WorldWideScience

Sample records for single-pulse xrd experiments

  1. Picosecond, single pulse electron linear accelerator

    International Nuclear Information System (INIS)

    Kikuchi, Riichi; Kawanishi, Masaharu

    1979-01-01

    The picosecond, single pulse electron linear accelerators, are described, which were installed in the Nuclear Engineering Laboratory of the University of Tokyo and in the Nuclear Radiation Laboratory of the Osaka University. The purpose of the picosecond, single pulse electron linear accelerators is to investigate the very short time reaction of the substances, into which gamma ray or electron beam enters. When the electrons in substances receive radiation energy, the electrons get high kinetic energy, and the energy and the electric charge shift, at last to the quasi-stable state. This transient state can be experimented with these special accelerators very accurately, during picoseconds, raising the accuracy of the time of incidence of radiation and also raising the accuracy of observation time. The outline of these picosecond, single pulse electron linear accelerators of the University of Tokyo and the Osaka University, including the history, the systems and components and the output beam characteristics, are explained. For example, the maximum energy 30 -- 35 MeV, the peak current 1 -- 8 n C, the pulse width 18 -- 40 ps, the pulse repetition rate 200 -- 720 pps, the energy spectrum 1 -- 1.8% and the output beam diameter 2 -- 5 mm are shown as the output beam characteristics of the accelerators in both universities. The investigations utilizing the picosecond single pulse electron linear accelerators, such as the investigation of short life excitation state by pulsed radiation, the dosimetry study of pulsed radiation, and the investigation of the transforming mechanism and the development of the transforming technology from picosecond, single pulse electron beam to X ray, vacuum ultraviolet ray and visual ray, are described. (Nakai, Y.)

  2. A Single-Pulse Integrator

    DEFF Research Database (Denmark)

    Miller, Arne

    1974-01-01

    A single-pulse integrator is described. It gives a relative measure of the integral of the output signal from a coil monitor on the Risø 10 MeV linear accelerator, and displays the value on a digital voltmeter. The reproduccibility is found to be better than ±1% for an accelerated pulse charge...

  3. An Integrated XRF/XRD Instrument for Mars Exobiology and Geology Experiments

    Science.gov (United States)

    Koppel, L. N.; Franco, E. D.; Kerner, J. A.; Fonda, M. L.; Schwartz, D. E.; Marshall, J. R.

    1993-01-01

    By employing an integrated x-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details characterizing the past and present environment on Mars and those relevant to the possibility of the origin and evolution of life will be acquired. A combined x-ray fluorescence/x-ray diffraction (XRF/XRD) instrument was breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for MESUR and future Mars missions. Among others, primary objectives for the exploration of Mars include the intense study of local areas on Mars to establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance, and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epoches; and to establish the global chemical and physical characteristics of the Martian surface. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment. Preliminary breadboard experiments confirmed the fundamental instrument design approach and measurement performance.

  4. Self triggered single pulse beam position monitor

    International Nuclear Information System (INIS)

    Rothman, J.L.; Blum, E.B.

    1993-01-01

    A self triggered beam position monitor (BPM) has been developed for the NSLS injection system to provide single pulse orbit measurements in the booster synchrotron, linac, and transport lines. The BPM integrates the negative going portion of 3 nS wide bipolar pickup electrode signals. The gated, self triggering feature confines critical timing components to the front end, relaxing external timing specifications. The system features a low noise high speed FET sampler, a fiber optic gate for bunch and turn selection, and an inexpensive interface to a standard PC data acquisition system

  5. Enhancement of beam pulse controllability for a single-pulse formation system of a cyclotron

    International Nuclear Information System (INIS)

    Kurashima, Satoshi; Miyawaki, Nobumasa; Kashiwagi, Hirotsugu; Okumura, Susumu; Taguchi, Mitsumasa; Fukuda, Mitsuhiro

    2015-01-01

    The single-pulse formation technique using a beam chopping system consisting of two types of high-voltage beam kickers was improved to enhance the quality and intensity of the single-pulse beam with a pulse interval over 1 μs at the Japan Atomic Energy Agency cyclotron facility. A contamination rate of neighboring beam bunches in the single-pulse beam was reduced to less than 0.1%. Long-term purification of the single pulse beam was guaranteed by the well-controlled magnetic field stabilization system for the cyclotron magnet. Reduction of the multi-turn extraction number for suppressing the neighboring beam bunch contamination was achieved by restriction of a beam phase width and precise optimization of a particle acceleration phase. In addition, the single-pulse beam intensity was increased by a factor of two or more by a combination of two types of beam bunchers using sinusoidal and saw-tooth voltage waveforms. Provision of the high quality intense single-pulse beam contributed to improve the accuracy of experiments for investigation of scintillation light time-profile and for neutron energy measurement by a time-of-flight method

  6. Combined XRD and XAS

    International Nuclear Information System (INIS)

    Ehrlich, S.N.; Hanson, J.C.; Lopez Camara, A.; Barrio, L.; Estrella, M.; Zhou, G.; Si, R.; Khalid, S.; Wang, Q.

    2011-01-01

    X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS) are complementary techniques for investigating the structure of materials. XRD probes long range order and XAFS probes short range order. We have combined the two techniques at one synchrotron beamline, X18A at the NSLS, allowing samples to be studied in a single experiment. This beamline will allow for coordinated measurements of local and long range structural changes in chemical transformations and phase transitions using both techniques.

  7. Effects of single pulse energy on the properties of ceramic coating prepared by micro-arc oxidation on Ti alloy

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jun-Hua [Department of Mechanical Engineering, Tsinghua University, Beijing 100084 (China); School of Materials Science and Engineering, Henan University of Science and Technology, Luoyang 471023 (China); Faculty of Mechanical and Electrical Engineering, Kunming University of Science and Technology, Kunming 650500 (China); Wang, Jin [Department of Mechanical Engineering, Tsinghua University, Beijing 100084 (China); Beijing Key Lab of Precision/Ultra-precision Manufacturing Equipments and Control, Beijing 100084 (China); Lu, Yan [School of Materials Science and Engineering, Henan University of Science and Technology, Luoyang 471023 (China); Du, Mao-Hua [Faculty of Mechanical and Electrical Engineering, Kunming University of Science and Technology, Kunming 650500 (China); Han, Fu-Zhu, E-mail: hanfuzhu@mail.tsinghua.edu.cn [Department of Mechanical Engineering, Tsinghua University, Beijing 100084 (China); Beijing Key Lab of Precision/Ultra-precision Manufacturing Equipments and Control, Beijing 100084 (China)

    2015-01-01

    Highlights: • Single pulse energy remarkably influences the properties of ceramic coating prepared by MAO on Ti alloy. • The accumulative time of impulse width is an important parameter in the scientific and rational measurement of the film forming law of ceramic coating. • The ceramic coating thickness approximately linearly increases with the cumulative time of impulse width. • Larger impulse width resulted in higher single pulse energy, film forming rates and thicker ceramic coating thickness. • The effects of single pulse energy on the micro-hardness and phase composition of ceramic coating are not as evident as those of frequency and duty cycle. - Abstract: The effects of single pulse energy on the properties of ceramic coating fabricated on a Ti–6Al–4V alloy via micro-arc oxidation (MAO) in aqueous solutions containing aluminate, phosphate, and some additives are investigated. The thickness, micro-hardness, surface and cross-sectional morphology, surface roughness, and compositions of the ceramic coating are studied using eddy current thickness meter, micro-hardness tester, JB-4C Precision Surface roughness meter, scanning electron microscopy (SEM) and X-ray diffraction (XRD). Single pulse energy remarkably influences the ceramic coating properties. The accumulative time of impulse width is an important parameter in the scientific and rational measurement of the film forming law of ceramic coating. The ceramic coating thickness approximately linearly increases with the cumulative time of impulse width. Larger impulse width resulted in higher single pulse energy, film forming rates and thicker ceramic coating thickness. The sizes of oxide particles, micro-pores and micro-cracks slightly increase with impulse width and single pulse energy. The main surface conversion products generated during MAO process in aqueous solutions containing aluminate are rutile TiO{sub 2}, anatase TiO{sub 2}, and a large amount of Al{sub 2}TiO{sub 5}. The effects of

  8. High-mechanical-strength single-pulse draw tower gratings

    Science.gov (United States)

    Rothhardt, Manfred W.; Chojetzki, Christoph; Mueller, Hans Rainer

    2004-11-01

    The inscription of fiber Bragg gratings during the drawing process is a very useful method to realize sensor arrays with high numbers of gratings and excellent mechanical strength and also type II gratings with high temperature stability. Results of single pulse grating arrays with numbers up to 100 and definite wavelengths and positions for sensor applications were achieved at 1550 nm and 830 nm using new photosensitive fibers developed in IPHT. Single pulse type I gratings at 1550 nm with more than 30% reflectivity were shown first time to our knowledge. The mechanical strength of this fiber with an Ormocer coating with those single pulse gratings is the same like standard telecom fibers. Weibull plots of fiber tests will be shown. At 830 nm we reached more than 10% reflectivity with single pulse writing during the fiber drawing in photosensitive fibers with less than 16 dB/km transmission loss. These gratings are useful for stress and vibration sensing applications. Type II gratings with reflectivity near 100% and smooth spectral shape and spectral width of about 1 nm are temperature stable up to 1200 K for short time. They are also realized in the fiber drawing process. These gratings are useful for temperature sensor applications.

  9. Overview - XRF and XRD

    International Nuclear Information System (INIS)

    Jenkins, R.

    1999-01-01

    Full text: While the roots of both X-ray Fluorescence Spectrometry (XRF) and X-ray Powder Diffractometry (XRD) go back 80 years or so, it is only in the last 30 years or so that both techniques have become widely used in the industrial and research environments. It is the experience of the author that all instrumental techniques go through four basic stages: 1. Innovation - someone has a bright idea 2. Application - people start to apply the bright idea 3. Frustration - the bright idea is found to have complications 4. Consolidation - the complications are understood and resolved. XRF went through these four stages by the mid 1980s. This means that, today, if one understands what one is doing, applies the correct (and generally well known) analytical strategy, there is a high probability that one will obtain the correct result. XRD, on the other hand, is still hovering between 3 and 4 on the list. Problems such as the effect of preferred orientation on intensities, difficulties in obtaining accurate data for larger d-spacings, etc., although better understood today, still pose significant challenges to those involved in both routine and research analysis. The development of low-cost computers has made a dramatic impact in both techniques and it is estimated that today, about 90% of all new spectrometer and diffractometer systems sold, are fully automated. There are about 30,000 X-ray spectrometers and about 25,000 diffractometers in use in the world today. Of these about one half are automated. The process of automation has brought its rewards as well as its consequences. In general, the automation of the two techniques has resulted in a poorer understanding of the instrumentation and methodology, on the part of the typical user. Many laboratories employ both techniques, since they are largely complimentary. This workshop will cover the basics of the two methods, highlighting the advantages and shortcomings of both. Copyright (1999) Australian X-ray Analytical

  10. High-pressure structural behaviour of HoVO4: combined XRD experiments and ab initio calculations

    International Nuclear Information System (INIS)

    Garg, Alka B; Errandonea, D; Rodríguez-Hernández, P; Muñoz, A; López-Moreno, S; Popescu, C

    2014-01-01

    We report a high-pressure experimental and theoretical investigation of the structural properties of zircon-type HoVO 4 . Angle-dispersive x-ray diffraction measurements were carried out under quasi-hydrostatic and partial non-hydrostatic conditions up to 28 and 23.7 GPa, respectively. In the first case, an irreversible phase transition is found at 8.2 GPa. In the second case, the onset of the transition is detected at 4.5 GPa, a second (reversible) transition is found at 20.4 GPa, and a partial decomposition of HoVO 4 was observed. The structures of the different phases have been assigned and their equations of state (EOS) determined. Experimental results have also been compared to theoretical calculations which fully agree with quasi-hydrostatic experiments. Theory also suggests the possibility of another phase transition at 32 GPa; i.e. beyond the pressure limit covered by present experiments. Furthermore, calculations show that deviatoric stresses could trigger the transition found at 20.4 GPa under non-hydrostatic conditions. The reliability of the present experimental and theoretical results is supported by the consistency between the values yielded for transition pressures and EOS parameters by the two methods. (paper)

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

    Energy Technology Data Exchange (ETDEWEB)

    Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.; Hunt, D.; Hahn, D.; Cradick, J. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Morgan, D. V. [National Security Technologies LLC, Los Alamos, New Mexico 87544 (United States)

    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 the 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.

  12. THE CRAB PULSAR AT CENTIMETER WAVELENGTHS. II. SINGLE PULSES

    Energy Technology Data Exchange (ETDEWEB)

    Hankins, T. H.; Eilek, J. A. [Physics Department, New Mexico Tech, Socorro, NM 87801 (United States); Jones, G., E-mail: thankins@aoc.nrao.edu [Columbia University, New York, NY 10027 (United States)

    2016-12-10

    We have carried out new, high-frequency, high-time-resolution observations of the Crab pulsar. Combining these with our previous data, we characterize bright single pulses associated with the Main Pulse, both the Low-Frequency and High-Frequency Interpulses, and the two  High-Frequency Components. Our data include observations at frequencies ranging from 1 to 43 GHz with time resolutions down to a fraction of a nanosecond. We find that at least two types of emission physics are operating in this pulsar. Both Main Pulses and Low-Frequency Interpulses, up to ∼10 GHz, are characterized by nanoshot emission—overlapping clumps of narrowband nanoshots, each with its own polarization signature. High-Frequency Interpulses, between 5 and 30 GHz, are characterized by spectral band emission—linearly polarized emission containing ∼30 proportionately spaced spectral bands. We cannot say whether the longer-duration High-Frequency Components pulses are due to a scattering process, or if they come from yet another type of emission physics.

