated using adsorbent bed height of 5.0 cm, with varying influent concentrations (10 mg/L and 50 mg/L) and flow rates (1.4 mL/min and 2.4 mL/min). The result shows that the breakthrough time for all metal ions ranged from 50 to 480 minutes. The maximum adsorption capacity was obtained at initial concentration of 10 mg/L and flow rate of 1.4 mL/min, with 2.22 mg/g of lead(II), 1.71 mg/g of cadmium(II) and 0.37 mg/g of manganese(II). The order of metal ions removal by natural bentonite is lead(II) > cadmium(II) > manganese(II). The sorption performance and the dynamic behaviour of the column were predicted using Adams-Bohart, Thomas, and Yoon-Nelson models. The linear regression analysis demonstrated that the Thomas and Yoon-Nelson models fitted well with the column adsorption data for all metal ions. The natural bentonite was effective for the treatment of wastewater laden with multi-metals, and the process parameters obtained from this work can be used at the industrial scale.

  15. Bentonite modification with pillarization method using metal stannum

    NASA Astrophysics Data System (ADS)

    Widjaya, Robert R.; Juwono, Ariadne L.; Rinaldi, Nino

    2017-11-01

    Clay minerals have received considerable attention in the last years because of their environmental compatibility, low cost, high selectivity, and operational simplicity. Although clays are very useful for many application in the field of catalysis, they have main disadvantage: their lack of pore volume and spesific surface area. Porosity and stability of these materials are improved by pillaring the clay layers with SnCl4, which leads to materials known as pillared clays (PILC). This research aims were to characterize the Bentonite and Sn-Bentonite as catalysts for cracking and oligomerization. The Sn-Bentonite was prepared by pillarization method with a variation in metal ratio of 5 mmol dan 10 mmol.gr-1 of bentonit. The catalyst characterized by X-ray Diffraction, X-ray Fluorescence, Fourier Transform Infra Red, Brunauer Emmett Teller, Thermogravimetric Analysis. The results showed that the Sn-Bentonite catalyst had large basal spacing and good porous structure, and the specific surface areas increased. XRF detected the Sn in the Bentonite and TGA results showed the ability Sn-Bentonite in receiving heat. FTIR test showed two type of acidity, broansted and lewis acid. The characterized results indicated that Sn-Bentonite with metal ratio 5 mmol.gr-1 better than Sn-Bentonite with metal ratio 10 mmol.gr-1, in which there was a significant increase the basal spacings, specific surface area, and pore volume. The TGA results for Sn-Bentonite appeared to be more thermally stable than Bentonite.

  16. Fabrication and photoactivity of ionic liquid-TiO2 structures for efficient visible-light-induced photocatalytic decomposition of organic pollutants in aqueous phase.

    PubMed

    Gołąbiewska, Anna; Paszkiewicz-Gawron, Marta; Sadzińska, Aleksandra; Lisowski, Wojciech; Grabowska, Ewelina; Zaleska-Medynska, Adriana; Łuczak, Justyna

    2018-01-01

    To investigate the effect of the ionic liquid (IL) chain length on the surface properties and photoactivity of TiO 2 , a series of TiO 2 microspheres have been synthesized via a solvothermal method assisted by 1-methyl-3-octadecylimidazolium chloride ([ODMIM][Cl]) and 1-methyl-3-tetradecylimidazolium chloride ([TDMIM][Cl]). All as-prepared samples were characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), diffuse reflectance spectroscopy (DRS), scanning transmission microscopy (STEM) and the Brunauer-Emmett-Teller (BET) surface area method, whereas the photocatalytic activity was evaluated by the degradation of phenol in aqueous solution under visible light irradiation (λ > 420 nm). The highest photoefficiency (four times higher than pristine TiO 2 ) was observed for the TiO 2 sample obtained in the presence of [TDMIM][Cl] for a IL to TiO 2 precursor molar ratio of 1:3. It was revealed that interactions between the ions of the ionic liquid and the surface of the growing titanium dioxide spheres results in a red-shift of absorption edge for the IL-TiO 2 semiconductors. In this regard, the direct increase of the photoactivity of IL-TiO 2 in comparison to pristine TiO 2 was observed. The active species trapping experiments indicated that O 2 •- is the main active species, created at the surface of the IL-TiO 2 material under visible-light illumination, and is responsible for the effective phenol degradation.

  17. Core-shell Fe3O4 polydopamine nanoparticles as sorbent for magnetic dispersive solid-phase extraction of copper from food samples.

    PubMed

    Yavuz, Emre; Tokalıoğlu, Şerife; Patat, Şaban

    2018-10-15

    In the present study, core-shell Fe 3 O 4 polydopamine nanoparticles were synthesized and used for the first time as an adsorbent for the vortex assisted magnetic dispersive solid phase extraction of copper from food samples. After elution, copper in the solutions was determined by FAAS. The adsorbent was characterized using X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller surface area, and zeta potential measurements. Various parameters affecting the magnetic dispersive solid-phase extraction were evaluated. The optimum pH and magnetic adsorbent amount were found to be 5 and 40 mg, respectively. Elution was made by 3 mL of 2 mol L -1 HNO 3 .The major advantage of the method is the fast equilibration during adsorption without the need for vortexing or shaking. The preconcentration factor and detection limit of the method were found to be 150 and 0.22 mg L -1 , respectively. The precision (as RSD%) and adsorption capacity of the method were 3.7% and 28 mg g -1 , respectively. The method was successfully verified by analyzing four certified reference materials (SPS-WW1 Batch 114 Wastewater, TMDA-53.3 Lake water, BCR-482 Lichen and 1573a Tomato Leaves) and by addition/recovery tests of copper standard solution in organic baby food, muesli, macaroni, honey, and milk samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

  18. Solvothermal synthesis of Bi2O3/BiVO4 heterojunction with enhanced visible-light photocatalytic performances

    NASA Astrophysics Data System (ADS)

    Ying, Wu; Jing, Wang; Yunfang, Huang; Yuelin, Wei; Zhixian, Sun; Xuanqing, Zheng; Chengkun, Zhang; Ningling, Zhou; Leqing, Fan; Jihuai, Wu

    2016-08-01

    Novel, three-dimensional, flower-like Bi2O3/BiVO4 heterojunction photocatalysts have been prepared by the combination of homogeneous precipitation and two-step solvothermal method followed by thermal solution of NaOH etching process. The as-obtained samples were fully characterized by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, Brunauer-Emmett-Teller surface area, and UV—vis diffuse-reflectance spectroscopy in detail. The crystallinity, microstructure, specific surface area, optical property and photocatalytic activity of samples greatly changed depending on solvothermal reaction time. The photocatalytic activities of samples were evaluated on the degradation of methyl orange (MO) under visible-light irradiation. The Bi2O3/BiVO4 exhibited much higher photocatalytic activities than pure BiVO4 and conventional TiO2 (P25). The result revealed that the three-dimensional heterojunction played a critical role in the separation of the electron and hole pairs and enhancement of the interfacial charge transfer efficiency, which was responsible for the enhanced photocatalytic activity. Project supported by the National Natural Science Foundation of China (Nos. 61306077, 21301060), the Fundamental Research Funds for the Central Universities (Nos. JB-ZR1109, JB-ZR1212), the National Science Foundation of Quanzhou City (No. 2014Z108), the Promotion Program for Young and Middle-aged Teachers in Science and Technology Research of Huaqiao University (No. ZQN-PY207), Discipline Innovation Team Project of Huaqiao University (No. 201320), and the Instrumental Analysis Center Huaqiao University.

  19. Simulating Picosecond X-ray Diffraction from shocked crystals by Post-processing Molecular Dynamics Calculations

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

    Kimminau, G; Nagler, B; Higginbotham, A

    2008-06-19

    Calculations of the x-ray diffraction patterns from shocked crystals derived from the results of Non-Equilibrium-Molecular-Dynamics (NEMD) simulations are presented. The atomic coordinates predicted by the NEMD simulations combined with atomic form factors are used to generate a discrete distribution of electron density. A Fast-Fourier-Transform (FFT) of this distribution provides an image of the crystal in reciprocal space, which can be further processed to produce quantitative simulated data for direct comparison with experiments that employ picosecond x-ray diffraction from laser-irradiated crystalline targets.

  20. Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

    DOE PAGES

    Fan, D.; Huang, J. W.; Zeng, X. L.; ...

    2016-05-23

    We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.« less

  1. Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

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

    Fan, D.; Luo, S. N., E-mail: sluo@pims.ac.cn; Key Laboratory of Advanced Technologies of Materials, Ministry of Education, Southwest Jiaotong University, Chengdu, Sichuan 610031

    We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; fracture is dominated by splitting cracks followed by wing cracks, and diffraction peaks are broadened likely due to mosaic spread. Our results demonstrate the potential of such multiscale measurements for studying high strain-rate phenomena at dynamic extremes.« less

  2. Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

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

    Fan, D.; Huang, J. W.; Zeng, X. L.

    We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera’s capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantifymore » lattice deformation and fracture; diffraction peak broadening is largely caused by fracture-induced strain inhomogeneity. Finally, our results demonstrate the potential of such multiscale measurements for revealing and understanding high strain-rate phenomena at dynamic extremes.« less

  3. Innovative diffraction gratings for high-resolution resonant inelastic soft x-ray scattering spectroscopy

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

    Voronov, D.L.; Warwick, T.; Gullikson, E. M.

    2016-07-27

    High-resolution Resonant Inelastic X-ray Scattering (RIXS) requires diffraction gratings with very exacting characteristics. The gratings should provide both very high dispersion and high efficiency which are conflicting requirements and extremely challenging to satisfy in the soft x-ray region for a traditional grazing incidence geometry. To achieve high dispersion one should increase the groove density of a grating; this however results in a diffraction angle beyond the critical angle range and results in drastic efficiency loss. The problem can be solved by use of multilayer coated blazed gratings (MBG). In this work we have investigated the diffraction characteristics of MBGs viamore » numerical simulations and have developed a procedure for optimization of grating design for a multiplexed high resolution imaging spectrometer for RIXS spectroscopy to be built in sector 6 at the Advanced Light Source (ALS). We found that highest diffraction efficiency can be achieved for gratings optimized for 4{sup th} or 5{sup th} order operation. Fabrication of such gratings is an extremely challenging technological problem. We present a first experimental prototype of these gratings and report its performance. High order and high line density gratings have the potential to be a revolutionary new optical element that should have great impact in the area of soft x-ray RIXS.« less

  4. Towards shot-noise limited diffraction experiments with table-top femtosecond hard x-ray sources.

    PubMed

    Holtz, Marcel; Hauf, Christoph; Weisshaupt, Jannick; Salvador, Antonio-Andres Hernandez; Woerner, Michael; Elsaesser, Thomas

    2017-09-01

    Table-top laser-driven hard x-ray sources with kilohertz repetition rates are an attractive alternative to large-scale accelerator-based systems and have found widespread applications in x-ray studies of ultrafast structural dynamics. Hard x-ray pulses of 100 fs duration have been generated at the Cu K α wavelength with a photon flux of up to 10 9 photons per pulse into the full solid angle, perfectly synchronized to the sub-100-fs optical pulses from the driving laser system. Based on spontaneous x-ray emission, such sources display a particular noise behavior which impacts the sensitivity of x-ray diffraction experiments. We present a detailed analysis of the photon statistics and temporal fluctuations of the x-ray flux, together with experimental strategies to optimize the sensitivity of optical pump/x-ray probe experiments. We demonstrate measurements close to the shot-noise limit of the x-ray source.

  5. Towards shot-noise limited diffraction experiments with table-top femtosecond hard x-ray sources

    PubMed Central

    Holtz, Marcel; Hauf, Christoph; Weisshaupt, Jannick; Salvador, Antonio-Andres Hernandez; Woerner, Michael; Elsaesser, Thomas

    2017-01-01

    Table-top laser-driven hard x-ray sources with kilohertz repetition rates are an attractive alternative to large-scale accelerator-based systems and have found widespread applications in x-ray studies of ultrafast structural dynamics. Hard x-ray pulses of 100 fs duration have been generated at the Cu Kα wavelength with a photon flux of up to 109 photons per pulse into the full solid angle, perfectly synchronized to the sub-100-fs optical pulses from the driving laser system. Based on spontaneous x-ray emission, such sources display a particular noise behavior which impacts the sensitivity of x-ray diffraction experiments. We present a detailed analysis of the photon statistics and temporal fluctuations of the x-ray flux, together with experimental strategies to optimize the sensitivity of optical pump/x-ray probe experiments. We demonstrate measurements close to the shot-noise limit of the x-ray source. PMID:28795079

  6. 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.

  7. Structure of phospholipid-cholesterol membranes: an x-ray diffraction study.

    PubMed

    Karmakar, Sanat; Raghunathan, V A

    2005-06-01

    We have studied the phase behavior of mixtures of cholesterol with dipalmitoyl phosphatidylcholine (DPPC), dimyristoyl phosphatidylcholine (DMPC), and dilauroyl phosphatidylethanolamine (DLPE), using x-ray diffraction techniques. Phosphatidylcholine (PC)-cholesterol mixtures are found to exhibit a modulated phase for cholesterol concentrations around 15 mol % at temperatures below the chain melting transition. Lowering the relative humidity from 98% to 75% increases the temperature range over which it exists. An electron density map of this phase in DPPC-cholesterol mixtures, calculated from the x-ray diffraction data, shows bilayers with a periodic height modulation, as in the ripple phase observed in many PCs in between the main- and pretransitions. However, these two phases differ in many aspects, such as the dependence of the modulation wavelength on the cholesterol content and thermodynamic stability at reduced humidities. This modulated phase is found to be absent in DLPE-cholesterol mixtures. At higher cholesterol contents the gel phase does not occur in any of these three systems, and the fluid lamellar phase is observed down to the lowest temperature studied (5 degrees C).

  8. X-ray diffraction analysis of residual stress in zirconia dental composites

    NASA Astrophysics Data System (ADS)

    Allahkarami, Masoud

    Dental restoration ceramic is a complex system to be characterized. Beside its essential biocompatibility, and pleasant appearance, it requires being mechanically strong in a catastrophic loading environment. Any design is restricted with geometry boundary and material property limits. Inspired by natural teeth, a multilayer ceramic is a smart way of achieving an enhanced restoration. Bi-layers of zirconia core covered by porcelain are known as one of the best multilayer restorations. Residual stresses may be introduced into a bi-layer dental ceramic restoration during its entire manufacturing process due to thermal expansion and elastic property mismatch. It is impossible to achieve a free of residual stresses bi-layer zirconia-porcelain restoration. The idea is to take the advantage of residual stress in design in such a way to prevent the crack initiation and progression. The hypothesis is a compressive residual stress at external contact surface would be enabling the restoration to endure a greater tensile stress. Optimizing the layers thickness, manufacturing process, and validating 3D simulations require development of new techniques of thickness, residual stresses and phase transformation measurement. In the present work, a combined mirco-tomography and finite element based method were adapted for thickness measurement. Two new 2D X-ray diffraction based techniques were adapted for phase transformation area mapping and combined phase transformation and residual stress measurement. Concerning the complex geometry of crown, an efficient method for X-ray diffraction data collection mapping on a given curved surface was developed. Finally a novel method for 3D dimensional x-ray diffraction data collection and visualization were introduced.

  9. ELECTRON MICROSCOPE AND X-RAY DIFFRACTION STUDIES ON A HOMOLOGOUS SERIES OF SATURATED PHOSPHATIDYLCHOLINES.

    PubMed

    ELBERS, P F; VERVERGAERT, P H

    1965-05-01

    Three homologous saturated phosphatidylcholines were studied by electron microscopy after tricomplex fixation. The results are compared with those obtained by x-ray diffraction analysis of the same and some other homologous compounds, in the dry crystalline state and after tricomplex fixation. By electron microscopy alternating dark and light bands are observed which are likely to correspond to phosphatide double layers. X-Ray diffraction reveals the presence of lamellar structures of regular spacing. The layer spacings obtained by both methods are in good agreement. From the electron micrographs the width of the polar parts of the double layers can be derived directly. The width of the carboxylglycerylphosphorylcholine moiety of the layers is found by extrapolating the x-ray diffraction data to zero chain length of the fatty acids. When from this width the contribution of the carboxylglyceryl part of the molecules is subtracted, again we find good agreement with the electron microscope measurements. An attempt has been made to account for the different layer spacings measured in terms of orientation of the molecules within the double layers.

  10. Quantitative analysis of crystalline pharmaceuticals in tablets by pattern-fitting procedure using X-ray diffraction pattern.

    PubMed

    Takehira, Rieko; Momose, Yasunori; Yamamura, Shigeo

    2010-10-15

    A pattern-fitting procedure using an X-ray diffraction pattern was applied to the quantitative analysis of binary system of crystalline pharmaceuticals in tablets. Orthorhombic crystals of isoniazid (INH) and mannitol (MAN) were used for the analysis. Tablets were prepared under various compression pressures using a direct compression method with various compositions of INH and MAN. Assuming that X-ray diffraction pattern of INH-MAN system consists of diffraction intensities from respective crystals, observed diffraction intensities were fitted to analytic expression based on X-ray diffraction theory and separated into two intensities from INH and MAN crystals by a nonlinear least-squares procedure. After separation, the contents of INH were determined by using the optimized normalization constants for INH and MAN. The correction parameter including all the factors that are beyond experimental control was required for quantitative analysis without calibration curve. The pattern-fitting procedure made it possible to determine crystalline phases in the range of 10-90% (w/w) of the INH contents. Further, certain characteristics of the crystals in the tablets, such as the preferred orientation, size of crystallite, and lattice disorder were determined simultaneously. This method can be adopted to analyze compounds whose crystal structures are known. It is a potentially powerful tool for the quantitative phase analysis and characterization of crystals in tablets and powders using X-ray diffraction patterns. Copyright 2010 Elsevier B.V. All rights reserved.

  11. PREFACE: XTOP 2004 -- 7th Biennial Conference on High Resolution X-Ray Diffraction and Imaging

    NASA Astrophysics Data System (ADS)

    Holý, Vaclav

    2005-05-01

    The 7th Biennial Conference on High Resolution X-Ray Diffraction and Imaging (XTOP 2004) was held in the Prague suburb of Pruhonice, Czech Republic, during 7-10 September 2004. It was organized by the Czech and Slovak Crystallographic Association in cooperation with the Institute of Physics, Academy of Sciences of the Czech Republic, Prague, Masaryk University, Brno, and Charles University, Prague. XTOP 2004 took place just after EPDIC IX (European Powder Diffraction Conference) organised in Prague by the same Association during 2-5 September 2004. The Organizing Committee was supported by an International Programme Committee including about 20 prominent scientists from several European and overseas countries, whose helpful suggestions for speakers are acknowledged. The conference was sponsored by the International Union of Crystallography and by several industrial sponsors; this sponsorship allowed us to support about 20 students and young scientists. In total, 147 official delegates and 8 accompanying persons from 16 countries of three continents attended our conference. The scientific programme of the conference was divided into 11 half-day sessions and 2 poster sessions. The participants presented 147 accepted contributions; of these 9 were 45-minute long invited talks, 34 were 20-minute oral presentations and 104 were posters. All posters were displayed for the whole meeting to ensure maximum exposure and interaction between delegates. We followed the very good experience from the previous conference, XTOP 2002, and also organized pre-conference tutorial lectures presented by experts in the field: `Imaging with hard synchrotron radiation' (J Härtwig, Grenoble), `High-resolution x-ray diffractometry: determination of strain and composition' (J Stangl, Linz), `X-ray grazing-incidence scattering from surfaces and nanostructures' (U Pietsch, Potsdam) and `Hard x-ray optics' (J Hrdý, Prague). According to the recommendation of the International Program Committee

  12. Molybdenum cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures

    NASA Astrophysics Data System (ADS)

    Matsuda, Kazuhiro; Tamura, Kozaburo; Katoh, Masahiro; Inui, Masanori

    2004-03-01

    We have developed a sample cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures. All parts of the cell are made of molybdenum which is resistant to the chemical corrosion of alkali metals. Single crystalline molybdenum disks electrolytically thinned down to 40 μm were used as the walls of the cell through which x rays pass. The crystal orientation of the disks was controlled in order to reduce the background from the cell. All parts of the cell were assembled and brazed together using a high-temperature Ru-Mo alloy. Energy dispersive x-ray diffraction measurements have been successfully carried out for fluid rubidium up to 1973 K and 16.2 MPa. The obtained S(Q) demonstrates the applicability of the molybdenum cell to x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures.

  13. Inorganic pyrophosphatase crystals from Thermococcus thioreducens for X-ray and neutron diffraction.

    PubMed

    Hughes, Ronny C; Coates, Leighton; Blakeley, Matthew P; Tomanicek, Steve J; Langan, Paul; Kovalevsky, Andrey Y; García-Ruiz, Juan M; Ng, Joseph D

    2012-12-01

    Inorganic pyrophosphatase (IPPase) from the archaeon Thermococcus thioreducens was cloned, overexpressed in Escherichia coli, purified and crystallized in restricted geometry, resulting in large crystal volumes exceeding 5 mm3. IPPase is thermally stable and is able to resist denaturation at temperatures above 348 K. Owing to the high temperature tolerance of the enzyme, the protein was amenable to room-temperature manipulation at the level of protein preparation, crystallization and X-ray and neutron diffraction analyses. A complete synchrotron X-ray diffraction data set to 1.85 Å resolution was collected at room temperature from a single crystal of IPPase (monoclinic space group C2, unit-cell parameters a=106.11, b=95.46, c=113.68 Å, α=γ=90.0, β=98.12°). As large-volume crystals of IPPase can be obtained, preliminary neutron diffraction tests were undertaken. Consequently, Laue diffraction images were obtained, with reflections observed to 2.1 Å resolution with I/σ(I) greater than 2.5. The preliminary crystallographic results reported here set in place future structure-function and mechanism studies of IPPase.

  14. Highly sensitive analysis of polycyclic aromatic hydrocarbons in environmental water with porous cellulose/zeolitic imidazolate framework-8 composite microspheres as a novel adsorbent coupled with high-performance liquid chromatography.

    PubMed

    Liang, Xiaotong; Liu, Shengquan; Zhu, Rong; Xiao, Lixia; Yao, Shouzhuo

    2016-07-01

    In this work, novel cellulose/zeolitic imidazolate frameworks-8 composite microspheres have been successfully fabricated and utilized as sorbent for environmental polycyclic aromatic hydrocarbons efficient extraction and sensitive analysis. The composite microspheres were synthesized through the in situ hydrothermal growth of zeolitic imidazolate frameworks-8 on cellulose matrix, and exhibited favorable hierarchical structure with chemical composition as assumed through scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction patterns, and Brunauer-Emmett-Teller surface areas characterization. A robust and highly efficient method was then successfully developed with as-prepared composite microspheres as novel solid-phase extraction sorbent with optimum extraction conditions, such as sorbent amount, sample volume, extraction time, desorption conditions, volume of organic modifier, and ionic strength. The method exhibited high sensitivity with low limit of detection down to 0.1-1.0 ng/L and satisfactory linearity with correlation coefficients ranging from 0.9988 to 0.9999, as well as good recoveries of 66.7-121.2% with relative standard deviations less than 10% for environmental polycyclic aromatic hydrocarbons analysis. Thus, our method was convenient and efficient for polycyclic aromatic hydrocarbons extraction and detection, potential for future environmental water samples analysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Novel development of nanocrystalline kesterite Cu2ZnSnS4 thin film with high photocatalytic activity under visible light illumination

    NASA Astrophysics Data System (ADS)

    Apostolopoulou, Andigoni; Mahajan, Sandip; Sharma, Ramphal; Stathatos, Elias

    2018-01-01

    Cu2ZnSnS4 (CZTS) represents a promising p-type direct band gap semiconductor with large absorption coefficient in the visible region of solar light. In the present study, a kesterite CZTS nanocrystalline film, with high purity, was successfully synthesized via the combination of successive ionic layer adsorption and reaction (SILAR) and chemical bath deposition (CBD) technique. The morphology and structural properties of the CZTS films were characterized by FE-SEM microscopy, porosimetry in terms of Brunauer-Emmett-Teller (BET) technique, X-ray diffraction and Raman spectroscopy. The as-prepared films under mild heat treatment at 250 °C in the presence of sulfur atmosphere exhibited fine nanostructure with 35 nm average particle size, high specific surface area of 53 m2/g and 9 nm pore diameter. The photocatalytic activity of the films was examined to the degradation of Basic Blue 41 (BB-41) and Acid Orange 8 (AO-8) organic azo dyes under visible light irradiation, demonstrating 97.5% and 70% discoloration for BB-41 and AO-8 respectively. Reusability of the CZTS films was also tested proving good stability over several repetitions. The reduction of photocatalyst's efficiency after three successive repetitions didn't exceed 5.6% and 8.5% for BB-41 and AO-8 respectively.

  16. Characterization of organo-modified bentonite sorbents: The effect of modification conditions on adsorption performance

    NASA Astrophysics Data System (ADS)

    Parolo, María E.; Pettinari, Gisela R.; Musso, Telma B.; Sánchez-Izquierdo, María P.; Fernández, Laura G.

    2014-11-01

    The organic modification of a natural bentonite was evaluated using two methods: exchanging the interlayer cations by hexadecyltrimethylammonium (HDTMA) and grafting with vinyltrimethoxysilane (VTMS) and γ-methacryloyloxy propyl trimethoxysilane (TMSPMA) on montmorillonite surface. The physicochemical characterization of all materials was made by X-ray diffraction (XRD), IR spectroscopy, thermogravimetric analysis (TGA) and Brunauer-Emmett-Teller (BET) surface area techniques. HDTMA cations and organosilanes were intercalated into the interlayer space of montmorillonite, as deduced from the increase of the basal spacing. IR spectroscopy, TGA and BET area give evidence of successful organic modification. The studies show a decrease in the IR absorption band intensity at 3465 cm-1 with surfactant modification, and also a decrease of mass loss due to adsorbed water observed in two samples: the organoclay and functionalized bentonites, which are evidences of a lower interlayer hydrophilicity. The efficiency of aniline removal onto natural bentonite, organobentonite and functionalized bentonites from aqueous solutions was evaluated. Aniline sorption on natural bentonite was studied using batch experiments, XRD and IR spectroscopy. The hydrophobic surface of organobentonite and functionalized bentonites increased the retention capacity for nonionic organic substances such as aniline on bentonites. The sorption properties of modified bentonite, through different modification methods, enhanced the potential industrial applications of bentonites in water decontamination.

  17. Hydrogen storage studies on palladium-doped carbon materials (AC, CB, CNMs) @ metal-organic framework-5.

    PubMed

    Viditha, V; Srilatha, K; Himabindu, V

    2016-05-01

    Metal organic frameworks (MOFs) are a rapidly growing class of porous materials and are considered as best adsorbents for their high surface area and extraordinary porosity. The MOFs are synthesized by using various chemicals like triethylamine, terepthalic acid, zinc acetate dihydrate, chloroform, and dimethylformamide (DMF). Synthesized MOFs are intercalated with palladium/activated carbon, carbon black, and carbon nanomaterials by chemical reduction method for the purpose of enhancing the hydrogen adsorption capacities. We have observed that the palladium doped activated carbon on MOF-5 showed high hydrogen storage capacity. This may be due to the affinity of the palladium toward hydrogen molecule. The samples are characterized by X-ray diffraction, scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) surface area analysis. We have observed a clear decrease in the BET surface area and pore volume. The obtained results show a better performance for the synthesized sample. To our best knowledge, no one has reported the work on palladium-doped carbon materials (activated carbon, carbon black, carbon nanomaterials) impregnated to the metal-organic framework-5. We have attempted to synthesize carbon nanomaterials using indigenously fabricated chemical vapor deposition (CVD) unit as a support. We have observed an increase in the hydrogen storage capacities.

  18. Generation of highly stable and active strong base sites on organized nano-porous alumina by calcium oxide

    NASA Astrophysics Data System (ADS)

    Tarlani, Aliakbar; Zarabadi, Mir Pouyan

    2013-02-01

    In a new approach, strong basic sites has been successfully prepared by loading of calcium nitrate (Ca) on organized nano-porous alumina (ONPA). The prepared CaONPAs were characterized by low-angle X-ray diffraction (XRD), N2 adsorption-desorption isotherms (Brunauer-Emmett-Teller (BET)-Barret-Joyner-Halenda (BJH)), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). Measuring of the amount of the basic sites and the basicity was carried out by titration method, temperature-programmed desorption (TPD-CO2) and Hammett indicators. Resistance of the basic sites was also tested by washing with water. N2 sorption measurements showed that supporting of the calcium nitrate on ONPA can lead to the bimodal porosity at lower loading. BET surface area of the bare ONPA was 212 m2/g which decreased to 111 m2/g for the 25% of loading of Ca (25CaONPA). The results pointed out that CaONPA samples have basicity between 18.4 < H_ < 22 for 15 and 25% of loadings and well-preserved of the basicity after washing with water especially for 5 and 15% samples. Also no crystalline phase of CaO was observed for 25CaONPA which was calcined at 600 °C.