  13. Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading

    Energy Technology Data Exchange (ETDEWEB)

    Fan, D.; Luo, S. N., E-mail: sluo@pims.ac.cn [The Peac Institute of Multiscale Sciences, Chengdu, Sichuan 610031 (China); Key Laboratory of Advanced Technologies of Materials, Ministry of Education, Southwest Jiaotong University, Chengdu, Sichuan 610031 (China); Huang, J. W.; Zeng, X. L.; Li, Y.; E, J. C.; Huang, J. Y. [The Peac Institute of Multiscale Sciences, Chengdu, Sichuan 610031 (China); Sun, T.; Fezzaa, K. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Wang, Z. [Physics Division P-25, Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States)

    2016-05-15

    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 quantify 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.

  14. Flame Motion In Gas Turbine Burner From Averages Of Single-Pulse Flame Fronts

    Energy Technology Data Exchange (ETDEWEB)

    Tylli, N.; Hubschmid, W.; Inauen, A.; Bombach, R.; Schenker, S.; Guethe, F. [Alstom (Switzerland); Haffner, K. [Alstom (Switzerland)

    2005-03-01

    Thermo acoustic instabilities of a gas turbine burner were investigated by flame front localization from measured OH laser-induced fluorescence single pulse signals. The average position of the flame was obtained from the superposition of the single pulse flame fronts at constant phase of the dominant acoustic oscillation. One observes that the flame position varies periodically with the phase angle of the dominant acoustic oscillation. (author)

  15. Wavelength dependence of the single pulse femtosecond laser ablation threshold of indium phosphide in the 400-2050 nm range

    International Nuclear Information System (INIS)

    Borowiec, A.; Tiedje, H.F.; Haugen, H.K.

    2005-01-01

    We present single pulse femtosecond laser ablation threshold measurements of InP obtained by optical, scanning electron, and atomic force microscopy. The experiments were conducted with laser pulses 65-175 fs in duration, in the wavelength range from 400 to 2050 nm, covering the photon energy region above and below the bandgap of InP. The ablation thresholds determined from depth and volume measurements varied from 87 mJ/cm 2 at 400 nm to 250 mJ/cm 2 at 2050 nm. In addition, crater depths and volumes were measured over a range of laser fluences extending well above the ablation threshold

  16. Design of a high-pressure single pulse shock tube for chemical kinetic investigations

    International Nuclear Information System (INIS)

    Tranter, R. S.; Brezinsky, K.; Fulle, D.

    2001-01-01

    A single pulse shock tube has been designed and constructed in order to achieve extremely high pressures and temperatures to facilitate gas-phase chemical kinetic experiments. Postshock pressures of greater than 1000 atmospheres have been obtained. Temperatures greater than 1400 K have been achieved and, in principle, temperatures greater than 2000 K are easily attainable. These high temperatures and pressures permit the investigation of hydrocarbon species pyrolysis and oxidation reactions. Since these reactions occur on the time scale of 0.5--2 ms the shock tube has been constructed with an adjustable length driven section that permits variation of reaction viewing times. For any given reaction viewing time, samples can be withdrawn through a specially constructed automated sampling apparatus for subsequent species analysis with gas chromatography and mass spectrometry. The details of the design and construction that have permitted the successful generation of very high-pressure shocks in this unique apparatus are described. Additional information is provided concerning the diaphragms used in the high-pressure shock tube

  17. Continuous single pulse resolved measurement of beam diameters at 200 kHz using optical transmission filters

    Science.gov (United States)

    Fruechtenicht, Johannes; Letsch, Andreas; Voss, Andreas; Abdou Ahmed, Marwan; Graf, Thomas

    2012-02-01

    We present a novel laser beam measurement setup which allows the determination of the beam diameter for each single pulse of a pulsed laser beam at repetition rates of up to 200 kHz. This is useful for online process-parameter control e.g. in micromachining or for laser source characterization. Basically, the developed instrument combines spatial transmission filters specially designed for instantaneous optical determination of the second order moments of the lateral intensity distribution of the light beam and photodiodes coupled to customized electronics. The acquisition is computer-based, enabling real-time operation for online monitoring or control. It also allows data storage for a later analysis and visualization of the measurement results. The single-pulse resolved beam diameter can be measured and recorded without any interruption for an unlimited number of pulses. It is only limited by the capacity of the data storage means. In our setup a standard PC and hard-disk provided 2 hours uninterrupted operation and recording of varying beam diameters at 200 kHz. This is about three orders of magnitude faster than other systems. To calibrate our device we performed experiments in cw and pulsed regimes and the obtained results were compared to those obtained with a commercial camera based system. Only minor deviations of the beam diameter values between the two instruments were observed, proving the reliability of our approach.

  18. Catastrophic optical mirror damage in diode lasers monitored during single-pulse operation

    DEFF Research Database (Denmark)

    Zegler, M.; Tomm, J.W.; Reeber, D.

    2009-01-01

    is achieved. The thermal runaway process is unambiguously related to the occurrence of a “thermal flash.” A one-by-one correlation between nearfield, thermal flash, thermal runaway, and structural damage is observed. The single-pulse excitation technique allows for controlling the propagation...

  19. Specific features of a single-pulse sliding discharge in neon near the threshold for spark breakdown

    Science.gov (United States)

    Trusov, K. K.

    2017-08-01

    Experimental data on the spatial structure of a single-pulse sliding discharge in neon at voltages below, equal to, and above the threshold for spark breakdown are discussed. The experiments were carried at gas pressures of 30 and 100 kPa and different polarities of the discharge voltage. Photographs of the plasma structure in two discharge chambers with different dimensions of the discharge zone and different thicknesses of an alumina dielectric plate on the surface of which the discharge develops are inspected. Common features of the prebreakdown discharge and its specific features depending on the voltage polarity and gas pressure are analyzed. It is shown that, at voltages below the threshold for spark breakdown, a low-current glow discharge with cathode and anode spots develops in the electrode gap. Above the breakdown threshold, regardless of the voltage polarity, spark channels directed from the cathode to the anode develop against the background of a low-current discharge.

  20. Dielectric breakdown and healing of anodic oxide films on aluminium under single pulse anodizing

    International Nuclear Information System (INIS)

    Sah, Santosh Prasad; Tatsuno, Yasuhiro; Aoki, Yoshitaka; Habazaki, Hiroki

    2011-01-01

    Research highlights: → We examined dielectric breakdown of anodic alumina by single pulse anodizing. → Current transients and morphology of discharge channels are dependent upon electrolyte and voltage. → There is a good correlation between current transient and morphology of discharge channel. → Healing of open discharge pores occurs in alkaline silicate, but not in pentaborate electrolyte. - Abstract: Single pulse anodizing of aluminium micro-electrode has been employed to study the behaviour of dielectric breakdown and subsequent oxide formation on aluminium in alkaline silicate and pentaborate electrolytes. Current transients during applying pulse voltage have been measured, and surface has been observed by scanning electron microscopy. Two types of current transients are observed, depending on the electrolyte and applied voltage. There is a good correlation between the current transient behaviour and the shape of discharge channels. In alkaline silicate electrolyte, circular open pores are healed by increasing the pulse width, but such healing is not obvious in pentaborate electrolyte.

  1. XRD alignment, calibration and performance

    International Nuclear Information System (INIS)

    Davy, L.

    2002-01-01

    Full text: The quality of any diffractometer system is very much dependent on the alignment, calibration and performance. The three subjects are very much related. Firstly, you must know how to carry out the full diffractometer alignment. XRD alignment is easy once you know how. The presentation will show you step by step to carry out the full alignment. Secondly, you need to know how to calibrate the diffractometer system. The presentation will show you how to calibrate the goniometer, detector etc. Thirdly, to prove the system is working within the manufacturer specification. The presentation will show you how to carry out the resolution, reproducibility and linearity test. Copyright (2002) Australian X-ray Analytical Association Inc

  2. Can a single pulse transcranial magnetic stimulation targeted to the motor cortex interrupt pain processing?

    Science.gov (United States)

    Kisler, Lee-Bareket; Gurion, Ilan; Granovsky, Yelena; Sinai, Alon; Sprecher, Elliot; Shamay-Tsoory, Simone; Weissman-Fogel, Irit

    2018-01-01

    The modulatory role of the primary motor cortex (M1), reflected by an inhibitory effect of M1-stimulation on clinical pain, motivated us to deepen our understanding of M1's role in pain modulation. We used Transcranial Magnetic Stimulation (TMS)-induced virtual lesion (VL) to interrupt with M1 activity during noxious heat pain. We hypothesized that TMS-VL will effect experimental pain ratings. Three VL protocols were applied consisting of single-pulse TMS to transiently interfere with right M1 activity: (1) VLM1- TMS applied to 11 subjects, 20 msec before the individual's first pain-related M1 peak activation, as determined by source analysis (sLORETA), (2) VL-50 (N = 16; TMS applied 50 ms prior to noxious stimulus onset), and (3) VL+150 (N = 16; TMS applied 150 ms after noxious stimulus onset). Each protocol included 3 conditions ('pain-alone', ' TMS-VL', and 'SHAM-VL'), each consisted of 30 noxious heat stimuli. Pain ratings were compared, in each protocol, for TMS-VL vs. SHAM-VL and vs. pain-alone conditions. Repeated measures analysis of variance, corrected for multiple comparisons revealed no significant differences in the pain ratings between the different conditions within each protocol. Therefore, our results from this exploratory study suggest that a single pulse TMS-induced VL that is targeted to M1 failed to interrupt experimental pain processing in the specific three stimulation timing examined here.

  3. Confocal μ-XRF, μ-XAFS, and μ-XRD Studies of Sediment from a Nuclear Waste Disposal Natural Analogue Site and Fractured Granite Following a Radiotracer Migration Experiment

    International Nuclear Information System (INIS)

    Denecke, Melissa A.; Brendebach, Boris; Rothe, Joerg; Simon, Rolf; Janssens, Koen; Nolf, Wout de; Vekemans, Bart; Falkenberg, Gerald; Somogyi, Andrea; Noseck, Ulrich

    2007-01-01

    Combined μ-XRF, μ-XAFS, and μ-XRD investigations of a uranium-rich tertiary sediment, from a nuclear repository natural analogue site, and a fractured granite bore core section after a column tracer experiment using a Np(V) containing cocktail have been performed. Most μ-XRF/μ-XAFS measurements are recorded in a confocal geometry to provide added depth information. The U-rich sediment results show uranium to be present as a tetravalent phosphate and that U(IV) is associated with As(V). Arsenic present is either As(V) or As(0). The As(0) forms thin coatings on the surface of pyrite nodules. A hypothesis for the mechanism of uranium immobilization is proposed, where arsenopyrite acted as reductant of ground water dissolved U(VI) leading to precipitation of less soluble U(IV) and thereby forming As(V). Results for the granite sample show the immobilized Np to be tetravalent and associated with facture material

  4. Development of dynamic simulation code for fuel cycle of fusion reactor. 1. Single pulse operation simulation

    Energy Technology Data Exchange (ETDEWEB)

    Aoki, Isao; Seki, Yasushi [Japan Atomic Energy Research Inst., Naka, Ibaraki (Japan). Naka Fusion Research Establishment; Sasaki, Makoto; Shintani, Kiyonori; Kim, Yeong-Chan

    1997-11-01

    A dynamic simulation code for the fuel cycle of a fusion experimental reactor has been developed. The code follows the fuel inventory change with time in the plasma chamber and the fuel cycle system during a single pulse operation. The time dependence of the fuel inventory distribution is evaluated considering the fuel burn and exhaust in the plasma chamber, purification and supply functions. For each subsystem of the plasma chamber and the fuel cycle system, the fuel inventory equation is written based on the equation of state considering the function of fuel burn, exhaust, purification, and supply. The processing constants of subsystem for the steady states were taken from the values in the ITER Conceptual Design Activity (CDA) report. Using the code, the time dependence of the fuel supply and inventory depending on the burn state and subsystem processing functions are shown. (author)

  5. Single-pulse and multi-pulse femtosecond laser damage of optical single films

    International Nuclear Information System (INIS)

    Yuan Lei; Zhao Yuan'an; He Hongbo; Shao Jianda; Fan Zhengxiu

    2006-01-01

    Laser-induced damage of a single 500 nm HfO 2 film and a single 500 nm ZrO 2 film were studied with single- and multi-pulse femtosecond laser. The laser-induced damage thresholds (LIDT) of both samples by the 1-on-1 method and the 1000-on-1 method were reported. It was discovered that the LIDT of the HfO 2 single film was higher than that of the ZrO 2 single film by both test methods, which was explained by simple Keldysh's multiphoton ionization theory. The LIDT of multi-pulse was lower than that of single-pulse for both samples as a result of accumulative effect. (authors)

  6. Timing Solution and Single-pulse Properties for Eight Rotating Radio Transients

    Energy Technology Data Exchange (ETDEWEB)

    Cui, B.-Y.; McLaughlin, M. A. [Department of Physics and Astronomy West Virginia University Morgantown, WV 26506 (United States); Boyles, J. [Department of Physics and Astronomy West Kentucky University Bowling Green, KY 42101 (United States); Palliyaguru, N. [Physics and Astronomy Department Texas Tech University Lubbock, TX 79409-1051 (United States)

    2017-05-01

    Rotating radio transients (RRATs), loosely defined as objects that are discovered through only their single pulses, are sporadic pulsars that have a wide range of emission properties. For many of them, we must measure their periods and determine timing solutions relying on the timing of their individual pulses, while some of the less sporadic RRATs can be timed by using folding techniques as we do for other pulsars. Here, based on Parkes and Green Bank Telescope (GBT) observations, we introduce our results on eight RRATs including their timing-derived rotation parameters, positions, and dispersion measures (DMs), along with a comparison of the spin-down properties of RRATs and normal pulsars. Using data for 24 RRATs, we find that their period derivatives are generally larger than those of normal pulsars, independent of any intrinsic correlation with period, indicating that RRATs’ highly sporadic emission may be associated with intrinsically larger magnetic fields. We carry out Lomb–Scargle tests to search for periodicities in RRATs’ pulse detection times with long timescales. Periodicities are detected for all targets, with significant candidates of roughly 3.4 hr for PSR J1623−0841 and 0.7 hr for PSR J1839−0141. We also analyze their single-pulse amplitude distributions, finding that log-normal distributions provide the best fits, as is the case for most pulsars. However, several RRATs exhibit power-law tails, as seen for pulsars emitting giant pulses. This, along with consideration of the selection effects against the detection of weak pulses, imply that RRAT pulses generally represent the tail of a normal intensity distribution.