  19. Preparation of chitosan/MCM-41-PAA nanocomposites and the adsorption behaviour of Hg(II) ions

    NASA Astrophysics Data System (ADS)

    Fu, Yong; Huang, Yue; Hu, Jianshe

    2018-03-01

    A novel functional hybrid mesoporous composite material (CMP) based on chitosan and MCM-41-PAA was reported and its application as an excellent adsorbent for Hg(II) ions was also investigated. Innovatively, MCM-41-PAA was prepared by using diatomite and polyacrylic acid (PAA) with integrated polymer-silica hybrid frameworks, and then CMP was fabricated by introducing MCM-41-PAA to chitosan using glutaraldehyde as a cross-linking agent. The structure and morphology of CMP were characterized by X-ray diffraction, Fourier transform infrared spectra, thermogravimetric analysis, scanning electron microscopy and Brunauer-Emmett-Teller measurements. The results showed that the CMP possessed multifunctional groups such as -OH, -COOH and -NH2 with large specific surface area. Adsorption behaviour of Hg(II) ions onto CMP was fitted better by the pseudo-second-order kinetic model and the Langmuir model when the initial Hg(II) concentration, pH, adsorption temperature and time were 200 mg l-1, 4, 298 K and 120 min, respectively, as the optimum conditions. The corresponding maximum adsorption capacity could reach 164 mg g-1. According to the thermodynamic parameters determined such as free energy, enthalpy and entropy, the adsorption process of Hg(II) ions was spontaneous endothermic adsorption.

  20. Novel porous CuO microrods: synthesis, characterization, and their photocatalysis property

    NASA Astrophysics Data System (ADS)

    Huang, Jiarui; Fu, Guijun; Shi, Chengcheng; Wang, Xinyue; Zhai, Muheng; Gu, Cuiping

    2014-09-01

    Porous copper oxide microrods have been synthesized via calcining copper glycinate monohydrate microrod precursor which was prepared in mild conditions without any template or additive. Several techniques, such as X-ray diffraction, field emission scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, and Brunauer-Emmett-Teller (BET) N2 adsorption-desorption analyses, were used to characterize the structure and morphology of the products. Scanning electron microscopy (SEM) analyses show that the precursor consists of a large quantity of uniform rod-like micro/nanostructures with typical lengths in the range of 25-40 μm and diameters in the range of 0.1-0.35 μm. The microrod-like precursors transformed into porous microrod products after calcination at 450 °C in flow air for 2 h. The BET surface area of the porous CuO microrods was calculated to be 8.5 m² g-1. In addition, the obtained porous CuO microrods were used as catalysts to photodegrade rhodamine B (RhB), methyl orange, methylene blue, eosin B, and p-nitrophenol. Compared with commercial CuO powders, the as-prepared porous CuO microrods exhibit superior properties on photocatalytic decomposition of RhB due to their porous hierarchical structures.

  1. Enhanced Defluoridation Capacity From Aqueous Media via Hydroxyapatite Decorated With Carbon Nanotube.

    PubMed

    Tang, Qingzi; Duan, Tongdan; Li, Peng; Zhang, Ping; Wu, Daishe

    2018-01-01

    In this work, the potential of a novel hydroxyapatite decorated with carbon nanotube composite (CNT-HAP) for fluoride removal was investigated. The synthesized CNT-HAP composite was systematically characterized by X-ray diffraction(XRD), Fourier Transform infrared spectroscopy(FTIR), scanning electron microscope (SEM) and Brunauer-Emmett-Teller(BET). Batch adsorption experiments were conducted to investigate the defluorination capacity of CNT-HAP. The CNT-HAP composite has a maximum adsorption capacity of 11.05 mg·g -1 for fluoride, and the isothermal adsorption data were fitted by the Freundlich model to calculate the thermodynamic parameters. Thermodynamic analysis implies that the adsorption of fluoride on CNT-HAP is a spontaneous process. Furthermore, the adsorption of fluoride follows pseudo-second-order model. The effects of solution pH, co-existing anions and reaction temperature on defluorination efficiency were examined to optimize the operation conditions for fluoride adsorption. It is found that the optimized pH-value for fluoride removal by CNT-HAP composite is 6. In addition, among five common anions studied in this work, the presence of [Formula: see text] and [Formula: see text] could considerably affect the fluoride removal by CNT-HPA in aqueous media. Finally, the underlying mechanism for the fluoride removal by CNT-HAP is analyzed, and an anion exchange process is proposed.

  2. Surface modification of TiO2 nanotubes by grafting with APTS coupling agents

    NASA Astrophysics Data System (ADS)

    Phan Duong, Hong; Le, Minh Duc; Dao, Hung Cuong; Chen, Chia-Yun

    2017-10-01

    Titanium dioxide nanotubes (TNTs) have been considered the promising nanostructures employed for many practical applications such as biomedical, photonic and optoelectronic devices. Nevertheless, strong aggregation of TNTs within various aqueous media significantly hindered their practical utilizations and the capability of dispersing TNTs in the desired solvents are urgent to be improved. Therefore, in this study, the methodic investigations have been performed on the grafted modification of 3-aminopropyl triethoxysilane (APTS) on the surfaces of synthesized TNTs. A preliminary study was carried out to evaluate the influences of key parameters, including the concentrations of coupling agents, temperatures and the reaction durations, on the grafting efficiency of the aminosilane using Statistical design of experiments (DoE) methodology. TNTs with approximately 10-20 nm in diameter were prepared with the controlled hydrothermal treatment of commercialized P25 particles. The obtained products were revealed by the modern physicochemical systems including x-ray diffraction (XRD), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) analysis. The additions of silane agent, reaction temperature and time have been adjusted to reveal the influences of the grafting efficiency (from 2.5 to 7.8 wt %) by thermal gravimetric analysis (TGA). Analysis of Fourier transform infrared spectroscopy (FTIR) has confirmed the successful link of Ti-O-Si chemical bonds on the grafted TNTs.

  3. Preparation of new diatomite-chitosan composite materials and their adsorption properties and mechanism of Hg(II).

    PubMed

    Fu, Yong; Xu, Xiaoxu; Huang, Yue; Hu, Jianshe; Chen, Qifan; Wu, Yaoqing

    2017-12-01

    A new composite absorbent with multifunctional and environmental-friendly structures was prepared using chitosan, diatomite and polyvinyl alcohol as the raw materials, and glutaraldehyde as a cross-linking agent. The structure and morphology of the composite absorbent, and its adsorption properties of Hg(II) in water were characterized with Fourier transform infrared (FT-IR) spectra, scanning electron microscope (SEM), X-ray diffraction (XRD), Brunauer Emmett Teller (BET) measurements and ultraviolet-visible (UV-Vis) spectra. The effect of the pH value and contact time on the removal rate and absorbance of Hg(II) was discussed. The adsorption kinetic model and static adsorption isotherm and regeneration of the obtained composite absorbent were investigated. The results indicated that the removal of Hg(II) on the composite absorbent followed a rapid adsorption for 50 min, and was close to the adsorption saturation after 1 h, which is in accord with the Langmuir adsorption isotherm model and the pseudo-second-order kinetic model. When the pH value, contact time and the mass of the composite absorbent was 3, 1 h and 100 mg, respectively, the removal rate of Hg(II) on the composite absorbent reached 77%, and the maximum adsorption capacity of Hg(II) reached 195.7 mg g -1 .

  4. Preparation of new diatomite–chitosan composite materials and their adsorption properties and mechanism of Hg(II)

    PubMed Central

    Fu, Yong; Xu, Xiaoxu; Huang, Yue; Hu, Jianshe; Chen, Qifan; Wu, Yaoqing

    2017-01-01

    A new composite absorbent with multifunctional and environmental-friendly structures was prepared using chitosan, diatomite and polyvinyl alcohol as the raw materials, and glutaraldehyde as a cross-linking agent. The structure and morphology of the composite absorbent, and its adsorption properties of Hg(II) in water were characterized with Fourier transform infrared (FT-IR) spectra, scanning electron microscope (SEM), X-ray diffraction (XRD), Brunauer Emmett Teller (BET) measurements and ultraviolet–visible (UV–Vis) spectra. The effect of the pH value and contact time on the removal rate and absorbance of Hg(II) was discussed. The adsorption kinetic model and static adsorption isotherm and regeneration of the obtained composite absorbent were investigated. The results indicated that the removal of Hg(II) on the composite absorbent followed a rapid adsorption for 50 min, and was close to the adsorption saturation after 1 h, which is in accord with the Langmuir adsorption isotherm model and the pseudo-second-order kinetic model. When the pH value, contact time and the mass of the composite absorbent was 3, 1 h and 100 mg, respectively, the removal rate of Hg(II) on the composite absorbent reached 77%, and the maximum adsorption capacity of Hg(II) reached 195.7 mg g−1. PMID:29308226

  5. Optimal condition for fabricating superhydrophobic Aluminum surfaces with controlled anodizing processes

    NASA Astrophysics Data System (ADS)

    Saffari, Hamid; Sohrabi, Beheshteh; Noori, Mohammad Reza; Bahrami, Hamid Reza Talesh

    2018-03-01

    A single step anodizing process is used to produce micro-nano structures on Aluminum (1050) substrates with sulfuric acid as electrolyte. Therefore, surface energy of the anodized layer is reduced using stearic acid modification. Undoubtedly, effects of different parameters including anodizing time, electrical current, and type and concentration of electrolyte on the final contact angle are systemically studied and optimized. Results show that anodizing current of 0.41 A, electrolyte (sulfuric acid) concentration of 15 wt.% and anodizing time of 90 min are optimal conditions which give contact angle as high as 159.2° and sliding angle lower than 5°. Moreover, the study reveals that adding oxalic acid to the sulfuric acid cannot enhance superhydrophobicity of the samples. Also, scanning electron microscopy images of samples show that irregular (bird's nest) structures present on the surface instead of high-ordered honeycomb structures expecting from normal anodizing process. Additionally, X-ray diffraction analysis of the samples shows that only amorphous structures present on the surface. The Brunauer-Emmett-Teller (BET) specific surface area of the anodized layer is 2.55 m2 g-1 in optimal condition. Ultimately, the surface keeps its hydrophobicity in air and deionized water (DIW) after one week and 12 weeks, respectively.

  6. Removal of dibutyl phthalate from aqueous environments using a nanophotocatalytic Fe, Ag-ZnO/VIS-LED system: modeling and optimization.

    PubMed

    Akbari-Adergani, B; Saghi, M H; Eslami, A; Mohseni-Bandpei, A; Rabbani, M

    2018-06-01

    An (Fe, Ag) co-doped ZnO nanostructure was synthesized by a simple chemical co-precipitation method and used for the degradation of dibutyl phthalate (DBP) in aqueous solution under visible light-emitting diode (LED) irradiation. (Fe, Ag) co-doped ZnO nanorods were characterized by powder X-ray diffraction, Fourier transform infrared spectroscopy, UV-VIS diffuse reflectance spectroscopy, elemental mapping, Field emission scanning electron microscopy, transmission electron microscope and Brunauer-Emmett-Teller surface area analysis. A Central Composite Design was used to optimize the reaction parameters for the removal of DBP by the (Fe, Ag) co-doped ZnO nanorods. The four main reaction parameters optimized in this study were the following: pH, time of radiation, concentration of the nanorods and initial DBP concentration. The interaction between the four parameters was studied and modeled using the Design Expert 10 software. A maximum reduction of 95% of DBP was achieved at a pH of 3, a photocatalyst concentration of 150 mg L -1 and a DBP initial DBP concentration of 15 mg L -1 . The results showed that the (Fe, Ag) co-doped ZnO nanorods under low power LED irradiation can be used as an effective photocatalyst for the removal of DBP from aqueous solutions.

  7. Enhanced reactivity of nanoscale iron particles through a vacuum annealing process

    NASA Astrophysics Data System (ADS)

    Riba, Olga; Barnes, Robert J.; Scott, Thomas B.; Gardner, Murray N.; Jackman, Simon A.; Thompson, Ian P.

    2011-10-01

    A reactivity study was undertaken to compare and assess the rate of dechlorination of chlorinated aliphatic hydrocarbons (CAHs) by annealed and non-annealed nanoscale iron particles. The current study aims to resolve the uncertainties in recently published work studying the effect of the annealing process on the reduction capability of nanoscale Fe particles. Comparison of the normalized rate constants (m2/h/L) obtained for dechlorination reactions of trichloroethene (TCE) and cis-1,2-dichloroethene (cis-1,2-DCE) indicated that annealing nanoscale Fe particles increases their reactivity 30-fold. An electron transfer reaction mechanism for both types of nanoscale particles was found to be responsible for CAH dechlorination, rather than a reduction reaction by activated H2 on the particle surface (i.e., hydrogenation, hydrogenolysis). Surface analysis of the particulate material using X-ray diffraction (XRD) and transmission electron microscopy (TEM) together with surface area measurement by Brunauer, Emmett, Teller (BET) indicate that the vacuum annealing process decreases the surface area and increases crystallinity. BET surface area analysis recorded a decrease in nanoscale Fe particle surface area from 19.0 to 4.8 m2/g and crystallite dimensions inside the particle increased from 8.7 to 18.2 nm as a result of annealing.

  8. Preparation of CaO/Fly ash as a catalyst inhibitor for transesterification process off palm oil in biodiesel production

    NASA Astrophysics Data System (ADS)

    Helwani, Z.; Fatra, W.; Saputra, E.; Maulana, R.

    2018-03-01

    A palm fly ash supported calcium oxide (CaO) catalyst was prepared and used in transesterification from off-grade palm oil for biodiesel production. The catalyst synthesized by loading CaO of calcium nitrate tetrahydrate (Ca(NO3)2.4H2O) into fly ash through impregnation method. The optimum catalyst preparation conditions were determined by influence of calcination temperature and weight ratio of Ca(NO3)2.4H2O and fly ash. Catalyst with highest catalytic activity was achieved when calcined at 800 °C and proportion of Ca(NO3)2.4H2O to fly ash is 80:20. Under the conditions of oil : methanol ratio of 1:6, catalyst dosage of 6 wt% and temperature of 70 °C for 2 h, the biodiesel yield reaches to 71.77%. CaO, SiO2, Ca(OH)2 and Ca2SiO4 were found in the catalyst through X-ray diffraction (XRD) while the basic strength of the catalyst H_ in the range 9.3 – 11. Surface area of the developed catalyst is 24.342 m2/g through Brunauer-Emmett-Teller (BET). Characteristics of biodiesel such as density, kinematic viscosity, acid value, flash point has been matched with standard for biodiesel specification of Indonesia.