  7. Timing Solution and Single-pulse Properties for Eight Rotating Radio Transients

    Science.gov (United States)

    Cui, B.-Y.; Boyles, J.; McLaughlin, M. A.; Palliyaguru, N.

    2017-05-01

    Rotating radio transients (RRATs), loosely defined as objects that are discovered through only their single pulses, are sporadic pulsars that have a wide range of emission properties. For many of them, we must measure their periods and determine timing solutions relying on the timing of their individual pulses, while some of the less sporadic RRATs can be timed by using folding techniques as we do for other pulsars. Here, based on Parkes and Green Bank Telescope (GBT) observations, we introduce our results on eight RRATs including their timing-derived rotation parameters, positions, and dispersion measures (DMs), along with a comparison of the spin-down properties of RRATs and normal pulsars. Using data for 24 RRATs, we find that their period derivatives are generally larger than those of normal pulsars, independent of any intrinsic correlation with period, indicating that RRATs’ highly sporadic emission may be associated with intrinsically larger magnetic fields. We carry out Lomb-Scargle tests to search for periodicities in RRATs’ pulse detection times with long timescales. Periodicities are detected for all targets, with significant candidates of roughly 3.4 hr for PSR J1623-0841 and 0.7 hr for PSR J1839-0141. We also analyze their single-pulse amplitude distributions, finding that log-normal distributions provide the best fits, as is the case for most pulsars. However, several RRATs exhibit power-law tails, as seen for pulsars emitting giant pulses. This, along with consideration of the selection effects against the detection of weak pulses, imply that RRAT pulses generally represent the tail of a normal intensity distribution.

  8. Investigating emotional top down modulation of ambiguous faces by single pulse TMS on early visual cortices

    Directory of Open Access Journals (Sweden)

    Zachary Adam Yaple

    2016-06-01

    Full Text Available Top-down processing is a mechanism in which memory, context and expectation are used to perceive stimuli. For this study we investigated how emotion content, induced by music mood, influences perception of happy and sad emoticons. Using single pulse TMS we stimulated right occipital face area (rOFA, primary visual cortex (V1 and vertex while subjects performed a face-detection task and listened to happy and sad music. At baseline, incongruent audio-visual pairings decreased performance, demonstrating dependence of emotion while perceiving ambiguous faces. However, performance of face identification decreased during rOFA stimulation regardless of emotional content. No effects were found between Cz and V1 stimulation. These results suggest that while rOFA is important for processing faces regardless of emotion, V1 stimulation had no effect. Our findings suggest that early visual cortex activity may not integrate emotional auditory information with visual information during emotion top-down modulation of faces.

  9. Interaction of single-pulse laser energy with bow shock in hypersonic flow

    Directory of Open Access Journals (Sweden)

    Hong Yanji

    2014-04-01

    Full Text Available Pressure sensing and schlieren imaging with high resolution and sensitivity are applied to the study of the interaction of single-pulse laser energy with bow shock at Mach 5. An Nd:YAG laser operated at 1.06 μm, 100 mJ pulse energy is used to break down the hypersonic flow in a shock tunnel. Three-dimensional Navier–Stokes equations are solved with an upwind scheme to simulate the interaction. The pressure at the stagnation point on the blunt body is measured and calculated to examine the pressure variation during the interaction. Schlieren imaging is used in conjunction with the calculated density gradients to examine the process of the interaction. The results show that the experimental pressure at the stagnation point on the blunt body and schlieren imaging fit well with the simulation. The pressure at the stagnation point on the blunt body will increase when the transmission shock approaches the blunt body and decrease with the formation of the rarefied wave. Bow shock is deformed during the interaction. Quasi-stationary waves are formed by high rate laser energy deposition to control the bow shock. The pressure and temperature at the stagnation point on the blunt body and the wave drag are reduced to 50%, 75% and 81% respectively according to the simulation. Schlieren imaging has provided important information for the investigation of the mechanism of the interaction.

  10. Meterwavelength Single-pulse Polarimetric Emission Survey. III. The Phenomenon of Nulling in Pulsars

    Energy Technology Data Exchange (ETDEWEB)

    Basu, Rahul; Mitra, Dipanjan; Melikidze, George I., E-mail: rahulbasu.astro@gmail.com [Janusz Gil Institute of Astronomy, University of Zielona Góra, ul. Szafrana 2, 65–516 Zielona Góra (Poland)

    2017-09-10

    A detailed analysis of nulling was conducted for the pulsars studied in the Meterwavelength Single-pulse Polarimetric Emission Survey. We characterized nulling in 36 pulsars including 17 pulsars where the phenomenon was reported for the first time. The most dominant nulls lasted for a short duration, less than five periods. Longer duration nulls extending to hundreds of periods were also seen in some cases. A careful analysis showed the presence of periodicities in the transition from the null to the burst states in 11 pulsars. In our earlier work, fluctuation spectrum analysis showed multiple periodicities in 6 of these 11 pulsars. We demonstrate that the longer periodicity in each case was associated with nulling. The shorter periodicities usually originate from subpulse drifting. The nulling periodicities were more aligned with the periodic amplitude modulation, indicating a possible common origin for both. The most prevalent nulls last for a single period and can be potentially explained using random variations affecting the plasma processes in the pulsar magnetosphere. On the other hand, longer-duration nulls require changes in the pair-production processes, which need an external triggering mechanism for the changes. The presence of periodic nulling puts an added constraint on the triggering mechanism, which also needs to be periodic.

  11. Single-pulse and burst-mode ablation of gold films measured by quartz crystal microbalance

    Science.gov (United States)

    Andrusyak, Oleksiy G.; Bubelnik, Matthew; Mares, Jeremy; McGovern, Theresa; Siders, Craig W.

    2005-02-01

    Femtosecond ablation has several distinct advantages: the threshold energy fluence for the onset of damage and ablation is orders of magnitude less than for traditional nanosecond laser machining, and by virtue of the rapid material removal of approximately an optical penetration depth per pulse, femtosecond machined cuts can be cleaner and more precise than those made with traditional nanosecond or longer pulse lasers. However, in many materials of interest, especially metals, this limits ablation rates to 10-100 nm/pulse. We present the results of using multiple pulse bursts to significantly increase the per-burst ablation rate compared to a single pulse with the same integrated energy, while keeping the peak intensity of each individual pulse below the air ionization limit. Femtosecond ablation with pulses centered at 800-nm having integrated energy of up to 30 mJ per pulse incident upon thin gold films was measured via resonance frequency shifts in a gold-electrode-coated quartz-crystal oscillator. Measurements were performed using Michelson-interferometer-based burst generators, with up to 2 ns pulse separations, as well as pulse shaping by programmable acousto-optic dispersive filter (Dazzler from FastLite) with up to 2 ps pulse separations.

  12. Single-pulse CARS based multimodal nonlinear optical microscope for bioimaging.

    Science.gov (United States)

    Kumar, Sunil; Kamali, Tschackad; Levitte, Jonathan M; Katz, Ori; Hermann, Boris; Werkmeister, Rene; Považay, Boris; Drexler, Wolfgang; Unterhuber, Angelika; Silberberg, Yaron

    2015-05-18

    Noninvasive label-free imaging of biological systems raises demand not only for high-speed three-dimensional prescreening of morphology over a wide-field of view but also it seeks to extract the microscopic functional and molecular details within. Capitalizing on the unique advantages brought out by different nonlinear optical effects, a multimodal nonlinear optical microscope can be a powerful tool for bioimaging. Bringing together the intensity-dependent contrast mechanisms via second harmonic generation, third harmonic generation and four-wave mixing for structural-sensitive imaging, and single-beam/single-pulse coherent anti-Stokes Raman scattering technique for chemical sensitive imaging in the finger-print region, we have developed a simple and nearly alignment-free multimodal nonlinear optical microscope that is based on a single wide-band Ti:Sapphire femtosecond pulse laser source. Successful imaging tests have been realized on two exemplary biological samples, a canine femur bone and collagen fibrils harvested from a rat tail. Since the ultra-broad band-width femtosecond laser is a suitable source for performing high-resolution optical coherence tomography, a wide-field optical coherence tomography arm can be easily incorporated into the presented multimodal microscope making it a versatile optical imaging tool for noninvasive label-free bioimaging.

  13. Residue specific hydration of primary cell wall potato pectin identified by solid-state 13C single-pulse MAS and CP/MAS NMR spectroscopy

    DEFF Research Database (Denmark)

    Larsen, Flemming Hofmann; Chrestensen, Inge Byg; Damager, Iben

    2011-01-01

    Hydration of rhamnogalacturonan-I (RG-I) derived from potato cell wall was analyzed by 13C single-pulse (SP) magic-angle-spinning (MAS) and 13C cross-polarization (CP) MAS nuclear magnetic resonance (NMR) and supported by 2H SP/MAS NMR experiments. The study shows that the arabinan side chains...... hydrate more readily than the galactan side chains and suggests that the overall hydration properties can be controlled by modifying the ratio of these side chains. Enzymatic modification of native (NA) RG-I provided samples with reduced content of arabinan (sample DA), galactan (sample DG), or both side...... chains (sample DB). Results of these samples suggested that hydration properties were determined by the length and character of the side chains. NA and DA exhibited similar hydration characteristics, whereas DG and DB were difficult to hydrate because of the less hydrophilic properties of the rhamnose...

  14. Surprise in simplicity: an unusual spectral evolution of a single pulse GRB 151006A

    Science.gov (United States)

    Basak, R.; Iyyani, S.; Chand, V.; Chattopadhyay, T.; Bhattacharya, D.; Rao, A. R.; Vadawale, S. V.

    2017-11-01

    We present a detailed analysis of GRB 151006A, the first gamma-ray burst (GRB) detected by AstroSat Cadmium-Zinc-Telluride Imager (CZTI). We study the long-term spectral evolution by exploiting the capabilities of Fermi and Swift satellites at different phases, which is complemented by the polarization measurement with the CZTI. While the light curve of the GRB in different energy bands shows a simple pulse profile, the spectrum shows an unusual evolution. The first phase exhibits a hard-to-soft evolution until ∼16-20 s, followed by a sudden increase in the spectral peak reaching a few MeV. Such a dramatic change in the spectral evolution in the case of a single pulse burst is reported for the first time. This is captured by all models we used namely, Band function, blackbody+Band and two blackbodies+power law. Interestingly, the Fermi Large Area Telescope also detects its first photon (>100 MeV) during this time. This new injection of energy may be associated with either the beginning of afterglow phase, or a second hard pulse of the prompt emission itself that, however, is not seen in the otherwise smooth pulse profile. By constructing Bayesian blocks and studying the hardness evolution we find a good evidence for a second hard pulse. The Swift data at late epochs (>T90 of the GRB) also show a significant spectral evolution consistent with the early second phase. The CZTI data (100-350 keV), though having low significance (1σ), show high values of polarization in the two epochs (77-94 per cent), in agreement with our interpretation.

  15. Meterwavelength Single-pulse Polarimetric Emission Survey. IV. The Period Dependence of Component Widths of Pulsars

    Science.gov (United States)

    Skrzypczak, Anna; Basu, Rahul; Mitra, Dipanjan; Melikidze, George I.; Maciesiak, Krzysztof; Koralewska, Olga; Filothodoros, Alexandros

    2018-02-01

    The core component width in normal pulsars, with periods (P) > 0.1 s, measured at the half-power point at 1 GHz, has a lower boundary line (LBL) that closely follows the P ‑0.5 scaling relation. This result is of fundamental importance for understanding the emission process and requires extended studies over a wider frequency range. In this paper we have carried out a detailed study of the profile component widths of 123 normal pulsars observed in the Meterwavelength Single-pulse Polarimetric Emission Survey at 333 and 618 MHz. The components in the pulse profile were separated into core and conal classes. We found that at both frequencies, the core, as well as the conal component widths versus period, had a LBL that followed the P ‑0.5 relation with a similar lower boundary. The radio emission in normal pulsars has been observationally shown to arise from a narrow range of heights around a few hundred kilometers above the stellar surface. In the past the P ‑0.5 relation has been considered as evidence for emission arising from last open dipolar magnetic field lines. We show that the P ‑0.5 dependence only holds if the trailing and leading half-power points of the component are associated with the last open field line. In such a scenario we do not find any physical motivation that can explain the P ‑0.5 dependence for both core and conal components as evidence for dipolar geometry in normal pulsars. We believe the period dependence is a result of a currently unexplained physical phenomenon.