  9. Activated carbon coated palygorskite as adsorbent by activation and its adsorption for methylene blue.

    PubMed

    Zhang, Xianlong; Cheng, Liping; Wu, Xueping; Tang, Yingzhao; Wu, Yucheng

    2015-07-01

    An activation process for developing the surface and porous structure of palygorskite/carbon (PG/C) nanocomposite using ZnCl2 as activating agent was investigated. The obtained activated PG/C was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field-emission scanning electron microscopy (SEM), and Brunauer-Emmett-Teller analysis (BET) techniques. The effects of activation conditions were examined, including activation temperature and impregnation ratio. With increased temperature and impregnation ratio, the collapse of the palygorskite crystal structure was found to accelerate and the carbon coated on the surface underwent further carbonization. XRD and SEM data confirmed that the palygorskite structure was destroyed and the carbon structure was developed during activation. The presence of the characteristic absorption peaks of CC and C-H vibrations in the FTIR spectra suggested the occurrence of aromatization. The BET surface area improved by more than 11-fold (1201 m2/g for activated PG/C vs. 106 m2/g for PG/C) after activation, and the material appeared to be mainly microporous. The maximum adsorption capacity of methylene blue onto the activated PG/C reached 351 mg/g. The activated PG/C demonstrated better compressive strength than activated carbon without palygorskite clay. Copyright © 2015. Published by Elsevier B.V.

  10. Synthesis and Electrochemical Analyses of Manganese Oxides for Super-Capacitors.

    PubMed

    Kim, Taewoo; Hwang, Hyein; Jang, Jaeyong; Park, Inyeong; Shim, Sang Eun; Baeck, Sung-Hyeon

    2015-11-01

    δ-Phase and α-phase manganese oxides were prepared using a hydrothermal method and their electrochemical properties were characterized. The influence of calcination temperature on the properties of manganese oxides was studied. Crystallinities were studied by X-ray diffraction, and scanning and transmission electron microscopy were utilized to examine morphologies. Average pore sizes and specific surface areas of samples were analyzed using the Barret-Joyner-Halenda and Brunauer-Emmett-Teller methods, respectively. After calcination in the range 300 degrees C to 600 degrees C, changes in morphology and crystallinity were observed. The flower-like shape of as synthesized samples became nanorod-like and the δ-phase changed to the α-phase. These changes may have been due to the removal of water during calcination. Furthermore, a transition stage in which the two phases coexisted was observed. Synthesized manganese oxides were mixed with carbon by sonification, to increase electric conductivity and to induce a synergistic effect between pseudo-capacitor and electric double layer capacitor (EDLC). Specific capacitances and rate durability of each composite were investigated by cyclic voltammetry in 1 M Na2SO4 electrolyte at different scan rates. MnO2 calcined at 400 degrees C exhibited the highest capacitance, probably due to its high surface area and more porous structure.

  11. Performance of MnO2 Crystallographic Phases in Rechargeable Lithium-Air Oxygen Cathode

    NASA Astrophysics Data System (ADS)

    Oloniyo, Olubukun; Kumar, Senthil; Scott, Keith

    2012-05-01

    Manganese dioxide (MnO2) has been shown to be effective for improving the efficiency of cathodes in lithium-air cells. Different crystallographic phases including α-, β-, and γ-MnO2 nanowires, α-MnO2 nanospheres, and α-MnO2 nanowires on carbon ( α-MnO2/C) were synthesized using the hydrothermal method. Their physical properties were examined using x-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) surface area measurements, and scanning electron microscopy (SEM) and found to be in agreement with the literature. Electrochemical properties of the synthesized catalyst particles were investigated by fabricating cathodes and testing them in a lithium-air cell with lithium hexafluorophosphate in propylene carbonate (LiPF6/PC) and tetra(ethylene glycol)dimethyl ether (LiTFSi/TEGDME) electrolytes. α-MnO2 had the highest discharge capacity in the LiTFSi/TEGDME electrolyte (2500 mAh/g), whilst α-MnO2/C in LiPF6/PC showed a significantly higher discharge capacity of 11,000 mAh/g based on total mass of the catalytic cathode. However, the latter showed poor capacity retention compared with γ-MnO2 nanowires, which was stable for up to 30 cycles. The reported discharge capacity is higher than recorded in previous studies on lithium-air cells.

  12. Double-shell Fe2O3 hollow box-like structure for enhanced photo-Fenton degradation of malachite green dye

    NASA Astrophysics Data System (ADS)

    Jiang, De Bin; Liu, Xiaoying; Xu, Xuan; Zhang, Yu Xin

    2018-01-01

    In this work we demonstrate the synthesis of novel Fe2O3 nanosheets with double-shell hollow morphology by replica molding from diatomite framework. The nanostructures of Fe2O3 nanosheets were examined by focused-ion-beam scanning electron microscopy (FIB/SEM), X-ray diffraction spectroscopy (XRD), Brunauer-Emmett-Teller (BET) specific surface area measurements and Fourier transform infrared (FT-IR) spectroscopy. The results reveal that (1) Pure Fe2O3 nanosheets were successfully obtained; (2) The double-shell Fe2O3 hollow structure achieved via the NaOH etching silica method was observed; (3) Fe2O3 nanosheets possessed uniformly distributed porous nanosheets. Such structural features enlarged the specific surface area of Fe2O3 nanosheets and led to more catalytic active sites. In the heterogeneous photo-Fenton reaction, the double-shell Fe2O3 hollow morphology exhibited excellent catalytic capability for the degradation of malachite green (MG) at circumneutral pH condition. Under optimum condition, MG solution was almost completely decolorized in 60 min (99.9%). The Fe2O3 nanosheets also showed good stability and recyclability, demonstrating great potential as a promising photo-Fenton catalyst for the effective degradation of MG dye in wastewater.

  13. Removal of elemental Mercury from flue gas using wheat straw chars modified by K2FeO4 reagent.

    PubMed

    Zhou, Jianfei; Liu, Yangxian; Pan, Jianfeng

    2017-12-01

    In this article, wheat straw (WS) char, a common agricultural waste and renewable biomass, was pyrolyzed and then modified by K 2 FeO 4 reagent to develop an efficient sorbent for removal of Hg 0 from flue gas. Brunauer-Emmett-Teller, scanning electron microscopy with energy spectrum and X-ray diffraction (XRD) were employed to characterize the sorbents. The effects of K 2 FeO 4 loading, reaction temperature, Hg 0 inlet concentration and concentrations of gas mixtures O 2 , NO and SO 2 in flue gas on Hg 0 removal were investigated in a fixed-bed reactor. The results show that K 2 FeO 4 -impregnation can improve pore structure of WS char and produce new active sites, which significantly enhance Hg 0 removal. Increasing Hg 0 inlet concentration significantly decreases Hg 0 removal efficiency. O 2 in flue gas promotes Hg 0 oxidation by replenishing the oxygen groups on the surface of modified chars. The presence of NO obviously promotes Hg 0 removal since it can oxidize Hg 0 to Hg(NO 3 ) 2 . SO 2 in flue gas significantly decreases Hg 0 removal efficiency due to the competition adsorption between SO 2 and Hg 0 . The increase in reaction temperature has a dual impact on Hg 0 removal.

  14. Performance of selective catalytic reduction of NO with NH3 over natural manganese ore catalysts at low temperature.

    PubMed

    Wang, Tao; Zhu, Chengzhu; Liu, Haibo; Xu, Yongpeng; Zou, Xuehua; Xu, Bin; Chen, Tianhu

    2018-02-01

    Natural manganese ore catalysts for selective catalytic reduction (SCR) of NO with NH 3 at low temperature in the presence and absence of SO 2 and H 2 O were systematically investigated. The physical and chemical properties of catalysts were characterized by X-ray diffraction, Brunauer-Emmett-Teller (BET) specific surface area, NH 3 temperature-programmed desorption (NH 3 -TPD) and NO-TPD methods. The results showed that natural manganese ore from Qingyang of Anhui Province had a good low-temperature activity and N 2 selectivity, and it could be a novel catalyst in terms of stability, good efficiency, good reusability and lower cost. The NO conversion exceeded 85% between 150°C and 300°C when the initial NO concentration was 1000 ppm. The activity was suppressed by adding H 2 O (10%) or SO 2 (100 or 200 ppm), respectively, and its activity could recover while the SO 2 supply is cut off. The simultaneous addition of H 2 O and SO 2 led to the increase of about 100% in SCR activity than bare addition of SO 2 . The formation of the amorphous MnO x , high concentration of lattice oxygen and surface-adsorbed oxygen groups and a lot of reducible species as well as adsorption of the reactants brought about excellent SCR performance and exhibited good SO 2 and H 2 O resistance.

  15. Rapid feedback of chemical vapor deposition growth mechanisms by operando X-ray diffraction

    DOE PAGES

    Martin, Aiden A.; Depond, Philip J.; Bagge-Hansen, Michael; ...

    2018-03-14

    An operando x-ray diffraction system is presented for elucidating optimal laser assisted chemical vapor deposition growth conditions. The technique is utilized to investigate deposition dynamics of boron-carbon materials using trimethyl borate precursor. Trimethyl borate exhibits vastly reduced toxicological and flammability hazards compared to existing precursors, but has previously not been applied to boron carbide growth. Crystalline boron-rich carbide material is produced in a narrow growth regime on addition of hydrogen during the growth phase at high temperature. Finally, the use of the operando x-ray diffraction system allows for the exploration of highly nonequilibrium conditions and rapid process control, which aremore » not possible using ex situ diagnostics.« less

  16. Rapid feedback of chemical vapor deposition growth mechanisms by operando X-ray diffraction

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

    Martin, Aiden A.; Depond, Philip J.; Bagge-Hansen, Michael

    An operando x-ray diffraction system is presented for elucidating optimal laser assisted chemical vapor deposition growth conditions. The technique is utilized to investigate deposition dynamics of boron-carbon materials using trimethyl borate precursor. Trimethyl borate exhibits vastly reduced toxicological and flammability hazards compared to existing precursors, but has previously not been applied to boron carbide growth. Crystalline boron-rich carbide material is produced in a narrow growth regime on addition of hydrogen during the growth phase at high temperature. Finally, the use of the operando x-ray diffraction system allows for the exploration of highly nonequilibrium conditions and rapid process control, which aremore » not possible using ex situ diagnostics.« less

  17. 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.

  18. A new theory for X-ray diffraction

    PubMed Central

    Fewster, Paul F.

    2014-01-01

    This article proposes a new theory of X-ray scattering that has particular relevance to powder diffraction. The underlying concept of this theory is that the scattering from a crystal or crystallite is distributed throughout space: this leads to the effect that enhanced scatter can be observed at the ‘Bragg position’ even if the ‘Bragg condition’ is not satisfied. The scatter from a single crystal or crystallite, in any fixed orientation, has the fascinating property of contributing simultaneously to many ‘Bragg positions’. It also explains why diffraction peaks are obtained from samples with very few crystallites, which cannot be explained with the conventional theory. The intensity ratios for an Si powder sample are predicted with greater accuracy and the temperature factors are more realistic. Another consequence is that this new theory predicts a reliability in the intensity measurements which agrees much more closely with experimental observations compared to conventional theory that is based on ‘Bragg-type’ scatter. The role of dynamical effects (extinction etc.) is discussed and how they are suppressed with diffuse scattering. An alternative explanation for the Lorentz factor is presented that is more general and based on the capture volume in diffraction space. This theory, when applied to the scattering from powders, will evaluate the full scattering profile, including peak widths and the ‘background’. The theory should provide an increased understanding of the reliability of powder diffraction measurements, and may also have wider implications for the analysis of powder diffraction data, by increasing the accuracy of intensities predicted from structural models. PMID:24815975

  19. A new theory for X-ray diffraction.

    PubMed

    Fewster, Paul F

    2014-05-01

    This article proposes a new theory of X-ray scattering that has particular relevance to powder diffraction. The underlying concept of this theory is that the scattering from a crystal or crystallite is distributed throughout space: this leads to the effect that enhanced scatter can be observed at the `Bragg position' even if the `Bragg condition' is not satisfied. The scatter from a single crystal or crystallite, in any fixed orientation, has the fascinating property of contributing simultaneously to many `Bragg positions'. It also explains why diffraction peaks are obtained from samples with very few crystallites, which cannot be explained with the conventional theory. The intensity ratios for an Si powder sample are predicted with greater accuracy and the temperature factors are more realistic. Another consequence is that this new theory predicts a reliability in the intensity measurements which agrees much more closely with experimental observations compared to conventional theory that is based on `Bragg-type' scatter. The role of dynamical effects (extinction etc.) is discussed and how they are suppressed with diffuse scattering. An alternative explanation for the Lorentz factor is presented that is more general and based on the capture volume in diffraction space. This theory, when applied to the scattering from powders, will evaluate the full scattering profile, including peak widths and the `background'. The theory should provide an increased understanding of the reliability of powder diffraction measurements, and may also have wider implications for the analysis of powder diffraction data, by increasing the accuracy of intensities predicted from structural models.

  20. A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies

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

    Szlachetko, J.; Institute of Physics, Jan Kochanowski University, 25-406 Kielce; Nachtegaal, M.

    2012-10-15

    We report on the design and performance of a wavelength-dispersive type spectrometer based on the von Hamos geometry. The spectrometer is equipped with a segmented-type crystal for x-ray diffraction and provides an energy resolution in the order of 0.25 eV and 1 eV over an energy range of 8000 eV-9600 eV. The use of a segmented crystal results in a simple and straightforward crystal preparation that allows to preserve the spectrometer resolution and spectrometer efficiency. Application of the spectrometer for time-resolved resonant inelastic x-ray scattering and single-shot x-ray emission spectroscopy is demonstrated.

  1. Medium Caliber Lead-Free Electric Primer. Version 2

    DTIC Science & Technology

    2012-09-01

    Toxic Substance Control Act TGA Thermogravimetric Analysis TNR Trinitroresorcinol V Voltage VDC Voltage Direct Current WSESRB Weapons System...variety of techniques including Thermogravimetric Analysis (TGA), base-hydrolysis, Surface Area Analysis using Brunauer, Emmett, Teller (BET...Distribution From Thermogravimetric Analysis Johnson, C. E.; Fallis, S.; Chafin, A. P.; Groshens, T. J.; Higa, K. T.; Ismail, I. M. K. and Hawkins, T. W

  2. Immobilization Effect of Morphological, Thermal and Optical Properties in Biotemplate on Zinc Oxide Nanocomposite from Chitosan

    NASA Astrophysics Data System (ADS)

    Karpuraranjith, M.; Thambidurai, S.