  16. Object-oriented identification of forested landslides with derivatives of single pulse LiDAR data

    Science.gov (United States)

    Van Den Eeckhaut, Miet; Kerle, Norman; Poesen, Jean; Hervás, Javier

    2012-11-01

    In contrast to the many studies that use expert-based analysis of LiDAR derivatives for landslide mapping in forested terrain, only few studies have attempted to develop (semi-)automatic methods for extracting landslides from LiDAR derivatives. While all these studies are pixel-based, it has not yet been tested whether object-oriented analysis (OOA) could be an alternative. This study investigates the potential of OOA using only single-pulse LiDAR derivatives, such as slope gradient, roughness and curvature to map landslides. More specifically, the focus is on both LiDAR data segmentation and classification of slow-moving landslides in densely vegetated areas, where spectral data do not allow accurate landslide identification. A multistage procedure has been developed and tested in the Flemish Ardennes (Belgium). The procedure consists of (1) image binarization and multiresolution segmentation, (2) classification of landslide parts (main scarps and landslide body segments) and non-landslide features (i.e. earth banks and cropland fields) with supervised support vector machines at the appropriate scale, (3) delineation of landslide flanks, (4) growing of a landslide body starting from its main scarp, and (5) final cleaning of the inventory map. The results obtained show that OOA using LiDAR derivatives allows recognition and characterization of profound morphologic properties of forested deep-seated landslides on soil-covered hillslopes, because more than 90% of the main scarps and 70% of the landslide bodies of an expert-based inventory were accurately identified with OOA. For mountainous areas with bedrock, on the other hand, creation of a transferable model is expected to be more difficult.

  17. SINGLE-PULSE RADIO OBSERVATIONS OF THE GALACTIC CENTER MAGNETAR PSR J1745–2900

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Zhen; Shen, Zhi-Qiang; Wu, Ya-Jun; Zhao, Rong-Bing; Fan, Qing-Yuan; Hong, Xiao-Yu; Jiang, Dong-Rong; Li, Bin; Liang, Shi-Guang; Ling, Quan-Bao; Liu, Qing-Hui; Qian, Zhi-Han; Zhang, Xiu-Zhong; Zhong, Wei-Ye; Ye, Shu-Hua [Shanghai Astronomical Observatory, Chinese Academy of Sciences, Shanghai 200030 (China); Wu, Xin-Ji [Department of Astronomy, Peking University, Beijing 100871 (China); Manchester, R. N. [CSIRO Astronomy and Space Science, P.O. Box 76, Epping, NSW 1710 (Australia); Weltevrede, P. [Jodrell Bank Centre for Astrophysics, School of Physics and Astronomy, University of Manchester, Manchester M13 9PL (United Kingdom); Yuan, Jian-Ping [Key Laboratory of Radio Astronomy, Chinese Academy of Sciences (China); Lee, Ke-Jia, E-mail: yanzhen@shao.ac.cn [Kavli Institute for Astronomy and Astrophysics, Peking University, Beijing 100871 (China)

    2015-11-20

    In this paper, we report radio observations of the Galactic Center magnetar PSR J1745–2900 at six epochs between 2014 June and October. These observations were carried out using the new Shanghai Tian Ma Radio Telescope at a frequency of 8.6 GHz. Both the flux density and integrated profile of PSR J1745–2900 show dramatic changes from epoch to epoch, showing that the pulsar was in its “erratic” phase. On MJD 56836, the flux density of this magnetar was about 8.7 mJy, which was 10 times larger than that reported at the time of discovery, enabling a single-pulse analysis. The emission is dominated by narrow “spiky” pulses that follow a log-normal distribution in peak flux density. From 1913 pulses, we detected 53 pulses whose peak flux densities are 10 times greater than that of the integrated profile. They are concentrated in pulse phase at the peaks of the integrated profile. The pulse widths at the 50% level of these bright pulses were between 0.°2 and 0.°9, much narrower than that of the integrated profile (∼12°). The observed pulse widths may be limited by interstellar scattering. No clear correlation was found between the widths and peak flux density of these pulses and no evidence was found for subpulse drifting. Relatively strong spiky pulses are also detected in the other five epochs of observation, showing the same properties as those detected in MJD 56836. These strong spiky pulses cannot be classified as “giant” pulses but are more closely related to normal pulse emission.

  18. Megajoule-class single-pulse KrF laser test facility as a logical step toward inertial fusion commercialization

    International Nuclear Information System (INIS)

    Harris, D.B.; Pendergrass, J.H.

    1985-01-01

    The cost and efficiency of megajoule-class KrF laser single pulse test facilities have been examined. A baseline design is described which illuminates targets with 5 MJ with shaped 10-ns pulses. The system uses 24 main amplifiers and operates with an optics operating fluence of 4.0 J/cm 2 . This system has 9.0% efficiency and costs $200/joule. Tradeoff studies indicate that large amplifier modules and high fluences lead to the lowest laser system costs, but that only a 20% cost savings can be realized by going to amplifier modules larger than 200 kJ and/or fluences greater than 4 J/cm 2 . The role of the megajoule-class single-pulse test facility towards inertial fusion commercialization will also be discussed

  19. Fabrication and optimization of the copper halide Laser's comparison of the double-discharge (Cu Cl) with the single-pulse operation (Cu Br)

    International Nuclear Information System (INIS)

    Sajad, B.; Behrozinia, S.; Nikzad, P.; Bassam, M. A.

    2009-01-01

    In this paper, the fabrication of a double-pulse copper chloride laser was investigated to study the effect of various parameters such as buffer gas pressure, temperature, and the delay time between two electrical discharge pulses, on laser output power. Moreover, a single-pulse copper bromide laser was fabricated to optimize the laser output power versus temperature, buffer gas pressure, and electrical input power and discharge frequency. The comparison of the results in single-pulse and double-pulse excitation indicates that the former is easier in operation and more power stability can be achieved using single pulse excitation.

  20. Single-pulse characteristics of the Xe(L) amplifier on the Xe35+ (3d→2p) transition array at λ ≅ 2.86 A

    International Nuclear Information System (INIS)

    Borisov, Alex B; Song Xiangyang; Zhang Ping; McCorkindale, John C; Khan, Shahab F; De Jonghe, Richard; Poopalasingam, Sankar; Zhao, Ji; Boyer, Keith; Rhodes, Charles K

    2006-01-01

    The triple comparison of (1) single-pulse spectral data, recorded with a CCD-equipped von Hamos spectrometer both axially and transversely; (2) axially measured time-integrated spectra registered on a film and (3) single-pulse x-ray images of the morphology of the self-trapped plasma channel, recorded simultaneously with the single-pulse spectra, establishes several leading characteristics of the saturated amplification observed on the Xe 35+ transition array at λ ≅ 2.86 A. The chief findings are (α) absolute positive correlation of amplification with the formation of a plasma channel, (β) a perfect spectral match of the amplified transitions in the comparison of axially recorded single-pulse and time-integrated film data and (γ) exact spectral correspondence of both the axially registered single-pulse and time-integrated film data with single-pulse transversely measured spectra exhibiting deep spectral hole burning at the position of the Xe 35+ array. (letter to the editor)

  1. Determination of Size Distributions in Nanocrystalline Powders by TEM, XRD and SAXS

    DEFF Research Database (Denmark)

    Jensen, Henrik; Pedersen, Jørgen Houe; Jørgensen, Jens Erik

    2006-01-01

    Crystallite size distributions and particle size distributions were determined by TEM, XRD, and SAXS for three commercially available TiO2 samples and one homemade. The theoretical Guinier Model was fitted to the experimental data and compared to analytical expressions. Modeling of the XRD spectra...... the size distribution obtained from the XRD experiments; however, a good agreement was obtained between the two techniques. Electron microscopy, SEM and TEM, confirmed the primary particle sizes, the size distributions, and the shapes obtained by XRD and SAXS. The SSEC78 powder and the commercially...

  2. A RD-ESPRIT algorithm for coherent DOA estimation in monostatic MIMO radar using a single pulse

    Science.gov (United States)

    Chen, Chen; Zhang, Xiaofei

    2014-08-01

    This paper discusses the problem of coherent direction of arrival (DOA) estimation in a monostatic multi-input multi-output (MIMO) radar using a single pulse, and proposes a reduced dimension (RD)-estimation of signal parameters via rotational invariance techniques (ESPRIT) algorithm. We reconstruct the received data and then utilise it to construct a set of Toeplitz matrices. After that, we use RD-ESPRIT to obtain the DOAs of the sources. The proposed algorithm is effective for coherent angle estimation based on a single pulse, and it has much better angle estimation performance than the forward backward spatial smoothing (FBSS)-ESPRIT algorithm and the ESPRIT-like of Li, as well as very close angle estimation performance to the ESPRIT-like of Han. For complexity comparison, our algorithm has very close complexity to the FBSS-ESPRIT algorithm, and lower complexity than the ESPRIT-like of Han and the ESPRIT-like of Li. Simulation results present the effectiveness and improvement of our approach.

  3. Secondary plasma formation after single pulse laser ablation underwater and its advantages for laser induced breakdown spectroscopy (LIBS).

    Science.gov (United States)

    Gavrilović, M R; Cvejić, M; Lazic, V; Jovićević, S

    2016-06-07

    In this work we present studies of spatial and temporal plasma evolution after single pulse ablation of an aluminium target in water. The laser ablation was performed using 20 ns long pulses emitted at 1064 nm. The plasma characterization was performed by fast photography, the Schlieren technique, shadowgraphy and optical emission spectroscopy. The experimental results indicate the existence of two distinct plasma stages: the first stage has a duration of approximately 500 ns from the laser pulse, and is followed by a new plasma growth starting from the crater center. The secondary plasma slowly evolves inside the growing vapor bubble, and its optical emission lasts over several tens of microseconds. Later, the hot glowing particles, trapped inside the vapor cavity, were detected during the whole cycle of the bubble, where the first collapse occurs after 475 μs from the laser pulse. Differences in the plasma properties during the two evolution phases are discussed, with an accent on the optical emission since its detection is of primary importance for LIBS. Here we demonstrate that the LIBS signal quality in single pulse excitation underwater can be greatly enhanced by detecting only the secondary plasma emission, and also by applying long acquisition gates (in the order of 10-100 μs). The presented results are of great importance for LIBS measurements inside a liquid environment, since they prove that a good analytical signal can be obtained by using nanosecond pulses from a single commercial laser source and by employing cost effective, not gated detectors.

  4. XRD and HREM studies of nanocrystalline Cu and Pd

    International Nuclear Information System (INIS)

    Nieman, G.W.; Weertmen, J.R.; Siegel, R.W.

    1991-01-01

    Consolidated powders of nanocrystalline Cu and Pd have been studied by x-ray diffraction (XRD) and high resolution electron microscopy (HREM) as part of an investigation of the mechanical behavior of nanocrystalline pure metals. XRD line broadening measurements were made to estimate rain size, qualitative grain size distribution and average long range strains in a number of samples. Mean grain sized range from 4-60 nm and have qualitatively narrow grain size distributions. Long range lattice strains are of the order of 0.2-3% in consolidated samples. These strains apparently persist and even increase in Cu samples after annealing at 0.35 Tm (498K) for 2h, accompanied by an apparent increase in grain size of ≥2x. Grain size, grain size distribution width and internal strains vary somewhat among samples produced under apparently identical processing conditions. HREM studies show that twins, stacking faults and low-index facets are abundant in as-consolidated nanocrystalline Cu samples. In this paper methodology, results and analysis of XRD and HREM experiments are presented

  5. Sampling system for fast single pulses; Realisation d'un dispositif d'echantillonnage d'un signal bref unique

    Energy Technology Data Exchange (ETDEWEB)

    Zenatti, D [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1969-07-01

    Development of a device for the enlargement of the domain of application of classical oscilloscopes to the observation of fast single pulses by application of the sampling principle. Its principal characteristics are: Bandwidth of 700 MHz; Maximum sensibility of 50 mV; Maximum amplitude of input signal of {+-} 1 V; Number of samples of 16; Samples separation of 0,2 ns. (author) [French] Realisation d'un dispositif permettant d'elargir le domaine d'utilisation des oscilloscopes classiques en appliquant le principe de l'echantillonnage a l'observation d'un signal bref unique. Les principales caracteristiques sont les suivantes: Bande passante de 700 MHz; Sensibilite maximale de 50 mV; Amplitude maximale du signal a echantillonner de {+-} 1 V; Nombre de points d'echantillonnage de 16; Pas d'echantillonnage de 0,2 ns. (auteur)

  6. 15N incorporation into organ proteins of newborn rats following single pulse-labelling with different tracers

    International Nuclear Information System (INIS)

    Wutzke, K.D.; Plath, C.; Richter, I.; Heine, W.; Zhukova, T.P.; Sorokina, E.G.; Friedrich, M.

    1987-01-01

    A short-chain 15 N-peptide mixture characterized by an average chain length of 2.3 was obtained when 15 N-labelled yeast protein was hydrolyzed enzymatically by thermitase from Thermoactinomyces vulgaris. Fifteen newborn Wistar rats were given a single pulse of [ 15 N]glycine. [ 15 N]H 4 Cl and [ 15 N]yeast protein thermitasehydrolysate (YPTH) in a dosage of 50 mg 15 N excess kg -1 by gastric tube. In comparison with [ 15 N]glycine the 15 N incorporation rates of brain, muscle and liver were approximately 150% higher after [ 15 N]YPTH application. Uniform labelling, high 15 N enrichment, almost complete absorption, avoidance of imbalances and the low price make this tracer substance superior to other tracers conventionally used for organ labelling. (author)

  7. The Israeli EA-FEL Upgrade Towards Long Pulse Operation for Ultra-High Resolution Single Pulse Coherent Spectroscopy

    CERN Document Server

    Gover, A; Kanter, M; Kapilevich, B; Litvak, B; Peleg, S; Socol, Y; Volshonok, M

    2005-01-01

    The Israeli Electrostatic Accelerator FEL (EA-FEL) is now being upgraded towards long pulse (1005s) operation and ultra-high resolution (10(-6)) single pulse coherent spectroscopy. We present quantitative estimations regarding the applications of controlled radiation chirp for spectroscopic applications with pulse-time Fourier Transform limited spectral resolution. Additionally, we describe a novel extraction-efficiency-improving scheme based on increase of accelerating voltage (boosting) after saturation is achieved. The efficiency of the proposed scheme is confirmed by theoretical and numerical calculations. The latter are performed using software, based on 3D space-frequency domain model. The presentation provides an overview of the upgrade status: the high-voltage terminal is being reconfigured to accept the accelerating voltage boost system; a new broad band low-loss resonator is being manufactured; multi-stage depressed collector is assembled.

  8. Expansion-limited aggregation of nanoclusters in a single-pulse laser-produced plume

    International Nuclear Information System (INIS)

    Gamaly, E. G.; Madsen, N. R.; Rode, A. V.; Golberg, D.

    2009-01-01

    Formation of carbon nanoclusters in a single-laser-pulse created ablation plume was studied both in vacuum and in a noble gas environment at various pressures. The developed theory provides cluster radius dependence on combination of laser parameters, properties of ablated material, and type and pressure of an ambient gas in agreement with experiments. The experiments were performed on carbon nanoclusters formed by laser ablation of graphite targets with 12 picosecond 532 nm laser pulses at MHz-range repetition rate in a broad range of ambient He, Ar, Kr, and Xe gas pressures from 2x10 -2 to 1500 Torr. The experimental results confirmed our theoretical prediction that the average size of the nanoparticles depends weakly on the type of the ambient gas used, and is determined exclusively by the single laser pulse parameters even at the repetition rate as high as 28 MHz with the time gap 36 ns between the pulses. The most important finding relates to the fact that in vacuum the cluster size is mainly determined by hydrodynamic expansion of the plume while in the ambient gas it is controlled by atomic diffusion in the gas. We demonstrate that the ultrashort pulses can be used for production of clusters with the size less than the critical value, which separates the particles with properties drastically different from those of a material in a bulk. The presented results of experiments on formation of carbon nanoclusters are in close agreement with the theoretical scaling. The developed theory is applicable for cluster formation from any monatomic material, such as silicon for example.

  9. Characterization of uranium silicide powder using XRD

    International Nuclear Information System (INIS)

    Garcia, Rafael H.L.; Saliba-Silva, Adonis M.; Carvalho, Elita F.U.; Lima, Nelson B.; Ichikawa, Rodrigo U.; Martinez, Luiz G.

    2013-01-01

    Uranium silicide (U 3 Si 2 ) is an intermetallic used as nuclear fuel in most modern MTR - Materials Test Reactor. Dispersed in aluminum, this fuel allows high uranium densities, up to 4.8 gU/cm 3 . At IPEN, the fabrication of fuel elements based on U 3 Si 2 for the IEA-R1 reactor is carried out in the Nuclear Fuel Center (CCN), by vacuum induction melting of uranium and silicon, followed by grinding. Before employed in a nuclear reactor, U 3 Si 2 must be submitted to a strict quality control, which includes granulometry, density, X-ray radiography for dispersion homogeneity, chemical and crystallographic characterization. Concerning phase composition for a qualified fuel, the fraction of U 3 Si 2 should be higher than 80wt.%. Aiming at the development of a routine methodology for quantification of phases via analysis of XRD data using the Rietved method, six samples from two production baths of CCN were submitted to X-ray diffraction. The data were analyzed using software GSAS and line profile analysis methods. The results suggest that fusion product have preferred orientation and grinding step is important for a better refinement. (author)

  10. Pressure Distribution on Inner Wall of Parabolic Nozzle in Laser Propulsion with Single Pulse

    Science.gov (United States)

    Cui, Cunyan; Hong, Yanji; Wen, Ming; Song, Junling; Fang, Juan

    2011-11-01

    A system based of dynamic pressure sensors was established to study the time resolved pressure distribution on the inner wall of a parabolic nozzle in laser propulsion. Dynamic calibration and static calibration of the test system were made and the results showed that frequency response was up to 412 kHz and linear error was less than 10%. Experimental model was a parabolic nozzle and three test points were preset along one generating line. This study showed that experimental results agreed well with those obtained by numerical calculation way in pressure evolution tendency. The peak value of the calculation was higher than that of the experiment at each tested orifice because of the limitation of the numerical models. The results of this study were very useful for analyzing the energy deposition in laser propulsion and modifying numerical models.

  11. Applications of the rotating orientation XRD method to oriented materials

    International Nuclear Information System (INIS)

    Guo Zhenqi; Li Fei; Jin Li; Bai Yu

    2009-01-01

    The rotating orientation x-ray diffraction (RO-XRD) method, based on conventional XRD instruments by a modification of the sample stage, was introduced to investigate the orientation-related issues of such materials. In this paper, we show its applications including the determination of single crystal orientation, assistance in crystal cutting and evaluation of crystal quality. The interpretation of scanning patterns by RO-XRD on polycrystals with large grains, bulk material with several grains and oriented thin film is also presented. These results will hopefully expand the applications of the RO-XRD method and also benefit the conventional XRD techniques. (fast track communication)

  12. Dose rate effect on micronuclei induction in human blood lymphocytes exposed to single pulse and multiple pulses of electrons.

    Science.gov (United States)

    Acharya, Santhosh; Bhat, N N; Joseph, Praveen; Sanjeev, Ganesh; Sreedevi, B; Narayana, Y

    2011-05-01

    The effects of single pulses and multiple pulses of 7 MV electrons on micronuclei (MN) induction in cytokinesis-blocked human peripheral blood lymphocytes (PBLs) were investigated over a wide range of dose rates per pulse (instantaneous dose rate). PBLs were exposed to graded doses of 2, 3, 4, 6, and 8 Gy of single electron pulses of varying pulse widths at different dose rates per pulse, ranging from 1 × 10(6) Gy s(-1) to 3.2 × 10(8) Gy s(-1). Different dose rates per pulse were achieved by changing the dose per electron pulse by adjusting the beam current and pulse width. MN yields per unit absorbed dose after irradiation with single electron pulses were compared with those of multiple pulses of electrons. A significant decrease in the MN yield with increasing dose rates per pulse was observed, when dose was delivered by a single electron pulse. However, no reduction in the MN yield was observed when dose was delivered by multiple pulses of electrons. The decrease in the yield at high dose rates per pulse suggests possible radical recombination, which leads to decreased biological damage. Cellular response to the presence of very large numbers of chromosomal breaks may also alter the damage.

  13. Saturated multikilovolt x-ray amplification with Xe clusters: single-pulse observation of Xe(L) spectral hole burning

    International Nuclear Information System (INIS)

    Borisov, Alex B; Davis, Jack; Song, Xiangyang; Koshman, Yevgeniya; Dai Yang; Boyer, Keith; Rhodes, Charles K

    2003-01-01

    Single-pulse measurements of spectral hole burning of Xe(L) 3d → 2p hollow atom transition arrays observed from a self-trapped plasma channel provide new information on the dynamics of saturated amplification in the λ ∼ 2.8-2.9 A region. The spectral hole burning on transitions in the Xe 34+ and Xe 35+ arrays reaches full suppression of the spontaneous emission and presents a corresponding width Δ h-bar ω x ∼ = 60 eV, a value adequate for efficient amplification of multikilovolt x-ray pulses down to a limiting length τ x ∼ 30 as. The depth of the suppression at 2.86 A indicates that the gain-to-loss ratio is ≥10. An independent determination of the x-ray pulse energy from damage produced on the surface of a Ti foil in the far field of the source gives a pulse energy of 20-30 μJ, a range that correlates well with the observation of the spectral hole burning and indicates an overall extraction efficiency of ∼10%. (letter to the editor)

  14. Shifts in the metabolic function of a benthic estuarine microbial community following a single pulse exposure to silver nanoparticles

    International Nuclear Information System (INIS)

    Echavarri-Bravo, Virginia; Paterson, Lynn; Aspray, Thomas J.; Porter, Joanne S.; Winson, Michael K.; Thornton, Barry; Hartl, Mark G.J.

    2015-01-01

    The increasing use of silver nanoparticles (AgNPs) as a biocidal agent and their potential accumulation in sediments may threaten non-target natural environmental bacterial communities. In this study a microcosm approach was established to investigate the effects of well characterized OECD AgNPs (NM-300) on the function of the bacterial community inhabiting marine estuarine sediments (salinity 31‰). The results showed that a single pulse of NM-300 AgNPs (1 mg L −1 ) that led to sediment concentrations below 6 mg Ag kg −1 dry weight inhibited the bacterial utilization of environmentally relevant carbon substrates. As a result, the functional diversity changed, but recovered after 120 h under the experimental conditions. This microcosm study suggests that AgNPs under environmentally relevant experimental conditions can negatively affect bacterial function and provides an insight into the understanding of the bacterial community response and resilience to AgNPs exposure, important for informing relevant regulatory measures. - Highlights: • AgNPs affected the bacterial community function in estuarine marine sediments. • AgNPs inhibited the bacterial utilization of environmentally relevant substrates. • Heterotrophic bacterial groups showed resilience to AgNPs after 120 h exposure. • AgNPs did not affect the bacterial community structure in sediments. - AgNPs inhibited the bacterial utilization of environmentally relevant substrates and caused temporary shifts in the bacterial functional diversity in marine estuarine sediments

  15. Long-duration nano-second single pulse lasers for observation of spectra from bulk liquids at high hydrostatic pressures

    International Nuclear Information System (INIS)

    Thornton, Blair; Sakka, Tetsuo; Masamura, Tatsuya; Tamura, Ayaka; Takahashi, Tomoko; Matsumoto, Ayumu

    2014-01-01

    The influence of laser pulse duration on the spectral emissions observed from bulk ionic solutions has been investigated for hydrostatic pressures between 0.1 and 30 MPa. Transient pressure, shadowgraph imaging and spectroscopic measurements were performed for single pulses of duration 20 and 150 ns. The transient pressure measurements show that for hydrostatic pressures up to 30 MPa, propagation of the high-pressure shockwave generated by the focused laser causes the local pressure to reduce below ambient levels during the time frame that spectroscopic measurements can be made. The pressure impulse and subsequent reduction in pressure are larger, with the latter lasting longer for the 150 ns pulse compared to a 20 ns pulse of the same energy. The 150 ns pulse generates larger cavities with significant enhancement of the spectral emissions observed compared to the 20 ns duration pulse for pressures up to 30 MPa. The results demonstrate that laser-induced breakdown using a long ns duration pulse offers an advantage over conventional, short ns duration pulses for the analysis of bulk ionic solutions at hydrostatic pressures between 0.1 and 30 MPa. - Highlights: • Long-ns-duration laser pulses enhance the spectra observed from bulk solutions. • Laser-induced shockwaves momentarily reduce pressures to below ambient levels. • 150 ns pulses generate larger cavities than 20 ns pulses of the same energy. • Hydrostatic pressures < 30 MPa have no significant effect on the observed spectra

  16. Proxy-based accelerated discovery of Fischer–Tropsch catalysts† †Electronic supplementary information (ESI) available: Details of synthesis, analysis and testing, validation experiments for high-throughput XRD and gas treatment, details of statistical analysis and calculations, tabulation of synthesis parameters and XRD results, alternatives to Fig. 3 highlighting different data points, FTS testing results displayed graphically. See DOI: 10.1039/c4sc02116a Click here for additional data file.

    Science.gov (United States)

    Boldrin, Paul; Gallagher, James R.; Combes, Gary B.; Enache, Dan I.; James, David; Ellis, Peter R.; Kelly, Gordon; Claridge, John B.

    2015-01-01

    Development of heterogeneous catalysts for complex reactions such as Fischer–Tropsch synthesis of fuels is hampered by difficult reaction conditions, slow characterisation techniques such as chemisorption and temperature-programmed reduction and the need for long term stability. High-throughput (HT) methods may help, but their use has until now focused on bespoke micro-reactors for direct measurements of activity and selectivity. These are specific to individual reactions and do not provide more fundamental information on the materials. Here we report using simpler HT characterisation techniques (XRD and TGA) along with ageing under Fischer–Tropsch reaction conditions to provide information analogous to metal surface area, degree of reduction and thousands of hours of stability testing time for hundreds of samples per month. The use of this method allowed the identification of a series of highly stable, high surface area catalysts promoted by Mg and Ru. In an advance over traditional multichannel HT reactors, the chemical and structural information we obtain on the materials allows us to identify the structural effects of the promoters and their effects on the modes of deactivation observed. PMID:29560180

  17. Sensitive detection of chlorine in iron oxide by single pulse and dual pulse laser-induced breakdown spectroscopy

    Science.gov (United States)

    Pedarnig, J. D.; Haslinger, M. J.; Bodea, M. A.; Huber, N.; Wolfmeir, H.; Heitz, J.

    2014-11-01

    The halogen chlorine is hard to detect in laser-induced breakdown spectroscopy (LIBS) mainly due to its high excited state energies of 9.2 and 10.4 eV for the most intense emission lines at 134.72 nm and 837.59 nm, respectively. We report on sensitive detection of Cl in industrial iron oxide Fe2O3 powder by single-pulse (SP) and dual-pulse (DP) LIBS measurements in the near infrared range in air. In compacted powder measured by SP excitation (Nd:YAG laser, 532 nm) Cl was detected with limit of detection LOD = 440 ppm and limit of quantitation LOQ = 720 ppm. Orthogonal DP LIBS was studied on pressed Fe2O3 pellets and Fe3O4 ceramics. The transmission of laser-induced plasma for orthogonal Nd:YAG 1064 nm and ArF 193 nm laser pulses showed a significant dependence on interpulse delay time (ipd) and laser wavelength (λL). The UV pulses (λL = 193 nm) were moderately absorbed in the plasma and the Cl I emission line intensity was enhanced while IR pulses (λL = 1064 nm) were not absorbed and Cl signals were not enhanced at ipd = 3 μs. The UV laser enhancement of Cl signals is attributed to the much higher signal/background ratio for orthogonal DP excitation compared to SP excitation and to the increased plasma temperature and electron number density. This enabled measurement at a very short delay time of td ≥ 0.1 μs with respect to the re-excitation pulse and detection of the very rapidly decaying Cl emission with higher efficiency.