    Biotemplate-based zinc oxide nanocomposite was effectively prepared via simple chemical precipitation route. The functional groups of amino (-NH2), hydroxyl (-OH) and O-Zn-O were confirmed and characterized by FTIR spectroscopy. The structural and morphological properties were confirmed by XRD, UV-Vis DRS, HR-SEM and TEM analyses. The elemental composition of carbon, nitrogen, zinc and oxygen was confirmed by energy-dispersive X-ray analysis (EDAX) and Brunauer-Emmett-Teller high surface area of materials was estimated to be 52.49m2/g, respectively. Thermogravimetric analysis (TGA) shows that biotemplate on zinc oxide nanocomposite has higher thermal stability than chitosan matrix. The results demonstrate that biotemplate on zinc oxide matrix causes immobilization effect among the two components. Therefore, chitosan-ZnO nanocomposite has a microcrystalline morphological structure and also good thermal stability, so it can be a promising material for sensors, medical, tissue engineering and wastewater treatment applications.

  3. 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.

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

    PubMed

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

    2010-08-30

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

  5. 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

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

    USGS Publications Warehouse

    Hauff, Phoebe L.; VanTrump, George

    1976-01-01

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

  7. Hydrothermal formation of tobermorite studied by in situ X-ray diffraction under autoclave condition.

    PubMed

    Kikuma, Jun; Tsunashima, Masamichi; Ishikawa, Tetsuji; Matsuno, Shin-ya; Ogawa, Akihiro; Matsui, Kunio; Sato, Masugu

    2009-09-01

    Hydrothermal formation of tobermorite from a pre-cured cake has been investigated by transmission X-ray diffraction (XRD) using high-energy X-rays from a synchrotron radiation source in combination with a newly designed autoclave cell. The autoclave cell has a large and thin beryllium window for wide-angle X-ray diffraction; nevertheless, it withstands a steam pressure of more than 1.2 MPa, which enables in situ XRD measurements in a temperature range of 373 to 463 K under a saturated steam pressure. Formation and/or decomposition of several components has been successfully observed during 7.5 h of reaction time. From the intensity changes of the intermediate materials, namely non-crystalline C-S-H and hydroxylellestadite, two pathways for tobermorite formation have been confirmed. Thus, the newly developed autoclave cell can be used for the analyses of reaction mechanisms under specific atmospheres and temperatures.

  8. Microstructural characterisation of proton irradiated niobium using X-ray diffraction technique

    NASA Astrophysics Data System (ADS)

    Dutta, Argha; Gayathri, N.; Neogy, S.; Mukherjee, P.

    2018-04-01

    The microstructural parameters in pure Nb, irradiated with 5 MeV proton beam have been evaluated as a function of dose using X-ray diffraction line profile analysis. In order to assess the microstructural changes in the homogeneous region and in the peak damage region of the damage energy deposition profile, X-ray diffraction patterns have been collected using two different geometries (Bragg-Brentano and parallel beam geometries). Different X-ray line profile analysis like Williamson-Hall (W-H) analysis, modified W-H analysis, double-Voigt analysis, modified Rietveld technique and convolutional multiple whole profile fitting have been employed to extract the microstructural parameters like coherent domain size, microstrain within the domain, dislocation density and arrangement of dislocations. The coherent domain size decreases drastically along with increase in microstrain and dislocation density in the first dose for both the geometries. With increasing dose, a decreasing trend in microstrain associated with decrease in dislocation density is observed for both the geometries. This is attributed to the formation of defect clusters due to irradiation which with increasing dose collapse to dislocation loops to minimise the strain in the matrix. This is corroborated with the observation of black dots and loops in the TEM images. No significant difference is observed in the trend of microstructural parameters between the homogeneous and peak damage region of the damage profile.

  9. Powder X-ray diffraction laboratory, Reston, Virginia

    USGS Publications Warehouse

    Piatak, Nadine M.; Dulong, Frank T.; Jackson, John C.; Folger, Helen W.

    2014-01-01

    The powder x-ray diffraction (XRD) laboratory is managed jointly by the Eastern Mineral and Environmental Resources and Eastern Energy Resources Science Centers. Laboratory scientists collaborate on a wide variety of research problems involving other U.S. Geological Survey (USGS) science centers and government agencies, universities, and industry. Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media. Customized laboratory procedures and analyses commonly are used to characterize non-routine samples including, but not limited to, organic and inorganic components in petroleum source rocks, ore and mine waste, clay minerals, and glassy phases. Procedures can be adapted to meet a variety of research objectives.

  10. Structural Order-Disorder Transformations Monitored by X-Ray Diffraction and Photoluminescence

    ERIC Educational Resources Information Center

    Lima, R. C.; Paris, E. C.; Leite, E. R.; Espinosa, J. W. M.; Souza, A. G.; Longo, E.

    2007-01-01

    A study was conducted to examine the structural order-disorder transformation promoted by controlled heat treatment using X-ray diffraction technique (XRD) and photoluminescence (PL) techniques as tools to monitor the degree of structural order. The experiment was observed to be versatile and easily achieved with low cost which allowed producing…

  11. X-Ray Diffraction Study of the Internal Structure of Supercooled Water

    NASA Technical Reports Server (NTRS)

    Dorsch, Robert G.; Boyd, Bemrose

    1951-01-01

    A Bragg X-ray spectrometer equipped with a volume-sensitive Geiger counter and Soller slits and employing filtered molybdenum Ka radiation was used to obtain a set of diffracted intensity curves as a Punction of angle for supercooled water. Diffracted intensity curves in the temperature region of 21 to -16 C were obtained. The minimum between the two main diffraction peaks deepened continuously with lowering temperature, indicating a gradual change in the internal structure of the water. No discontinuity in this trend was noted at the melting point. The internal structure of supercooled water was concluded to become progressively more ice-like as the temperature is lowered.

  12. Microscopy of biological sample through advanced diffractive optics from visible to X-ray wavelength regime.

    PubMed

    Di Fabrizio, Enzo; Cojoc, Dan; Emiliani, Valentina; Cabrini, Stefano; Coppey-Moisan, Maite; Ferrari, Enrico; Garbin, Valeria; Altissimo, Matteo

    2004-11-01

    The aim of this report is to demonstrate a unified version of microscopy through the use of advanced diffractive optics. The unified scheme derives from the technical possibility of realizing front wave engineering in a wide range of electromagnetic spectrum. The unified treatment is realized through the design and nanofabrication of phase diffractive elements (PDE) through which wave front beam shaping is obtained. In particular, we will show applications, by using biological samples, ranging from micromanipulation using optical tweezers to X-ray differential interference contrast (DIC) microscopy combined with X-ray fluorescence. We report some details on the design and physical implementation of diffractive elements that besides focusing also perform other optical functions: beam splitting, beam intensity, and phase redistribution or mode conversion. Laser beam splitting is used for multiple trapping and independent manipulation of micro-beads surrounding a cell as an array of tweezers and for arraying and sorting microscopic size biological samples. Another application is the Gauss to Laguerre-Gauss mode conversion, which allows for trapping and transfering orbital angular momentum of light to micro-particles immersed in a fluid. These experiments are performed in an inverted optical microscope coupled with an infrared laser beam and a spatial light modulator for diffractive optics implementation. High-resolution optics, fabricated by means of e-beam lithography, are demonstrated to control the intensity and the phase of the sheared beams in x-ray DIC microscopy. DIC experiments with phase objects reveal a dramatic increase in image contrast compared to bright-field x-ray microscopy. Besides the topographic information, fluorescence allows detection of certain chemical elements (Cl, P, Sc, K) in the same setup, by changing the photon energy of the x-ray beam. (c) 2005 Wiley-Liss, Inc.

  13. SU-E-I-77: X-Ray Coherent Scatter Diffraction Pattern Modeling in GEANT4.

    PubMed

    Kapadia, A; Samei, E; Harrawood, B; Sahbaee, P; Chawla, A; Tan, Z; Brady, D

    2012-06-01

    To model X-ray coherent scatter diffraction patterns in GEANT4 for simulating experiments involving material detection through diffraction pattern measurement. Although coherent scatter cross-sections are modeled accurately in GEANT4, diffraction patterns for crystalline materials are not yet included. Here we describe our modeling of crystalline diffraction patterns in GEANT4 for specific materials and the validation of the results against experimentally measured data. Coherent scatter in GEANT4 is currently based on Hubbell's non-relativistic form factor tabulations from EPDL97. We modified the form-factors by introducing an interference function that accounts for the angular dependence between the Rayleigh-scattered photons and the photon wavelength. The modified form factors were used to replace the inherent form-factors in GEANT4. The simulation was tested using monochromatic and polychromatic x-ray beams (separately) incident on objects containing one or more elements with modified form-factors. The simulation results were compared against the experimentally measured diffraction images of corresponding objects using an in-house x-ray diffraction imager for validation. The comparison was made using the following metrics: number of diffraction rings, radial distance, absolute intensity, and relative intensity. Sharp diffraction pattern rings were observed in the monochromatic simulations at locations consistent with the angular dependence of the photon wavelength. In the polychromatic simulations, the diffraction patterns exhibited a radial blur consistent with the energy spread of the polychromatic spectrum. The simulated and experimentally measured patterns showed identical numbers of rings with close agreement in radial distance, absolute and relative intensities (barring statistical fluctuations). No significant change was observed in the execution time of the simulations. This work demonstrates the ability to model coherent scatter diffraction in GEANT4 in

  14. Real-time x-ray diffraction measurements of shocked polycrystalline tin and aluminum.

    PubMed

    Morgan, Dane V; Macy, Don; Stevens, Gerald

    2008-11-01

    A new, fast, single-pulse x-ray diffraction (XRD) diagnostic for determining phase transitions in shocked polycrystalline materials has been developed. The diagnostic consists of a 37-stage Marx bank high-voltage pulse generator coupled to a needle-and-washer electron beam diode via coaxial cable, producing line and bremsstrahlung x-ray emission in a 35 ns pulse. The characteristic K(alpha) lines from the selected anodes of silver and molybdenum are used to produce the diffraction patterns, with thin foil filters employed to remove the characteristic K(beta) line emission. The x-ray beam passes through a pinhole collimator and is incident on the sample with an approximately 3 x 6 mm(2) spot and 1 degrees full width half maximum angular divergence in a Bragg-reflecting geometry. For the experiments described in this report, the angle between the incident beam and the sample surface was 8.5 degrees . A Debye-Scherrer diffraction image was produced on a phosphor located 76 mm from the polycrystalline sample surface. The phosphor image was coupled to a charge-coupled device camera through a coherent fiber-optic bundle. Dynamic single-pulse XRD experiments were conducted with thin foil samples of tin, shock loaded with a 1 mm vitreous carbon back window. Detasheet high explosive with a 2-mm-thick aluminum buffer was used to shock the sample. Analysis of the dynamic shock-loaded tin XRD images revealed a phase transformation of the tin beta phase into an amorphous or liquid state. Identical experiments with shock-loaded aluminum indicated compression of the face-centered-cubic aluminum lattice with no phase transformation.

  15. Enhanced photo-stability and photocatalytic activity of Ag3PO4 via modification with BiPO4 and polypyrrole

    NASA Astrophysics Data System (ADS)

    Cai, Li; Jiang, Hui; Wang, Luxi

    2017-10-01

    Ag3PO4 photocatalysts modified with BiPO4 and polypyrrole (PPy) were successfully synthesized via a combination of co-precipitation hydrothermal technique and oxidative polymerization method. Their morphologies, structures and optical and electronic properties were characterized by means of scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscope (TEM), Brunauer-Emmett-Teller (BET) surface areas, X-ray diffraction (XRD), fourier transform infrared spectra (FT-IR), X-ray photo-electron spectroscopy (XPS), UV-vis diffuse reflection spectra (UV-vis DRS), photocurrent technique and electrochemical impedance spectra (EIS). The typical triphenylmethane dye (malachite green) was chosen as a target organic contaminants to estimate the photocatalytic activities and photo-stabilities of Ag3PO4-BiPO4-PPy heterostructures under visible light irradiation. The results indicated that the existence of BiPO4 and PPy not only showed great influences on the photocatalytic activity, but also significantly enhanced photo-stability of Ag3PO4 in repeated and long-term applications. The degradation conversion of Ag3PO4-BiPO4-PPy heterostructures (ABP-3) was 1.58 times of that of pure Ag3PO4. The photo-corrosion phenomenon of Ag3PO4 was effectively avoided. The photocatalytic activity of up to 87% in the Ag3PO4-BiPO4-PPy heterostructures (ABP-3) can be remained after five repeated cycles, while only about 33% of the degradation efficiency can be reserved in pure Ag3PO4. The possible mechanism of enhanced photo-stability and photocatalytic activity of Ag3PO4-BiPO4-PPy heterostructures was also discussed in this work.

  16. Time-spliced X-ray diffraction imaging of magnetism dynamics in a NdNiO3 thin film

    NASA Astrophysics Data System (ADS)

    Beyerlein, Kenneth R.

    2018-03-01

    Diffraction imaging of nonequilibrium dynamics at atomic resolution is becoming possible with X-ray free-electron lasers. However, there are unresolved problems with applying this method to objects that are confined in only one dimension. Here I show that reliable one-dimensional coherent diffraction imaging is possible by splicing together images recovered from different time delays in an optical pump X-ray probe experiment. The time and space evolution of antiferromagnetic order in a vibrationally excited complex oxide heterostructure is recovered from time-resolved measurements of a resonant soft X-ray diffraction peak. Midinfrared excitation of the substrate is shown to lead to a demagnetization front that propagates at a velocity exceeding the speed of sound, a critical observation for the understanding of driven phase transitions in complex condensed matter.

  17. Time-spliced X-ray diffraction imaging of magnetism dynamics in a NdNiO3 thin film.

    PubMed

    Beyerlein, Kenneth R

    2018-02-27

    Diffraction imaging of nonequilibrium dynamics at atomic resolution is becoming possible with X-ray free-electron lasers. However, there are unresolved problems with applying this method to objects that are confined in only one dimension. Here I show that reliable one-dimensional coherent diffraction imaging is possible by splicing together images recovered from different time delays in an optical pump X-ray probe experiment. The time and space evolution of antiferromagnetic order in a vibrationally excited complex oxide heterostructure is recovered from time-resolved measurements of a resonant soft X-ray diffraction peak. Midinfrared excitation of the substrate is shown to lead to a demagnetization front that propagates at a velocity exceeding the speed of sound, a critical observation for the understanding of driven phase transitions in complex condensed matter.