  18. Simulation investigation of thermal phase transformation and residual stress in single pulse EDM of Ti-6Al-4V

    Science.gov (United States)

    Tang, Jiajing; Yang, Xiaodong

    2018-04-01

    The thermal phase transformation and residual stress are ineluctable in the electrical discharge machining (EDM) process, and they will greatly affect the working performances of the machined surface. This paper presents a simulation study on the thermal phase transformation and residual stress in single-pulse EDM of Ti-6Al-4V, which is the most popular titanium alloy in fields such as aircraft engine and some other leading industries. A multi-physics model including thermal, hydraulic, metallography and structural mechanics was developed. Based on the proposed model, the thickness and metallographic structure of the recast layer and heat affected layer (HAZ) were investigated. The distribution and characteristics of residual stress around the discharge crater were obtained. The recast layer and HAZ at the center of crater are found to be the thinnest, and their thicknesses gradually increase approaching the periphery of the crater. The recast layer undergoes a complete α‧ (martensitic) transformation, while the HAZ is mainly composed by the α  +  β  +  α‧ three-phase microstructure. Along the depth direction of crater, the Von Mises stress increases first and then decreases, reaching its maximal value near the interface of recast layer and HAZ. In the recast layer, both compressive stress component and tensile stress component are observed. ANOVA results showed that the influence of discharge current on maximal tensile stress is more significant than that of pulse duration, while the pulse duration has more significant influence on average thickness of the recast layer and the depth location of the maximal tensile stress. The works conducted in this study will help to evaluate the quality and integrity of EDMed surface, especially when the non-destructive testing is difficult to achieve.

  19. [Identification of Dens Draconis and Os Draconis by XRD method].

    Science.gov (United States)

    Chen, Guang-Yun; Wu, Qi-Nan; Shen, Bei; Chen, Rong

    2012-04-01

    To establish an XRD method for evaluating the quality of Os Draconis and Dens Draconis and applying in judgement of the counterfeit. Dens Draconis, Os Draconis and the counterfeit of Os Draconis were analyzed by XRD. Their diffraction patterns were clustered analysis and evaluated their similarity degree. Established the analytical method of Dens Draconis and Os Draconis basing the features fingerprint information of the 10 common peaks by XRD pattern. Obtained the XRD pattern of the counterfeit of Os Draconis. The similarity degree of separate sources of Dens Draconis was high,while the similarity degree of separate sources of Os Draconis was significant different from each other. This method can be used for identification and evaluation of Os Draconis and Dens Draconis. It also can be used for identification the counterfeit of Os Draconis effectively.

  20. Deep tissue optical imaging of upconverting nanoparticles enabled by exploiting higher intrinsic quantum yield through use of millisecond single pulse excitation with high peak power

    DEFF Research Database (Denmark)

    Liu, Haichun; Xu, Can T.; Dumlupinar, Gökhan

    2013-01-01

    We have accomplished deep tissue optical imaging of upconverting nanoparticles at 800 nm, using millisecond single pulse excitation with high peak power. This is achieved by carefully choosing the pulse parameters, derived from time-resolved rate-equation analysis, which result in higher intrinsic...... quantum yield that is utilized by upconverting nanoparticles for generating this near infrared upconversion emission. The pulsed excitation approach thus promises previously unreachable imaging depths and shorter data acquisition times compared with continuous wave excitation, while simultaneously keeping...... therapy and remote activation of biomolecules in deep tissues....

  1. XRD spectra of new YBaCuO superconductors

    Indian Academy of Sciences (India)

    superconductors of YBaCuO materials by solid state reac- tion. They used the ... The XRD spectra and critical temperatures are shown to be the same as that of ... samples were synthesized by solid state reaction using raw materials Y2O3 ...

  2. Qualitative soil mineral analysis by EDXRF, XRD and AAS probes

    International Nuclear Information System (INIS)

    Singh, Virendra; Agrawal, H.M.

    2012-01-01

    Soil minerals study is vital in terms of investigating the major soil forming compounds and to find out the fate of minor and trace elements, essential for the soil–plant interaction purpose. X-ray diffraction (XRD) has been a popular technique to search out the phases for different types of samples. For the soil samples, however, employing XRD is not so straightforward due to many practical problems. In the current approach, principal component analysis (PCA) has been used to have an idea of the minerals present, in qualitative manner, in the soil under study. PCA was used on the elemental concentrations data of 17 elements, determined by the energy dispersive X-ray fluorescence (EDXRF) technique. XRD analysis of soil samples has been done also to identify the minerals of major elements. Some prior treatments, like removal of silica by polytetrafluoroethylene (PTFE) slurry and grinding with alcohol, were given to samples to overcome the peak overlapping problems and to attain fine particle size which is important to minimize micro-absorption corrections, to give reproducible peak intensities and to minimize preferred orientation. A 2θ step of 0.05°/min and a longer dwell time than normal were used to reduce interferences from background noise and to increase the counting statistics. Finally, the sequential extraction procedure for metal speciation study has been applied on soil samples. Atomic absorption spectroscopy (AAS) was used to find the concentrations of metal fractions bound to various forms. Applying all the three probes, the minerals in the soils can be studied and identified, successfully. - Highlights: ► Qualitative soil minerals analysis by EDXRF, AAS and XRD methods. ► There is a requirement of other means and methods due to inadequacy of XRD. ► Principal component analysis (PCA) provides an idea of minerals present in soil. ► Trace elements complexes can be determined by AAS probe. ► EDXRF, AAS and XRD, in combination, enable

  3. Sampling system for fast single pulses; Realisation d'un dispositif d'echantillonnage d'un signal bref unique

    Energy Technology Data Exchange (ETDEWEB)

    Zenatti, D. [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1969-07-01

    Development of a device for the enlargement of the domain of application of classical oscilloscopes to the observation of fast single pulses by application of the sampling principle. Its principal characteristics are: Bandwidth of 700 MHz; Maximum sensibility of 50 mV; Maximum amplitude of input signal of {+-} 1 V; Number of samples of 16; Samples separation of 0,2 ns. (author) [French] Realisation d'un dispositif permettant d'elargir le domaine d'utilisation des oscilloscopes classiques en appliquant le principe de l'echantillonnage a l'observation d'un signal bref unique. Les principales caracteristiques sont les suivantes: Bande passante de 700 MHz; Sensibilite maximale de 50 mV; Amplitude maximale du signal a echantillonner de {+-} 1 V; Nombre de points d'echantillonnage de 16; Pas d'echantillonnage de 0,2 ns. (auteur)

  4. XRD Investigation of Some Thermal Degraded Starch Based Materials

    Directory of Open Access Journals (Sweden)

    Mihai Todica

    2016-01-01

    Full Text Available The thermal degradation of some starch based materials was investigated using XRD method. The samples were obtained by thermal extrusion of mixtures of different proportions of starch, glycerol, and water. Such materials are suitable for the manufacturing of low pollutant packaging. Thermal degradation is one of the simplest ways to destroy such materials and this process is followed by structural modification of the local ordering of samples, water evaporation, crystallization, oxidation, or destruction of the chemical bonds. These modifications need to be studied in order to reduce to the minimum production of pollutant residues by burning process. XRD measurements show modification of the local ordering of the starch molecules depending on the temperature and initial composition of the samples. The molecular ordering perturbation is more pronounced in samples with low content of starch.

  5. Quantitative XRD analysis of {110} twin density in biotic aragonites.

    Science.gov (United States)

    Suzuki, Michio; Kim, Hyejin; Mukai, Hiroki; Nagasawa, Hiromichi; Kogure, Toshihiro

    2012-12-01

    {110} Twin densities in biotic aragonite have been estimated quantitatively from the peak widths of specific reflections in powder X-ray diffraction (XRD) patterns, as well as direct confirmation of the twins using transmission electron microscopy (TEM). Influence of the twin density on the peak widths in the XRD pattern was simulated using DIFFaX program, regarding (110) twin as interstratification of two types of aragonite unit layers with mirrored relationship. The simulation suggested that the twin density can be estimated from the difference of the peak widths between 111 and 021, or between 221 and 211 reflections. Biotic aragonite in the crossed-lamellar microstructure (three species) and nacreous microstructure (four species) of molluscan shells, fish otoliths (two species), and a coral were investigated. The XRD analyses indicated that aragonite crystals in the crossed-lamellar microstructure of the three species contain high density of the twins, which is consistent with the TEM examination. On the other hand, aragonite in the nacre of the four species showed almost no difference of the peak widths between the paired reflections, indicating low twin densities. The results for the fish otoliths were varied between the species. Such variation of the twin density in biotic aragonites may reflect different schemes of crystal growth in biomineralization. Copyright © 2012 Elsevier Inc. All rights reserved.

  6. XRD is the main key to the mechanochemical processing

    International Nuclear Information System (INIS)

    Mozaffari, M.; Amighian, J.

    2000-01-01

    Mechanochemical processing is a process that makes use of chemical reactions mechanically activated by high-energy ball milling (HEBM). This technique has been the subject of great interest in recent years due to its promise for producing improved novel materials. Ultra fine powders in the range 10-100 nm can be obtained by mixing the right ratio of the components, appropriate for a desired phase. These raw materials together with several hardened-steel vial and milled for an optimum time using Spex or Planetary mills. In this process 2 factors, milling time and the ball to powder mass ratio, should carefully be optimized. These will be checked by successive XRD patterns. To see the ability of XRD in this technique, some single phase Ni-Al and Mn ferrites were prepared. The main key to the formation of different phases at any stage of processing was XRD patterns. Also by using Scherrer formula it was possible to measure the particle size of the milled powders. (Author)

  7. XRD and SEM analysis of hydroxyapatite during immersion in stimulated physiological solutions

    International Nuclear Information System (INIS)

    Yusof Abdullah; Idris Besar; Rosmamuhamadani Ramli; Abd Razak Daud

    2000-01-01

    XRD and SEM techniques were used to analyse the apatite layer developed on the synthetic hydroxyapatite surface following immersion in the simulated body fluid (SBF) that mimics the conditions of material experiences after implantation in the human body. Initially, the new layers formed after 7 day's incubation and increased with immersion time as crystallization of apatite phase. The XRD confirmed that the deposited layer was hydroxyapatite and crystallographically. With time, the crystal growth become more random and the intensity of the peaks decreased. During immersion, hydroxyapatite was precipitated from the SBF and coherently scattered with very small crystal. The SEM observation shows that the new precipitates were increased as well as incubation period increased. Therefore, hydroxyapatite ceramics are suggested to have very good biocompatibility. (Author)

  8. Single-pulse measurement of density and temperature in a turbulent, supersonic flow using UV laser spectroscopy

    Science.gov (United States)

    Fletcher, D. G.; Mckenzie, R. L.

    1992-01-01

    Nonintrusive measurements of density and temperature and their turbulent fluctuation levels have been obtained in the boundary layer of an unseeded, Mach 2 wind tunnel flow. The spectroscopic technique that was used to make the measurements is based on the combination of laser-induced oxygen fluorescence and Raman scattering by oxygen and nitrogen from the same laser pulse. Results from this demonstration experiment compare favorably with previous measurements obtained in the same facility from conventional probes and an earlier spectroscopic technique.

  9. XRD and SEM study of alumina silicate porcelain insulator

    Science.gov (United States)

    Duddi, Dharmender; Singh, G. P.; Kalra, Swati; Shekhawat, M. S.; Tak, S. K.

    2018-05-01

    Higher strength electrical porcelain is a requirement of industry. This will be achieved by a specific composition of raw materials, which is consisted of clays and feldspars. Water absorption, particle size and insulating properties are of special interest now a day. China clay, Ball clay and Quartz are widely used by ceramic industries in Bikaner district of Rajasthan. Sample for present study were prepared by mixing of above clay, feldspar with MnO2, then shrinkage is observed. Bar shaped samples were prepared and heated up to a temperature of about 1185° C to observe shrinkage. For phase study of XRD and SEM are observed.

  10. A new method for obtaining time resolved optical spectra of transients produced by a single pulse of electrons

    International Nuclear Information System (INIS)

    Gordon, S.; Schmidt, K.H.; Martin, J.E.

    1975-01-01

    The essential features of the kinetic spectroscopic method and the kinetic spectrophotometric method are summarized. It is stated that the new method embodies some of the advantages of both. A diagram of the apparatus is shown. This is essentially a version of a conventional pulse radiolysis experimental arrangement with the modification that the usual monochromator is replaced by a spectrograph equipped with a horizontal and a vertical slit and the usual photomultiplier-amplifier detector is replaced by a streak camera (TRW) incorporating an image converter tube (ICT) and a TV camera interfaced to a 2000 channel Biomation transient recorder. The time resolved absorption spectrum (or emission spectrum) is displayed on the P-11 phosphor of the ICT. This image is focussed on the photoelements of the TV tube. The TV camera scans the image of the spectrum stored on these elements and the output of this scan is stored in the Biomation. This recorder is in turn interfaced to a Sigma 5 computer. Results are presented for several experiments, from which it is concluded that with the present equipment absorbances down to 0.02 can be measured, and a time resolution of 1ns can be achieved. It is stated that with improved equipment it should be possible to extend the time resolution of the method to less than 50 picoseconds. (U.K.)

  11. Green synthesis of silver nanoparticles and their characterization by XRD

    Science.gov (United States)

    Mehta, B. K.; Chhajlani, Meenal; Shrivastava, B. D.