  18. Crystallization and preliminary X-ray diffraction analysis of a chitin-binding domain of hyperthermophilic chitinase from Pyrococcus furiosus

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

    Nakamura, Tsutomu; Ishikawa, Kazuhiko; Hagihara, Yoshihisa

    The expression, purification and preliminary X-ray diffraction studies of a chitin-binding domain of the chitinase from P. furiosus are reported. The crystallization and preliminary X-ray diffraction analysis of the chitin-binding domain of chitinase from a hyperthermophilic archaeon, Pyrococcus furiosus, are reported. The recombinant protein was prepared using an Escherichia coli overexpression system and was crystallized by the hanging-drop vapour-diffusion method. An X-ray diffraction data set was collected to 1.70 Å resolution. The crystal belonged to space group P4{sub 3}2{sub 1}2 or P4{sub 1}2{sub 1}2. The unit-cell parameters were determined to be a = b = 48.8, c = 85.0 Å.

  19. X-ray diffraction studies of shocked lunar analogs

    NASA Technical Reports Server (NTRS)

    Hanss, R. E.

    1979-01-01

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

  20. Purification, crystallization and preliminary X-ray diffraction experiment of nattokinase from Bacillus subtilis natto.

    PubMed

    Yanagisawa, Yasuhide; Chatake, Toshiyuki; Chiba-Kamoshida, Kaori; Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki; Yasuda, Ichiro; Morimoto, Yukio

    2010-12-01

    Nattokinase is a single polypeptide chain composed of 275 amino acids (molecular weight 27,724) which displays strong fibrinolytic activity. Moreover, it can activate other fibrinolytic enzymes such as pro-urokinase and tissue plasminogen activator. In the present study, native nattokinase from Bacillus subtilis natto was purified using gel-filtration chromatography and crystallized to give needle-like crystals which could be used for X-ray diffraction experiments. The crystals belonged to space group C2, with unit-cell parameters a=74.3, b=49.9, c=56.3 Å, β=95.2°. Diffraction images were processed to a resolution of 1.74 Å with an Rmerge of 5.2% (15.3% in the highest resolution shell) and a completeness of 69.8% (30.0% in the highest resolution shell). This study reports the first X-ray diffraction analysis of nattokinase.

  1. Unified Theory for Decoding the Signals from X-Ray Florescence and X-Ray Diffraction of Mixtures.

    PubMed

    Chung, Frank H

    2017-05-01

    For research and development or for solving technical problems, we often need to know the chemical composition of an unknown mixture, which is coded and stored in the signals of its X-ray fluorescence (XRF) and X-ray diffraction (XRD). X-ray fluorescence gives chemical elements, whereas XRD gives chemical compounds. The major problem in XRF and XRD analyses is the complex matrix effect. The conventional technique to deal with the matrix effect is to construct empirical calibration lines with standards for each element or compound sought, which is tedious and time-consuming. A unified theory of quantitative XRF analysis is presented here. The idea is to cancel the matrix effect mathematically. It turns out that the decoding equation for quantitative XRF analysis is identical to that for quantitative XRD analysis although the physics of XRD and XRF are fundamentally different. The XRD work has been published and practiced worldwide. The unified theory derives a new intensity-concentration equation of XRF, which is free from the matrix effect and valid for a wide range of concentrations. The linear decoding equation establishes a constant slope for each element sought, hence eliminating the work on calibration lines. The simple linear decoding equation has been verified by 18 experiments.

  2. Probing multi-scale mechanical damage in connective tissues using X-ray diffraction.

    PubMed

    Bianchi, Fabio; Hofmann, Felix; Smith, Andrew J; Thompson, Mark S

    2016-11-01

    The accumulation of microstructural collagen damage following repetitive loading is linked to painful and debilitating tendon injuries. As a hierarchical, semi-crystalline material, collagen mechanics can be studied using X-ray diffraction. The aim of the study was to describe multi-structural changes in tendon collagen following controlled plastic damage (5% permanent strain). We used small angle X-ray scattering (SAXS) to interrogate the spacing of collagen molecules within a fibril, and wide angle X-ray scattering (WAXS) to measure molecular strains under macroscopic loading. Simultaneous recordings of SAXS and WAXS patterns, together with whole-tissue strain in physiologically hydrated rat-tail tendons were made during increments of in situ tensile loading. Results showed that while tissue level modulus was unchanged, fibril modulus decreased significantly, and molecular modulus significantly increased. Further, analysis of higher order SAXS peaks suggested structural changes in the gap and overlap regions, possibly localising the damage to molecular cross-links. Our results provide new insight into the fundamental damage processes at work in collagenous tissues and point to new directions for their mitigation and repair. This article reports the first in situ loading synchrotron studies on mechanical damage in collagenous tissues. We provide new insight into the nano- and micro-structural mechanisms of damage processes. Pre-damaged tendons showed differential alteration of moduli at macro, micro and nano-scales as measured using X-ray scattering techniques. Detailed analysis of higher order diffraction peaks suggested damage is localised to molecular cross-links. The results are consistent with previous X-ray scattering studies of tendons and also with recent thermal stability studies on damaged material. Detailed understanding of damage mechanisms is essential in the development of new therapies promoting tissue repair. Copyright © 2016 Acta Materialia Inc

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

    PubMed Central

    2013-01-01

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

  4. Big Sky and Greenhorn Drill Holes and CheMin X-ray Diffraction

    NASA Image and Video Library

    2015-12-17

    The graph at right presents information from the NASA Curiosity Mars rover's onboard analysis of rock powder drilled from the "Big Sky" and "Greenhorn" target locations, shown at left. X-ray diffraction analysis of the Greenhorn sample inside the rover's Chemistry and Mineralogy (CheMin) instrument revealed an abundance of silica in the form of noncrystalline opal. The broad hump in the background of the X-ray diffraction pattern for Greenhorn, compared to Big Sky, is diagnostic of opal. The image of Big Sky at upper left was taken by the rover's Mars Hand Lens Imager (MAHLI) camera the day the hole was drilled, Sept. 29, 2015, during the mission's 1,119th Martian day, or sol. The Greenhorn hole was drilled, and the MAHLI image at lower left was taken, on Oct. 18, 2015 (Sol 1137). http://photojournal.jpl.nasa.gov/catalog/PIA20272

  5. 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.

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

    PubMed

    Martí-Rujas, Javier; Kawano, Masaki

    2013-02-19

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

  7. Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

    PubMed Central

    Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

    2016-01-01

    We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions. PMID:27324109

  8. Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

    NASA Astrophysics Data System (ADS)

    Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

    2016-06-01

    We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions.

  9. TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA

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

    Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka

    Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speedmore » higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens.« less

  10. TAKASAGO-6 apparatus for cryogenic coherent X-ray diffraction imaging of biological non-crystalline particles using X-ray free electron laser at SACLA.

    PubMed

    Kobayashi, Amane; Sekiguchi, Yuki; Takayama, Yuki; Oroguchi, Tomotaka; Shirahama, Keiya; Torizuka, Yasufumi; Manoda, Masahiro; Nakasako, Masayoshi; Yamamoto, Masaki

    2016-05-01

    Coherent X-ray diffraction imaging (CXDI) is a technique for structure analyses of non-crystalline particles with dimensions ranging from micrometer to sub-micrometer. We have developed a diffraction apparatus named TAKASAGO-6 for use in single-shot CXDI experiments of frozen-hydrated non-crystalline biological particles at cryogenic temperature with X-ray free electron laser pulses provided at a repetition rate of 30 Hz from the SPring-8 Angstrom Compact free-electron LAser. Specimen particles are flash-cooled after being dispersed on thin membranes supported by specially designed disks. The apparatus is equipped with a high-speed translation stage with a cryogenic pot for raster-scanning of the disks at a speed higher than 25 μm/33 ms. In addition, we use devices assisting the easy transfer of cooled specimens from liquid-nitrogen storages to the cryogenic pot. In the current experimental procedure, more than 20 000 diffraction patterns can be collected within 1 h. Here we report the key components and performance of the diffraction apparatus. Based on the efficiency of the diffraction data collection and the structure analyses of metal particles, biological cells, and cellular organelles, we discuss the future application of this diffraction apparatus for structure analyses of biological specimens.

  11. Template-free approach to synthesize hierarchical porous nickel cobalt oxides for supercapacitors

    NASA Astrophysics Data System (ADS)

    Chang, Jie; Sun, Jing; Xu, Chaohe; Xu, Huan; Gao, Lian

    2012-10-01

    Nickel cobalt oxides with various Ni/Co ratios were synthesized using a facile template-free approach for electrochemical supercapacitors. The texture and morphology of the nanocomposites were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller analysis (BET). The results show that a hierarchical porous structure assembled from nanoflakes with a thickness of ~10 nm was obtained, and the ratio of nickel to cobalt in the nanocomposites was very close to the precursors. Cyclic voltammetry (CV) and galvanostatic charge and discharge tests were carried out to study the electrochemical performance. Both nickel cobalt oxides (Ni-Co-O-1 with Ni : Co = 1, Ni-Co-O-2 with Ni : Co = 2) outperform pure NiO and Co3O4. The Ni-Co-O-1 and Ni-Co-O-2 possess high specific capacities of 778.2 and 867.3 F g-1 at 1 A g-1 and capacitance retentions of 84.1% and 92.3% at 10 A g-1, respectively. After full activation, the Ni-Co-O-1 and Ni-Co-O-2 could achieve a maximum value of 971 and 1550 F g-1 and remain at ~907 and ~1450 F g-1 at 4 A g-1, respectively. Also, the nickel cobalt oxides show high capacity retention when fast charging.Nickel cobalt oxides with various Ni/Co ratios were synthesized using a facile template-free approach for electrochemical supercapacitors. The texture and morphology of the nanocomposites were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller analysis (BET). The results show that a hierarchical porous structure assembled from nanoflakes with a thickness of ~10 nm was obtained, and the ratio of nickel to cobalt in the nanocomposites was very close to the precursors. Cyclic voltammetry (CV) and galvanostatic charge and discharge tests were carried out to study the electrochemical performance. Both nickel cobalt oxides (Ni-Co-O-1 with Ni : Co = 1, Ni-Co-O-2 with Ni

  12. Comparative analysis of ex-situ and operando X-ray diffraction experiments for lithium insertion materials

    NASA Astrophysics Data System (ADS)

    Brant, William R.; Li, Dan; Gu, Qinfen; Schmid, Siegbert

    2016-01-01

    A comparative study of ex-situ and operando X-ray diffraction techniques using the fast lithium ion conductor Li0.18Sr0.66Ti0.5Nb0.5O3 is presented. Ex-situ analysis of synchrotron X-ray diffraction data suggests that a single phase material exists for all discharges to as low as 0.422 V. For samples discharged to 1 V or lower, i.e. with higher lithium content, it is possible to determine the lithium position from the X-ray data. However, operando X-ray diffraction from a coin cell reveals that a kinetically driven two phase region occurs during battery cycling below 1 V. Through monitoring the change in unit cell dimension during electrochemical cycling the dynamics of lithium insertion are explored. A reduction in the rate of unit cell expansion of 22(2)% part way through the first discharge and 13(1)% during the second discharge is observed. This reduction may be caused by a drop in lithium diffusion into the bulk material for higher lithium contents. A more significant change is a jump in the unit cell expansion by 60(2)% once the lithium content exceeds one lithium ion per vacant site. It is suggested that this jump is caused by damping of octahedral rotations, thus establishing a link between lithium content and octahedral rotations.

  13. X-Ray Diffraction Study of Elemental Erbium to 65 GPa

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

    Pravica, M.G.; Lipinska-Kalita, K.; Quine, Z.

    2006-02-02

    We have investigated phase transitions in elemental erbium in a diamond anvil cell up to 65 GPa using x-ray powder diffraction methods. We present preliminary evidence of a series of phase transitions that appear to follow the expected hcp {yields} Sm-type {yields} dhcp {yields} distorted fcc sequence. In particular, we believe that we have evidence for the predicted dhcp {yields} distorted fcc transition between 43 GPa and 65 GPa.

  14. Coherent diffraction of single Rice Dwarf virus particles using hard X-rays at the Linac Coherent Light Source.

    PubMed

    Munke, Anna; Andreasson, Jakob; Aquila, Andrew; Awel, Salah; Ayyer, Kartik; Barty, Anton; Bean, Richard J; Berntsen, Peter; Bielecki, Johan; Boutet, Sébastien; Bucher, Maximilian; Chapman, Henry N; Daurer, Benedikt J; DeMirci, Hasan; Elser, Veit; Fromme, Petra; Hajdu, Janos; Hantke, Max F; Higashiura, Akifumi; Hogue, Brenda G; Hosseinizadeh, Ahmad; Kim, Yoonhee; Kirian, Richard A; Reddy, Hemanth K N; Lan, Ti-Yen; Larsson, Daniel S D; Liu, Haiguang; Loh, N Duane; Maia, Filipe R N C; Mancuso, Adrian P; Mühlig, Kerstin; Nakagawa, Atsushi; Nam, Daewoong; Nelson, Garrett; Nettelblad, Carl; Okamoto, Kenta; Ourmazd, Abbas; Rose, Max; van der Schot, Gijs; Schwander, Peter; Seibert, M Marvin; Sellberg, Jonas A; Sierra, Raymond G; Song, Changyong; Svenda, Martin; Timneanu, Nicusor; Vartanyants, Ivan A; Westphal, Daniel; Wiedorn, Max O; Williams, Garth J; Xavier, Paulraj Lourdu; Yoon, Chun Hong; Zook, James

    2016-08-01

    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. The diffraction data are available through the Coherent X-ray Imaging Data Bank (CXIDB) as a resource for algorithm development, the contents of which are described here.