    2017-05-01

    A cost effective and environment friendly technique for green synthesis of silver nanoparticles has been reported. Silver nanoparticles have been synthesized using ethanol extract of fruits of Santalum album (Family Santalaceae), commonly known as East Indian sandalwood. Fruits of S.album were collected and crushed. Ethanol was added to the crushed fruits and mixture was exposed to microwave for few minutes. Extract was concentrated by Buchi rotavaporator. To this extract, 1mM aqueous solution of silver nitrate (AgNO3) was added. After about 24 hr incubation Ag+ ions in AgNO3 solution were reduced to Ag atoms by the extract. Silver nanoparticles were obtained in powder form. X-ray diffraction (XRD) pattern of the prepared sample of silver nanoparticles was recorded The diffractogram has been compared with the standard powder diffraction card of JCPDS silver file. Four peaks have been identified corresponding to (hkl) values of silver. The XRD study confirms that the resultant particles are silver nanoparticles having FCC structure. The average crystalline size D, the value of the interplanar spacing between the atoms, d, lattice constant and cell volume have been estimated. Thus, silver nanoparticles with well-defined dimensions could be synthesized by reduction of metal ions due to fruit extract of S.album.

  12. A Combined XRD/XRF Instrument for Lunar Resource Assessment

    Science.gov (United States)

    Vaniman, D. T.; Bish, D. L.; Chipera, S. J.; Blacic, J. D.

    1992-01-01

    Robotic surface missions to the Moon should be capable of measuring mineral as well as chemical abundances in regolith samples. Although much is already known about the lunar regolith, our data are far from comprehensive. Most of the regolith samples returned to Earth for analysis had lost the upper surface, or it was intermixed with deeper regolith. This upper surface is the part of the regolith most recently exposed to the solar wind; as such it will be important to resource assessment. In addition, it may be far easier to mine and process the uppermost few centimeters of regolith over a broad area than to engage in deep excavation of a smaller area. The most direct means of analyzing the regolith surface will be by studies in situ. In addition, the analysis of the impact-origin regolith surfaces, the Fe-rich glasses of mare pyroclastic deposits, are of resource interest, but are inadequately known; none of the extensive surface-exposed pyroclastic deposits of the Moon have been systematically sampled, although we know something about such deposits from the Apollo 17 site. Because of the potential importance of pyroclastic deposits, methods to quantify glass as well as mineral abundances will be important to resource evaluation. Combined x ray diffraction (XRD) and x ray fluorescence (XRF) analysis will address many resource characterization problems on the Moon. XRF methods are valuable for obtaining full major-element abundances with high precision. Such data, collected in parallel with quantitative mineralogy, permit unambiguous determination of both mineral and chemical abundances where concentrations are high enough to be of resource grade. Collection of both XRD and XRF data from a single sample provides simultaneous chemical and mineralogic information. These data can be used to correlate quantitative chemistry and mineralogy as a set of simultaneous linear equations, the solution of which can lead to full characterization of the sample. The use of

  13. Retrospective Study on Laser Treatment of Oral Vascular Lesions Using the "Leopard Technique": The Multiple Spot Irradiation Technique with a Single-Pulsed Wave.

    Science.gov (United States)

    Miyazaki, Hidetaka; Ohshiro, Takafumi; Romeo, Umberto; Noguchi, Tadahide; Maruoka, Yutaka; Gaimari, Gianfranco; Tomov, Georgi; Wada, Yoshitaka; Tanaka, Kae; Ohshiro, Toshio; Asamura, Shinichi

    2018-06-01

    This study aimed to retrospectively evaluate the efficacy and safety of laser treatment of oral vascular lesions using the multiple spot irradiation technique with a single-pulsed wave. In laser therapy for vascular lesions, heat accumulation induced by excessive irradiation can cause adverse events postoperatively, including ulcer formation, resultant scarring, and severe pain. To prevent heat accumulation and side effects, we have applied a multiple pulsed spot irradiation technique, the so-called "leopard technique" (LT) to oral vascular lesions. This approach was originally proposed for laser treatment of nevi. It can avoid thermal concentration at the same spot and spare the epithelium, which promotes smooth healing. The goal of the study was to evaluate this procedure and treatment outcomes. The subjects were 46 patients with 47 oral vascular lesions treated with the LT using a Nd:YAG laser (1064 nm), including 24 thick lesions treated using a combination of the LT and intralesional photocoagulation. All treatment outcomes were satisfactory without serious complications such as deep ulcer formation, scarring, bleeding, or severe swelling. Laser therapy with the LT is a promising less-invasive treatment for oral vascular lesions.

  14. Kinetics of the Thermal Decomposition of Tetramethylsilane behind the Reflected Shock Waves in a Single Pulse Shock Tube (SPST) and Modeling Study

    Science.gov (United States)

    Parandaman, A.; Sudhakar, G.; Rajakumar, B.

    Thermal reactions of Tetramethylsilane (TMS) diluted in argon were studied behind the reflected shock waves in a single-pulse shock tube (SPST) over the temperature range of 1085-1221 K and pressures varied between 10.6 and 22.8 atm. The stable products resulting from the decomposition of TMS were identified and quantified using gas chromatography and also verified with Fourier Transform Infrared (FTIR) spectrometer. The major reaction products are methane (CH4) and ethylene (C2H4). The minor reaction products are ethane (C2H6) and propylene (C3H6). The initiation of mechanism in the decomposition of TMS takes plays via the Si-C bond scission by ejecting the methyl radicals (CH3) and trimethylsilyl radicals ((CH3)3Si). The measured temperature dependent rate coefficient for the total decomposition of TMS was to be ktotal = 1.66 ×1015 exp (-64.46/RT) s-1 and for the formation of CH4 reaction channel was to be k = 2.20 × 1014 exp (-60.15/RT) s-1, where the activation energies are given in kcal mol-1. A kinetic scheme containing 17 species and 28 elementary reactions was used for the simulation using chemical kinetic simulator over the temperature range of 1085-1221 K. The agreement between the experimental and simulated results was satisfactory.

  15. Assessment of Event-Related EEG Power After Single-Pulse TMS in Unresponsive Wakefulness Syndrome and Minimally Conscious State Patients.

    Science.gov (United States)

    Formaggio, Emanuela; Cavinato, Marianna; Storti, Silvia Francesca; Tonin, Paolo; Piccione, Francesco; Manganotti, Paolo

    2016-03-01

    In patients without a behavioral response, non-invasive techniques and new methods of data analysis can complement existing diagnostic tools by providing a method for detecting covert signs of residual cognitive function and awareness. The aim of this study was to investigate the brain oscillatory activities synchronized by single-pulse transcranial magnetic stimulation (TMS) delivered over the primary motor area in the time-frequency domain in patients with the unresponsive wakefulness syndrome or in a minimally conscious state as compared to healthy controls. A time-frequency analysis based on the wavelet transform was used to characterize rapid modifications of oscillatory EEG rhythms induced by TMS in patients as compared to healthy controls. The pattern of EEG changes in the patients differed from that of healthy controls. In the controls there was an early synchronization of slow waves immediately followed by a desynchronization of alpha and beta frequency bands over the frontal and centro-parietal electrodes, whereas an opposite early synchronization, particularly over motor areas for alpha and beta and over the frontal and parietal electrodes for beta power, was seen in the patients. In addition, no relevant modification in slow rhythms (delta and theta) after TMS was noted in patients. The clinical impact of these findings could be relevant in neurorehabilitation settings for increasing the awareness of these patients and defining new treatment procedures.

  16. Towards diffractive imaging with single pulses of FEL radiation. Dynamics within irradiatied samples and their influence on the analysis of imaging data

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Fenglin

    2010-08-15

    3D single particle coherent diffraction imaging (CDI) of bioparticles (such as proteins, macromolecules and viruses) is one of the main possible applications of the new generation of light sources: free-electron lasers (FELs), which are now available at FLASH (Hamburg, Germany) and LCLS (Stanford, U.S.A.). The extremely bright and ultrashort FEL pulses potentially enable CDI to achieve high resolution down to subnanometer length scale. However, intense FEL pulses cause serious radiation damage in bioparticles, even during single shots, which may set the resolution limits for CDI with FELs. Currently, since the signal-to-noise ratio is very low for small biological particles, direct experimental study of radiation damage in the single particle imaging is fairly difficult. Single atomic (noble gas) clusters become good objects to reveal effects of radiation damage processes on CDI with FEL radiation. This thesis studies three aspects of the radiation damage problem, which are treated in three independent chapters: (1) Molecular Dynamics simulations to quantitively describe radiation damage processes within irradiated atomic clusters during single pulses; (2) reconstruction analysis of single-shot CDI diffraction patterns of atomic clusters, which may potentially help to understand the radiation damage occurring in biological samples; and (3) testing the effects of coating water layers in CDI, which is supposed to minimize the radiation damage in irradiated bioparticles. (orig.)

  17. Study of archaeological objects by neutron imaging, xrd and xrf

    International Nuclear Information System (INIS)

    Dinca, M.; Dinu, A. D.; Stanciulescu, M. G.; Mandescu, D.

    2015-01-01

    Archaeological objects were borrowed from Arges County History Museum (ACHM) and investigated at the Institute for Nuclear Research (INR). Metallic objects made in iron, copper alloys and silver discovered in southern part of Romania, mostly Dacian and Roman origin, were investigated. For imaging was used the neutron and gamma imaging facility from tangential channel of the TRIGA ACPR to put in evidence the internal structure of the objects. For elemental and chemical composition, concentration levels in objects were performed investigations by X-ray fluorescence (XRF) and X-ray diffraction (XRD). These investigations offer valuable information in archaeological research about composition, structure of the bulk, presence of alteration, inclusions, typology of the location of material extraction, manufacturing techniques etc. This work is an example of application of neutron imaging and other radiation-based analytical methods for cultural heritage research that had the aim to involve some of the non-destructive investigation methods available at INR. (authors)

  18. High temperature XRD of Cu2GeSe3

    International Nuclear Information System (INIS)

    Premkumar, D. S.; Malar, P.; Chetty, Raju; Mallik, Ramesh Chandra

    2015-01-01

    The Cu 2 GeSe 3 is prepared by solid state synthesis method. The high temperature XRD has been done at different temperature from 30 °C to 450 °C. The reitveld refinement confirms Cu 2 GeSe 3 phase and orthorhombic crystal structure. The lattice constants are increasing with increase in the temperature and their rate of increase with respect to temperature are used for finding the thermal expansion coefficient. The calculation of the linear and volume coefficient of thermal expansion is done from 30 °C to 400 °C. Decrease in the values of linear expansion coefficients with temperature are observed along a and c axis. Since thermal expansion coefficient is the consequence of the distortion of atoms in the lattice; this can be further used to find the minimum lattice thermal conductivity at given temperature

  19. Identification of unknown sample using NAA, EDXRF, XRD techniques

    International Nuclear Information System (INIS)

    Dalvi, Aditi A.; Swain, K.K.; Chavan, Trupti; Remya Devi, P.S.; Wagh, D.N.; Verma, R.

    2015-01-01

    Analytical Chemistry Division (ACD), Bhabha Atomic Research Centre (BARC) receives samples from law enforcement agencies such as Directorate of Revenue Intelligence, Customs for analysis. Five unknown grey powdered samples were received for identification and were suspected to be Iridium (Ir). Identification of unknown sample is always a challenging task and suitable analytical techniques have to be judiciously utilized for arriving at the conclusion. Qualitative analysis was carried out using Jordan Valley, EX-3600 M Energy dispersive X-ray fluorescence (EDXRF) spectrometer at ACD, BARC. A SLP series LEO Si (Li) detector (active area: 30 mm 2 ; thickness: 3.5 mm; resolution: 140 eV at 5.9 keV of Mn K X-ray) was used during the measurement and only characteristic X-rays of Ir (Lα: 9.17 keV and Lβ: 10.70 keV) was seen in the X-ray spectrum. X-ray diffraction (XRD) measurement results indicated that the Ir was in the form of metal. To confirm the XRD data, neutron activation analysis (NAA) was carried out by irradiating samples and elemental standards (as comparator) in graphite reflector position of Advanced Heavy Water Reactor Critical Facility (AHWR CF) reactor, BARC, Mumbai. After suitable decay period, gamma activity measurements were carried out using 45% HPGe detector coupled to 8 k multi channel analyzer. Characteristic gamma line at 328.4 keV of the activation product 194 Ir was used for quantification of iridium and relative method of NAA was used for concentration calculations. NAA results confirmed that all the samples were Iridium metal. (author)

  20. Some feature of interpretation of tension single pulsed electromagnetic field of the Earth to create the model parameter fields physical properties

    Directory of Open Access Journals (Sweden)

    Mokritskaya T.P.

    2014-12-01

    Full Text Available Stochastic analysis of the results of different methods of obtaining and processing of information allows us to solve problems on a qualitatively different level. This is important when creating complex earth models and fields of its parameters, particularly the physical properties. Application of remote sensing methods (geophysical investigations with the registration of a single pulse intensity of the electromagnetic field of the Earth (EIEMPZ seismic profiling, is expanding. Interesting results of the joint interpretation of the results of geophysical and laboratory studies of physical soil. Interesting results of the joint interpretation of the results of geophysical and laboratory studies of physical soil. For the first time a methodology for assessing the state of the soil [3] applied for a joint interpretation of materials determine the field strength EMPZ, seismic profiling, and laboratory techniques. This has allowed to characterize the state of the geological environment and to build a model of inhomogeneous density distribution of fractured rocks at depth. In this paper we made a mathematical analysis of the results of research and talus deposits eluvial clay Taurian series, studied at one of the construction sites southern coast at a depth of 12.0 -25.0 m. Methods of statistical analysis, assessment of homogeneity and symmetrically distributed, rank correlation and multiple regression analysis described in [3]. The analysis of the spatial distribution of areas extrem value of EMPZ, heterogeneity of seismic rigidity. Statistical characteristics of indicators of physical properties reflect the genetic characteristics of the formation and the current state of silty-clay sediments of different genesis.It is proved that the regression model can be applied to interpret the state of the array in the construction of geodynamic model. It is established that the creation of forward-looking (dynamic models for the distribution of the physical

  1. Characterization of North American lignite fly ashes. II. XRD Mineralogy

    International Nuclear Information System (INIS)

    McCarthy, G.J.; Johansen, D.M.; Thedchanamoorthy, A.; Steinwand, S.J.; Swanson, K.D.