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

    Paul, Nibedita; Deka, Amrita; Mohanta, Dambarudhar, E-mail: best@tezu.ernet.in

    The present work reports on the effect of Tb³⁺ doping on the luminescence and photocatalytic performance of nano-structured titania derived through a sol-gel route. X-ray diffraction patterns have revealed the existence of anatase phase with and without Tb³⁺ doping and with an improved orientation factor along (004) and (200) planes. Transmission electron microscopy and selective area electron diffraction studies, while exhibiting ample poly-crystallinity feature, have predicted an average particle size of ~9 nm and ~6 nm for the un-doped and 5% Tb³⁺ doped nano-titania samples; respectively. Apart from emissions accompanied by different types of defects, Tb³⁺ related transitions, such as,more » ⁵D₃ → ⁷F₅, ⁵D₃ → ⁷F₄, and ⁵D₄ → ⁷F₆ were identified in the photoluminescence spectra. Brunauer-Emmett-Teller surface area analysis, as carried out on a Tb³⁺ doped nano-titania system, has demonstrated a more-open hysteretic loop owing to significant difference of N₂ adsorption/desorption rates. The photocatalytic activity of nano-titania, as evaluated from the nature of degradation of methyl orange under UV illumination, exhibited the highest efficiency for a Tb³⁺ doping level of 2.5%. The augmented photocatalytic degradation has also been discussed in the light of a model based on pseudo first-order kinetics.« less

  16. HiSPoD: a program for high-speed polychromatic X-ray diffraction experiments and data analysis on polycrystalline samples

    DOE PAGES

    Sun, Tao; Fezzaa, Kamel

    2016-06-17

    Here, a high-speed X-ray diffraction technique was recently developed at the 32-ID-B beamline of the Advanced Photon Source for studying highly dynamic, yet non-repeatable and irreversible, materials processes. In experiments, the microstructure evolution in a single material event is probed by recording a series of diffraction patterns with extremely short exposure time and high frame rate. Owing to the limited flux in a short pulse and the polychromatic nature of the incident X-rays, analysis of the diffraction data is challenging. Here, HiSPoD, a stand-alone Matlab-based software for analyzing the polychromatic X-ray diffraction data from polycrystalline samples, is described. With HiSPoD,more » researchers are able to perform diffraction peak indexing, extraction of one-dimensional intensity profiles by integrating a two-dimensional diffraction pattern, and, more importantly, quantitative numerical simulations to obtain precise sample structure information.« less

  17. Monochromatic X-ray sources based on a mechanism of real and virtual photon diffraction in crystals

    NASA Astrophysics Data System (ADS)

    Wagner, A. R.; Kuznetsov, S. I.; Potylitsyn, A. P.; Razin, S. V.; Uglov, S. R.; Zabaev, V. N.

    2008-09-01

    A source of monochromatic X-ray radiation is wanted in industry, science, medicine and so on. Many ways of making such a source are known. The present work describes two mechanisms for the creation of a monochromatic X-ray beam, which are parametric X-ray radiation (PXR) and bremsstrahlung diffraction (DBS). Both the experiments were carried out using an electron beam at a microtron. During the first experiment, the DBS process was investigated as a scattering of the Bremsstrahlung (BS) beam on the crystallographic surfaces of tungsten and pyrolytic graphite crystals. The second experiment consisted in the registration of the PXR and DBS yield during the passage of the electrons through the same crystals as in the first experiment. The spectral and orientation radiation characteristics and simulation results obtained for the DBS and PXR processes are presented. It is shown that the usage of mosaic crystalline targets is rather useful in order to obtain a monochromatic X-ray source based on bremsstrahlung diffraction from moderately relativistic electrons.

  18. Non-conventional applications of a noninvasive portable X-ray diffraction/fluorescence instrument

    NASA Astrophysics Data System (ADS)

    Chiari, Giacomo; Sarrazin, Philippe; Heginbotham, Arlen

    2016-11-01

    Noninvasive techniques have become widespread in the cultural heritage analytical domain. The popular handheld X-ray fluorescence (XRF) devices give the elemental composition of all the layers that X-rays can penetrate, but no information on how atoms are bound together or at which depth they are located. A noninvasive portable X-ray powder diffraction/X-ray fluorescence (XRD/XRF) device may offer a solution to these limitations, since it can provide information on the composition of crystalline materials. This paper introduces applications of XRD beyond simple phase recognition. The two fundamental principles for XRD are: (1) the crystallites should be randomly oriented, to ensure proper intensity to all the diffraction peaks, and (2) the material should be positioned exactly in the focal plane of the instrument, respecting its geometry, as any displacement of the sample would results in 2 θ shifts of the diffraction peaks. In conventional XRD, the sample is ground and set on the properly positioned sample holder. Using a noninvasive portable instrument, these two requirements are seldom fulfilled. The position, size and orientation of a given crystallite within a layered structure depend on the object itself. Equation correlating the displacement (distance from the focal plane) versus peak shift (angular difference in 2 θ from the standard value) is derived and used to determine the depth at which a given substance is located. The quantitative composition of two binary Cu/Zn alloys, simultaneously present, was determined measuring the cell volume and using Vegard's law. The analysis of the whole object gives information on the texture and possible preferred orientations of the crystallites, which influences the peak intensity. This allows for the distinction between clad and electroplated daguerreotypes in the case of silver and between ancient and modern gilding for gold. Analyses of cross sections can be carried out successfully. Finally, beeswax, used in

  19. X-ray absorption fine structure and x-ray diffraction studies of crystallographic grains in nanocrystalline FePd:Cu thin films

    NASA Astrophysics Data System (ADS)

    Krupinski, M.; Perzanowski, M.; Polit, A.; Zabila, Y.; Zarzycki, A.; Dobrowolska, A.; Marszalek, M.

    2011-03-01

    FePd alloys have recently attracted considerable attention as candidates for ultrahigh density magnetic storage media. In this paper we investigate FePd thin alloy film with a copper admixture composed of nanometer-sized grains. [Fe(0.9 nm)/Pd(1.1 nm)/Cu(d nm)]×5 multilayers were prepared by thermal deposition at room temperature in UHV conditions on Si(100) substrates covered by 100 nm SiO2. The thickness of the copper layer has been changed from 0 to 0.4 nm. After deposition, the multilayers were rapidly annealed at 600 °C in a nitrogen atmosphere, which resulted in the creation of the FePd:Cu alloy. The structure of alloy films obtained this way was determined by x-ray diffraction (XRD), glancing angle x-ray diffraction, and x-ray absorption fine structure (EXAFS). The measurements clearly showed that the L10 FePd:Cu nanocrystalline phase has been formed during the annealing process for all investigated copper compositions. This paper concentrates on the crystallographic grain features of FePd:Cu alloys and illustrates that the EXAFS technique, supported by XRD measurements, can help to extend the information about grain size and grain shape of poorly crystallized materials. We show that, using an appropriate model of the FePd:Cu grains, the comparison of EXAFS and XRD results gives a reasonable agreement.

  20. Purification, crystallization and preliminary X-ray diffraction experiment of nattokinase from Bacillus subtilis natto

    PubMed Central

    Yanagisawa, Yasuhide; Chatake, Toshiyuki; Chiba-Kamoshida, Kaori; Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki; Yasuda, Ichiro; Morimoto, Yukio

    2010-01-01

    Nattokinase is a single polypeptide chain composed of 275 amino acids (molecular weight 27 724) which displays strong fibrinolytic activity. Moreover, it can activate other fibrinolytic enzymes such as pro-urokinase and tissue plasminogen activator. In the present study, native nattokinase from Bacillus subtilis natto was purified using gel-filtration chromatography and crystallized to give needle-like crystals which could be used for X-ray diffraction experiments. The crystals belonged to space group C2, with unit-cell parameters a = 74.3, b = 49.9, c = 56.3 Å, β = 95.2°. Diffraction images were processed to a resolution of 1.74 Å with an R merge of 5.2% (15.3% in the highest resolution shell) and a completeness of 69.8% (30.0% in the highest resolution shell). This study reports the first X-ray diffraction analysis of nattokinase. PMID:21139221

  1. Online in situ x-ray diffraction setup for structural modification studies during swift heavy ion irradiation

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

    Grygiel, C.; Lebius, H.; Bouffard, S.

    2012-01-15

    The high energy density of electronic excitations due to the impact of swift heavy ions can induce structural modifications in materials. We present an x-ray diffractometer called ALIX (''Analyse en Ligne sur IRRSUD par diffraction de rayons X''), which has been set up at the low-energy beamline (IRRadiation SUD - IRRSUD) of the Grand Accelerateur National d'Ions Lourds facility, to allow the study of structural modification kinetics as a function of the ion fluence. The x-ray setup has been modified and optimized to enable irradiation by swift heavy ions simultaneously to x-ray pattern recording. We present the capability of ALIXmore » to perform simultaneous irradiation-diffraction by using energy discrimination between x-rays from diffraction and from ion-target interaction. To illustrate its potential, results of sequential or simultaneous irradiation-diffraction are presented in this article to show radiation effects on the structural properties of ceramics. Phase transition kinetics have been studied during xenon ion irradiation of polycrystalline MgO and SrTiO{sub 3}. We have observed that MgO oxide is radiation-resistant to high electronic excitations, contrary to the high sensitivity of SrTiO{sub 3}, which exhibits transition from the crystalline to the amorphous state during irradiation. By interpreting the amorphization kinetics of SrTiO{sub 3}, defect overlapping models are discussed as well as latent track characteristics. Together with a transmission electron microscopy study, we conclude that a single impact model describes the phase transition mechanism.« less

  2. Grazing-incidence X-ray diffraction from a crystal with subsurface defects

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

    Gaevskii, A. Yu., E-mail: transilv@mail.ru; Golentus, I. E.

    2015-03-15

    The diffraction of X rays incident on a crystal surface under grazing angles under conditions of total external reflection has been investigated. An approach is proposed in which exact solutions to the dynamic problem of grazing-incidence diffraction in an ideal crystal are used as initial functions to calculate the diffuse component of diffraction in a crystal with defects. The diffuse component of diffraction is calculated for a crystal with surface defects of a dilatation-center type. Exact formulas of the continuum theory which take into account the mirror-image forces are used for defect-induced atomic displacements. Scattering intensity maps near Bragg peaksmore » are constructed for different scan modes, and the conditions for detecting primarily the diffuse component are determined. The results of dynamic calculations of grazing-incidence diffraction in defect-containing crystals are compared with calculations in the kinematic approximation.« less

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

    NASA Astrophysics Data System (ADS)

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

    2006-05-01

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

  4. Density of bunched threading dislocations in epitaxial GaN layers as determined using X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Barchuk, M.; Holý, V.; Rafaja, D.

    2018-04-01

    X-ray diffraction is one of the most popular experimental methods employed for determination of dislocation densities, as it can recognize both the strain fields and the local lattice rotations produced by dislocations. The main challenge of the quantitative analysis of the dislocation density is the formulation of a suitable microstructure model, which describes the dislocation arrangement and the effect of the interactions between the strain fields from neighboring dislocations reliably in order to be able to determine the dislocation densities precisely. The aim of this study is to prove the capability of X-ray diffraction and two computational methods, which are frequently used for quantification of the threading dislocation densities from X-ray diffraction measurements, in the special case of partially bunched threading dislocations. The first method is based on the analysis of the dislocation-controlled crystal mosaicity, and the other one on the analysis of diffuse X-ray scattering from threading dislocations. The complementarity of both methods is discussed. Furthermore, it is shown how the complementarity of these methods can be used to improve the results of the quantitative analysis of bunched and thus inhomogeneously distributed threading dislocations and to get a better insight into the dislocation arrangement.

  5. Amorphous Phase Characterization Through X-Ray Diffraction Profile Modeling: Implications for Amorphous Phases in Gale Crater Rocks and Soils

    NASA Technical Reports Server (NTRS)

    Achilles, C. N.; Downs, G. W.; Downs, R. T.; Morris, R. V.; Rampe, E. B.; Ming, D. W.; Chipera, S. J.; Blake, D. F.; Vaniman, D. T.; Bristow, T. F.; hide

    2018-01-01

    The CheMin X-ray diffraction instrument on the Mars Science Laboratory rover has analyzed 18 rock and soil samples in Gale crater. Diffraction data allow for the identification of major crystalline phases based on the positions and intensities of well-defined peaks and also provides information regarding amorphous and poorly-ordered materials based on the shape and positions of broad scattering humps. The combination of diffraction data, elemental chemistry from APXS (Alpha Particle X-ray Spectrometer) and evolved gas analyses (EGA) from SAM (Sample Analysis at Mars) help constrain possible amorphous materials present in each sample (e.g., glass, opal, iron oxides, sulfates) but are model dependent. We present a novel method to characterize amorphous material in diffraction data and, through this approach, aim to characterize the phases collectively producing the amorphous profiles in CheMin diffraction data. This method may be applied to any diffraction data from samples containing X-ray amorphous materials, not just CheMin datasets, but we re-strict our discussion to Martian-relevant amorphous phases and diffraction data measured by CheMin or CheMin-like instruments.

  6. Crystallization and X-ray diffraction analysis of a catalytic domain of hyperthermophilic chitinase from Pyrococcus furiosus

    PubMed Central

    Mine, Shouhei; Nakamura, Tsutomu; Hirata, Kunio; Ishikawa, Kazuhiko; Hagihara, Yoshihisa; Uegaki, Koichi

    2006-01-01

    The crystallization and preliminary X-ray diffraction analysis of a catalytic domain of chitinase (PF1233 gene) from the hyperthermophilic archaeon Pyrococcus furiosus is reported. The recombinant protein, prepared using an Escherichia coli expression system, was crystallized by the hanging-drop vapour-diffusion method. An X-ray diffraction data set was collected at the undulator beamline BL44XU at SPring-8 to a resolution of 1.50 Å. The crystals belong to space group P212121, with unit-cell parameters a = 90.0, b = 92.8, c = 107.2 Å. PMID:16880559

  7. Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography.

    PubMed

    Gicquel, Yannig; Schubert, Robin; Kapis, Svetlana; Bourenkov, Gleb; Schneider, Thomas; Perbandt, Markus; Betzel, Christian; Chapman, Henry N; Heymann, Michael

    2018-04-24

    This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The devices are patterned from epoxy glue using soft lithography and are suitable for in situ X-ray diffraction experiments at room temperature. The sample wells are lidded on both sides with polymeric polyimide foil windows that allow diffraction data collection with low X-ray background. This fabrication method is undemanding and inexpensive. After the sourcing of a SU-8 master wafer, all fabrication can be completed outside of a cleanroom in a typical research lab environment. The chip design and fabrication protocol utilize capillary valving to microfluidically split an aqueous reaction into defined nanoliter sized droplets. This loading mechanism avoids the sample loss from channel dead-volume and can easily be performed manually without using pumps or other equipment for fluid actuation. We describe how isolated nanoliter sized drops of protein solution can be monitored in situ by dynamic light scattering to control protein crystal nucleation and growth. After suitable crystals are grown, complete X-ray diffraction datasets can be collected using goniometer based in situ fixed target serial X-ray crystallography at room temperature. The protocol provides custom scripts to process diffraction datasets using a suite of software tools to solve and refine the protein crystal structure. This approach avoids the artefacts possibly induced during cryo-preservation or manual crystal handling in conventional crystallography experiments. We present and compare three protein structures that were solved using small crystals with dimensions of approximately 10-20 µm grown in chip. By crystallizing and diffracting in situ, handling and hence mechanical disturbances of fragile crystals is minimized. The protocol details how to fabricate a custom X-ray transparent microfluidic chip suitable for in situ serial crystallography

  8. Grating-based holographic diffraction methods for X-rays and neutrons: phase object approximation and dynamical theory

    DOE PAGES

    Feng, Hao; Ashkar, Rana; Steinke, Nina; ...

    2018-02-01

    A method dubbed grating-based holography was recently used to determine the structure of colloidal fluids in the rectangular grooves of a diffraction grating from X-ray scattering measurements. Similar grating-based measurements have also been recently made with neutrons using a technique called spin-echo small-angle neutron scattering. The analysis of the X-ray diffraction data was done using an approximation that treats the X-ray phase change caused by the colloidal structure as a small perturbation to the overall phase pattern generated by the grating. In this paper, the adequacy of this weak phase approximation is explored for both X-ray and neutron grating holography.more » Additionally, it is found that there are several approximations hidden within the weak phase approximation that can lead to incorrect conclusions from experiments. In particular, the phase contrast for the empty grating is a critical parameter. Finally, while the approximation is found to be perfectly adequate for X-ray grating holography experiments performed to date, it cannot be applied to similar neutron experiments because the latter technique requires much deeper grating channels.« less

  9. 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

  10. Cheetah: software for high-throughput reduction and analysis of serial femtosecond X-ray diffraction data

    PubMed Central

    Barty, Anton; Kirian, Richard A.; Maia, Filipe R. N. C.; Hantke, Max; Yoon, Chun Hong; White, Thomas A.; Chapman, Henry

    2014-01-01

    The emerging technique of serial X-ray diffraction, in which diffraction data are collected from samples flowing across a pulsed X-ray source at repetition rates of 100 Hz or higher, has necessitated the development of new software in order to handle the large data volumes produced. Sorting of data according to different criteria and rapid filtering of events to retain only diffraction patterns of interest results in significant reductions in data volume, thereby simplifying subsequent data analysis and management tasks. Meanwhile the generation of reduced data in the form of virtual powder patterns, radial stacks, histograms and other meta data creates data set summaries for analysis and overall experiment evaluation. Rapid data reduction early in the analysis pipeline is proving to be an essential first step in serial imaging experiments, prompting the authors to make the tool described in this article available to the general community. Originally developed for experiments at X-ray free-electron lasers, the software is based on a modular facility-independent library to promote portability between different experiments and is available under version 3 or later of the GNU General Public License. PMID:24904246

  11. Hydrothermal Synthesis of Platinum-Group-Metal-Free Catalysts: Structural Elucidation and Oxygen Reduction Catalysis

    DOE PAGES

    Gokhale, Rohan; Tsui, Lok-Kun; Roach, Kristin; ...

    2017-12-07

    In this paper, a hydrothermal approach to generate a platinum-group-metal-free (PGM-free) Fe-N-C catalyst for the oxygen reduction reaction (ORR) is introduced. The process involves partial carbonization by hydrothermal means followed by thermal treatment to obtain the final catalysts. Detailed X-ray scattering analysis of the glucose-imidazole catalysts (termed as GLU-IMID-C catalysts), obtained for the first time with the use of CarbonXS GUI program, reveals the presence of face-centered cubic (FCC) iron nanoparticles embedded in partially graphitic carbon in all catalyst variations. We also report the physical characterization of these catalysts by using X-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface area analysis, and transmissionmore » electron microscopy. The electrocatalytic behavior of the catalysts towards oxygen reduction is studied separately in acidic and alkaline electrolytes by rotating ring disk electrode measurements. The catalysts exhibit high ORR activity in acidic (0.5 M H 2SO 4) and alkaline (0.1 M KOH) electrolytes. Lastly, a precursor structure-performance relationship of these catalysts and their performance trends in both electrolytes has been discussed in this work.« less

  12. Hydrothermal Synthesis of Platinum-Group-Metal-Free Catalysts: Structural Elucidation and Oxygen Reduction Catalysis

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

    Gokhale, Rohan; Tsui, Lok-Kun; Roach, Kristin

    In this paper, a hydrothermal approach to generate a platinum-group-metal-free (PGM-free) Fe-N-C catalyst for the oxygen reduction reaction (ORR) is introduced. The process involves partial carbonization by hydrothermal means followed by thermal treatment to obtain the final catalysts. Detailed X-ray scattering analysis of the glucose-imidazole catalysts (termed as GLU-IMID-C catalysts), obtained for the first time with the use of CarbonXS GUI program, reveals the presence of face-centered cubic (FCC) iron nanoparticles embedded in partially graphitic carbon in all catalyst variations. We also report the physical characterization of these catalysts by using X-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface area analysis, and transmissionmore » electron microscopy. The electrocatalytic behavior of the catalysts towards oxygen reduction is studied separately in acidic and alkaline electrolytes by rotating ring disk electrode measurements. The catalysts exhibit high ORR activity in acidic (0.5 M H 2SO 4) and alkaline (0.1 M KOH) electrolytes. Lastly, a precursor structure-performance relationship of these catalysts and their performance trends in both electrolytes has been discussed in this work.« less

  13. Coherent diffraction of single Rice Dwarf virus particles using hard X-rays at the Linac Coherent Light Source

    PubMed Central

    Munke, Anna; Andreasson, Jakob; Aquila, Andrew; Awel, Salah; Ayyer, Kartik; Barty, Anton; Bean, Richard J.; Berntsen, Peter; Bielecki, Johan; Boutet, Sébastien; Bucher, Maximilian; Chapman, Henry N.; Daurer, Benedikt J.; DeMirci, Hasan; Elser, Veit; Fromme, Petra; Hajdu, Janos; Hantke, Max F.; Higashiura, Akifumi; Hogue, Brenda G.; Hosseinizadeh, Ahmad; Kim, Yoonhee; Kirian, Richard A.; Reddy, Hemanth K.N.; Lan, Ti-Yen; Larsson, Daniel S.D.; Liu, Haiguang; Loh, N. Duane; Maia, Filipe R.N.C.; Mancuso, Adrian P.; Mühlig, Kerstin; Nakagawa, Atsushi; Nam, Daewoong; Nelson, Garrett; Nettelblad, Carl; Okamoto, Kenta; Ourmazd, Abbas; Rose, Max; van der Schot, Gijs; Schwander, Peter; Seibert, M. Marvin; Sellberg, Jonas A.; Sierra, Raymond G.; Song, Changyong; Svenda, Martin; Timneanu, Nicusor; Vartanyants, Ivan A.; Westphal, Daniel; Wiedorn, Max O.; Williams, Garth J.; Xavier, Paulraj Lourdu; Yoon, Chun Hong; Zook, James

    2016-01-01

    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. The diffraction data are available through the Coherent X-ray Imaging Data Bank (CXIDB) as a resource for algorithm development, the contents of which are described here. PMID:27478984

  14. Coherent diffraction of single Rice Dwarf virus particles using hard X-rays at the Linac Coherent Light Source

    DOE PAGES

    Munke, Anna; Andreasson, Jakob; Aquila, Andrew; ...

    2016-08-01

    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

  15. In situ synchrotron X-ray diffraction study on epitaxial-growth dynamics of III–V semiconductors

    NASA Astrophysics Data System (ADS)

    Takahasi, Masamitu

    2018-05-01

    The application of in situ synchrotron X-ray diffraction (XRD) to the molecular-beam epitaxial (MBE) growth of III–V semiconductors is overviewed along with backgrounds of the diffraction theory and instrumentation. X-rays are sensitive not only to the surface of growing films but also to buried interfacial structures because of their large penetration depth. Moreover, a spatial coherence length up to µm order makes X-rays widely applicable to the characterization of low-dimensional structures, such as quantum dots and wires. In situ XRD studies during growth were performed using an X-ray diffractometer, which was combined with an MBE chamber. X-ray reciprocal space mapping at a speed matching a typical growth rate was achieved using intense X-rays available from a synchrotron light source and an area detector. The importance of measuring the three-dimensional distribution of XRD intensity in a reciprocal space map is demonstrated for the MBE growth of two-, one-, and zero-dimensional structures. A large amount of information about the growth process of two-dimensional InGaAs/GaAs(001) epitaxial films has been provided by three-dimensional X-ray reciprocal mappings, including the anisotropic strain relaxation, the compositional inhomogeneity, and the evolution of surface and interfacial roughness. For one-dimensional GaAs nanowires grown in a Au-catalyzed vapor-liquid–solid mode, the relationship between the diameter of the nanowires and the formation of polytypes has been suggested on the basis of in situ XRD measurements. In situ three-dimensional X-ray reciprocal space mapping is also shown to be useful for determining the lateral and vertical sizes of self-assembled InAs/GaAs(001) quantum dots as well as their internal strain distributions during growth.

  16. Specimen preparation for cryogenic coherent X-ray diffraction imaging of biological cells and cellular organelles by using the X-ray free-electron laser at SACLA

    PubMed Central

    Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka; Okajima, Koji; Fukuda, Asahi; Oide, Mao; Yamamoto, Masaki; Nakasako, Masayoshi

    2016-01-01

    Coherent X-ray diffraction imaging (CXDI) allows internal structures of biological cells and cellular organelles to be analyzed. CXDI experiments have been conducted at 66 K for frozen-hydrated biological specimens at the SPring-8 Angstrom Compact Free-Electron Laser facility (SACLA). In these cryogenic CXDI experiments using X-ray free-electron laser (XFEL) pulses, specimen particles dispersed on thin membranes of specimen disks are transferred into the vacuum chamber of a diffraction apparatus. Because focused single XFEL pulses destroy specimen particles at the atomic level, diffraction patterns are collected through raster scanning the specimen disks to provide fresh specimen particles in the irradiation area. The efficiency of diffraction data collection in cryogenic experiments depends on the quality of the prepared specimens. Here, detailed procedures for preparing frozen-hydrated biological specimens, particularly thin membranes and devices developed in our laboratory, are reported. In addition, the quality of the frozen-hydrated specimens are evaluated by analyzing the characteristics of the collected diffraction patterns. Based on the experimental results, the internal structures of the frozen-hydrated specimens and the future development for efficient diffraction data collection are discussed. PMID:27359147

  17. Specimen preparation for cryogenic coherent X-ray diffraction imaging of biological cells and cellular organelles by using the X-ray free-electron laser at SACLA.

    PubMed

    Kobayashi, Amane; Sekiguchi, Yuki; Oroguchi, Tomotaka; Okajima, Koji; Fukuda, Asahi; Oide, Mao; Yamamoto, Masaki; Nakasako, Masayoshi

    2016-07-01

    Coherent X-ray diffraction imaging (CXDI) allows internal structures of biological cells and cellular organelles to be analyzed. CXDI experiments have been conducted at 66 K for frozen-hydrated biological specimens at the SPring-8 Angstrom Compact Free-Electron Laser facility (SACLA). In these cryogenic CXDI experiments using X-ray free-electron laser (XFEL) pulses, specimen particles dispersed on thin membranes of specimen disks are transferred into the vacuum chamber of a diffraction apparatus. Because focused single XFEL pulses destroy specimen particles at the atomic level, diffraction patterns are collected through raster scanning the specimen disks to provide fresh specimen particles in the irradiation area. The efficiency of diffraction data collection in cryogenic experiments depends on the quality of the prepared specimens. Here, detailed procedures for preparing frozen-hydrated biological specimens, particularly thin membranes and devices developed in our laboratory, are reported. In addition, the quality of the frozen-hydrated specimens are evaluated by analyzing the characteristics of the collected diffraction patterns. Based on the experimental results, the internal structures of the frozen-hydrated specimens and the future development for efficient diffraction data collection are discussed.

  18. Nanox: a miniature mechanical stress rig designed for near-field X-ray diffraction imaging techniques.

    PubMed

    Gueninchault, N; Proudhon, H; Ludwig, W

    2016-11-01

    Multi-modal characterization of polycrystalline materials by combined use of three-dimensional (3D) X-ray diffraction and imaging techniques may be considered as the 3D equivalent of surface studies in the electron microscope combining diffraction and other imaging modalities. Since acquisition times at synchrotron sources are nowadays compatible with four-dimensional (time lapse) studies, suitable mechanical testing devices are needed which enable switching between these different imaging modalities over the course of a mechanical test. Here a specifically designed tensile device, fulfilling severe space constraints and permitting to switch between X-ray (holo)tomography, diffraction contrast tomography and topotomography, is presented. As a proof of concept the 3D characterization of an Al-Li alloy multicrystal by means of diffraction contrast tomography is presented, followed by repeated topotomography characterization of one selected grain at increasing levels of deformation. Signatures of slip bands and sudden lattice rotations inside the grain have been shown by means of in situ topography carried out during the load ramps, and diffraction spot peak broadening has been monitored throughout the experiment.

  19. Nanox: a miniature mechanical stress rig designed for near-field X-ray diffraction imaging techniques

    PubMed Central

    Gueninchault, N.; Proudhon, H.; Ludwig, W.

    2016-01-01

    Multi-modal characterization of polycrystalline materials by combined use of three-dimensional (3D) X-ray diffraction and imaging techniques may be considered as the 3D equivalent of surface studies in the electron microscope combining diffraction and other imaging modalities. Since acquisition times at synchrotron sources are nowadays compatible with four-dimensional (time lapse) studies, suitable mechanical testing devices are needed which enable switching between these different imaging modalities over the course of a mechanical test. Here a specifically designed tensile device, fulfilling severe space constraints and permitting to switch between X-ray (holo)tomography, diffraction contrast tomography and topotomography, is presented. As a proof of concept the 3D characterization of an Al–Li alloy multicrystal by means of diffraction contrast tomography is presented, followed by repeated topotomography characterization of one selected grain at increasing levels of deformation. Signatures of slip bands and sudden lattice rotations inside the grain have been shown by means of in situ topography carried out during the load ramps, and diffraction spot peak broadening has been monitored throughout the experiment. PMID:27787253

  20. Adsorption, oxidation, and reduction behavior of arsenic in the removal of aqueous As(III) by mesoporous Fe/Al bimetallic particles.

    PubMed

    Cheng, Zihang; Fu, Fenglian; Dionysiou, Dionysios D; Tang, Bing

    2016-06-01

    In this study, mesoporous iron/aluminum (Fe/Al) bimetallic particles were synthesized and employed for the removal of aqueous As(III). Scanning electron microscopy and energy dispersive spectroscopy (SEM-EDS), Brunauer-Emmett-Teller (BET) analysis method, Vibrating-sample magnetometry (VSM), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FTIR) were employed to characterize the Fe/Al bimetals before and after reaction with As(III). The physical properties, compositions, and structures of Fe/Al bimetallic particles as well as the As(III) removal mechanism were investigated. The characterization of the bimetallic particles after the reaction has revealed the removal of As(III) is a complex process including surface adsorption and oxidation, and intraparticle reduction. The good As(III) removal capability and stability of the Fe/Al bimetallic particles exhibited its great potential as an effective and environmental friendly agent for As(III) removal from water. Copyright © 2016 Elsevier Ltd. All rights reserved.