    1988-01-01

    X-ray powder diffraction has been used to determine the crystalline phase mineralogy in samples of fly ash from each of the lignite mining areas of North America. The characteristic phases of North Dakota lignite fly ashes were periclase, lime, merwinite and the sulfate phases anhydrite, thenardite and a sodalite-structure phase. Mullite was absent in these low-Al/sub 2/O/sub 3/ ashes. Montana lignite ash mineralogy had characteristics of ND lignite and MT subbituminous coal fly ashes; mullite and C/sub 3/A were present and the alkali sulfates were absent. Texas and Louisiana lignite fly ashes had the characteristic mineralogy of bituminous coal fly ash: quartz, mullite, ferrite-spinel (magnetite) and minor hematite. Even though their analytical CaO contents were 7-14%, all but one lacked crystalline CaO-containing phases. Lignite fly ashes from Saskatchewan were generally the least crystalline of those studied and had a mineralogy consisting of quartz, mullite, ferrite spinel and periclase. Quantitative XRD data were obtained. The position of the diffuse scattering maximum in the x-ray diffractograms was indicative of the glass composition of the lignite fly ash

  2. XRD characterisation of nanoparticle size and shape distributions

    International Nuclear Information System (INIS)

    Armstrong, N.; Kalceff, W.; Cline, J.P.; Bonevich, J.

    2004-01-01

    Full text: The form of XRD lines and the extent of their broadening provide useful structural information about the shape, size distribution, and modal characteristics of the nanoparticles comprising the specimen. Also, the defect content of the nanoparticles can be determined, including the type, dislocation density, and stacking faults/twinning. This information is convoluted together and can be grouped into 'size' and 'defect' broadening contributions. Modern X-ray diffraction analysis techniques have concentrated on quantifying the broadening arising from the size and defect contributions, while accounting for overlapping of profiles, instrumental broadening, background scattering and noise components. We report on a combined Bayesian/Maximum Entropy (MaxEnt) technique developed for use in the certification of a NIST Standard Reference Material (SRM) for size-broadened line profiles. The approach used was chosen because of its generality in removing instrumental broadening from the observed line profiles, and its ability to determine not only the average crystallite size, but also the distribution of sizes and the average shape of crystallites. Moverover, this Bayesian/MaxEnt technique is fully quantitative, in that it also determines uncertainties in the crystallite-size distribution and other parameters. Both experimental and numerical simulations of size broadened line-profiles modelled on a range of specimens with spherical and non-spherical morphologies are presented to demonstrate how this information can be retrieved from the line profile data. The sensitivity of the Bayesian/MaxEnt method to determining the size distribution using varying a priori information are emphasised and discussed

  3. Accurate quantitative XRD phase analysis of cement clinkers

    International Nuclear Information System (INIS)

    Kern, A.

    2002-01-01

    Full text: Knowledge about the absolute phase abundance in cement clinkers is a requirement for both, research and quality control. Traditionally, quantitative analysis of cement clinkers has been carried out by theoretical normative calculation from chemical analysis using the so-called Bogue method or by optical microscopy. Therefore chemical analysis, mostly performed by X-ray fluorescence (XRF), forms the basis of cement plan control by providing information for proportioning raw materials, adjusting kiln and burning conditions, as well as cement mill feed proportioning. In addition, XRF is of highest importance with respect to the environmentally relevant control of waste recovery raw materials and alternative fuels, as well as filters, plants and sewage. However, the performance of clinkers and cements is governed by the mineralogy and not the elemental composition, and the deficiencies and inherent errors of Bogue as well as microscopic point counting are well known. With XRD and Rietveld analysis a full quantitative analysis of cement clinkers can be performed providing detailed mineralogical information about the product. Until recently several disadvantages prevented the frequent application of the Rietveld method in the cement industry. As the measurement of a full pattern is required, extended measurement times made an integration of this method into existing automation environments difficult. In addition, several drawbacks of existing Rietveld software such as complexity, low performance and severe numerical instability were prohibitive for automated use. The latest developments of on-line instrumentation, as well as dedicated Rietveld software for quantitative phase analysis (TOPAS), now make a decisive breakthrough possible. TOPAS not only allows the analysis of extremely complex phase mixtures in the shortest time possible, but also a fully automated online phase analysis for production control and quality management, free of any human interaction

  4. Understanding changes in cellulose crystalline structure of lignocellulosic biomass during ionic liquid pretreatment by XRD.

    Science.gov (United States)

    Zhang, Jiafu; Wang, Yixun; Zhang, Liye; Zhang, Ruihong; Liu, Guangqing; Cheng, Gang

    2014-01-01

    X-ray diffraction (XRD) was used to understand the interactions of cellulose in lignocellulosic biomass with ionic liquids (ILs). The experiment was designed in such a way that the process of swelling and solubilization of crystalline cellulose in plant cell walls was followed by XRD. Three different feedstocks, switchgrass, corn stover and rice husk, were pretreated using 1-butyl-3-methylimidazolium acetate ([C4mim][OAc]) at temperatures of 50-130°C for 6h. At a 5 wt.% biomass loading, increasing pretreatment temperature led to a drop in biomass crystallinity index (CrI), which was due to swelling of crystalline cellulose. After most of the crystalline cellulose was swollen with IL molecules, a low-order structure was found in the pretreated samples. Upon further increasing temperature, cellulose II structure started to form in the pretreated biomass samples as a result of solubilization of cellulose in [C4mim][OAc] and subsequent regeneration. Copyright © 2013 Elsevier Ltd. All rights reserved.

  5. Nickel oxide reduction studied by environmental TEM and in situ XRD

    DEFF Research Database (Denmark)

    Jeangros, Q.; Hansen, Thomas Willum; Wagner, Jakob Birkedal

    2012-01-01

    Paar furnace and a mass spectrometer to complement and extrapolate the ETEM data to higher pressures and gas flows. Diffraction peak intensities, crystallite sizes (obtained using the Scherrer formula) and H2/H2O mass spectrometer signals are monitored. The recorded images and diffraction patterns show...... that the presence and stagnation of H2O vapour created upon reduction blocks H2 access to the reactive sites, decreasing the reaction rate at a high conversion fraction. The gas flow is low and may not evacuate the product gas efficiently around the Ni(O) particles. Complementary XRD experiments point towards...... the same conclusion and underline the impact of the pressure and gas flow on the kinetics. It is possible to determine an approximate activation energy for NiO reduction inside the ETEM using the Kissinger method [8], which is based on measurements of the shift in the temperature at which the reaction rate...

  6. Laboratory Detection and Analysis of Organic Compounds in Rocks Using HPLC and XRD Methods

    Science.gov (United States)

    Dragoi, D.; Kanik, I.; Bar-Cohen, Y.; Sherrit, S.; Tsapin, A.; Kulleck, J.

    2004-01-01

    In this work we describe an analytical method for determining the presence of organic compounds in rocks, limestone, and other composite materials. Our preliminary laboratory experiments on different rocks/limestone show that the organic component in mineralogical matrices is a minor phase on order of hundreds of ppm and can be better detected using high precision liquid chromatography (HPLC). The matrix, which is the major phase, plays an important role in embedding and protecting the organic molecules from the harsh Martian environment. Some rocks bear significant amounts of amino acids therefore, it is possible to identify these phases using powder x-ray diffraction (XRD) by crystallizing the organic. The method of detection/analysis of organics, in particular amino acids, that have been associated with life will be shown in the next section.

  7. Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

    Science.gov (United States)

    Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.

    2004-01-01

    Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

  8. Polycrystalline oxides formation during transient oxidation of (001) Cu-Ni binary alloys studied by in situ TEM and XRD

    International Nuclear Information System (INIS)

    Yang, J.C.; Li, Z.Q.; Sun, L.; Zhou, G.W.; Eastman, J.A.; Fong, D.D.; Fuoss, P.H.; Baldo, P.M.; Rehn, L.E.; Thompson, L.J.

    2009-01-01

    The nucleation and growth of Cu 2 O and NiO islands due to oxidation of Cu x Ni 1-x (001) films were monitored, at various temperatures, by in situ ultra-high vacuum (UHV) transmission electron microscopy (TEM) and in situ synchrotron X-ray diffraction (XRD). In remarkable contrast to our previous observations of Cu and Cu-Au oxidation, irregular-shaped polycrystalline oxide islands formed with respect to the Cu-Ni alloy film, and an unusual second oxide nucleation stage was noted. In situ XRD experiments revealed that NiO formed first epitaxially, then other orientations appeared, and finally polycrystalline Cu 2 O developed as the oxidation pressure was increased. The segregation of Ni and Cu towards or away, respectively, from the alloy surface during oxidation could disrupt the surface and cause polycrystalline oxide formation.

  9. Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF

    Science.gov (United States)

    Blake, D. F.; Bish, D.; Vaniman, D.; Chipera, S.; Sarrazin, P.; Collins, S. A.; Elliott, S. T.

    2001-01-01

    X-Ray Diffraction (XRD) is the most direct and accurate method for determining mineralogy. The CHEMIN XRD/XRF instrument has shown promising results on a variety of mineral and rock samples. Additional information is contained in the original extended abstract.

  10. Moessbauer and XRD Characterization of the Mineral Matter of Coal from the Guachinte Mine in Colombia

    International Nuclear Information System (INIS)

    Reyes, F.; Perez Alcazar, G. A.; Barraza, J. M.; Bohorquez, A.; Tabares, J. A.; Speziali, N. L.

    2003-01-01

    The aim of this work was the characterization and differentiation, using Moessbauer spectroscopy (MS) and X-ray diffraction (XRD), of coal samples with different ash and sulfur contents obtained in three places corresponding at cuts in different seams from the Guachinte mine, Valle, Colombia. The mineral phases identified by XRD were in general kaolinite, quartz, pyrite and gypsum, and in particular dolomite and calcite. MS confirms the presence of pyrite and kaolinite, besides evidences the additional presence of jarosite which was not detected by the XRD results due their low amounts. In the high mineral matter ash sample quartz and hematite was identified by XRD, the last one confirmed by MS results. A second phase in this sample was detected by Moessbauer spectroscopy, which could be superparamagnetic hematite. Rietveld refinement for XRD pattern from a sample is reported.

  11. Synchrotron-based XRD from rat bone of different age groups

    Energy Technology Data Exchange (ETDEWEB)

    Rao, D.V., E-mail: dvrao_9@yahoo.com [Science Based Applications to Engineering (SBAI), Physics Division, University of Rome “La Sapienza”, Via Scarpa 10, 00161 Roma (Italy); Gigante, G.E. [Science Based Applications to Engineering (SBAI), Physics Division, University of Rome “La Sapienza”, Via Scarpa 10, 00161 Roma (Italy); Cesareo, R.; Brunetti, A. [Istituto di Matematica e Fisica, Università di Sassari, Via Vienna 2, 07100 Sassari (Italy); Schiavon, N. [Hercules Laboratory, University of Evora (Portugal); Akatsuka, T.; Yuasa, T. [Department of Bio-System Engineering, Faculty of Engineering, Yamagata University, Yonezawa-shi, Yamagata 992-8510 (Japan); Takeda, T. [Allied Health Science, Kitasato University, 1-15-1 Kitasato, Sagamihara, Kanagawa 228-8555 (Japan)

    2017-05-01

    Synchrotron-based XRD spectra from rat bone of different age groups (w, 56 w and 78w), lumber vertebra at early stages of bone formation, Calcium hydroxyapatite (HAp) [Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}] bone fill with varying composition (60% and 70%) and bone cream (35–48%), has been acquired with 15 keV synchrotron X-rays. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15 keV X-rays (λ = 0.82666 A{sup 0}). Diffraction data were quantitatively analyzed using the Rietveld refinement approach, which allowed us to characterize the structure of these samples in their early stages. Hydroxyapatite, received considerable attention in medical and materials sciences, since these materials are the hard tissues, such as bone and teeth. Higher bioactivity of these samples gained reasonable interest for biological application and for bone tissue repair in oral surgery and orthopedics. The results obtained from these samples, such as phase data, crystalline size of the phases, as well as the degree of crystallinity, confirm the apatite family crystallizing in a hexagonal system, space group P6{sub 3}/m with the lattice parameters of a = 9.4328 Å and c = 6.8842 Å (JCPDS card #09-0432). Synchrotron-based XRD patterns are relatively sharp and well resolved and can be attributed to the hexagonal crystal form of hydroxyapatite. All the samples were examined with scanning electron microscope at an accelerating voltage of 15 kV. The presence of large globules of different sizes is observed, in small age groups of the rat bone (8w) and lumber vertebra (LV), as distinguished from, large age groups (56 and 78w) in all samples with different magnification, reflects an amorphous phase without significant traces of crystalline phases. Scanning electron microscopy (SEM) was used to characterize the morphology and crystalline properties of Hap, for all the samples, from 2 to 100 μm resolution. - Highlights: • For

  12. Synchrotron-based XRD from rat bone of different age groups.

    Science.gov (United States)

    Rao, D V; Gigante, G E; Cesareo, R; Brunetti, A; Schiavon, N; Akatsuka, T; Yuasa, T; Takeda, T

    2017-05-01

    Synchrotron-based XRD spectra from rat bone of different age groups (w, 56 w and 78w), lumber vertebra at early stages of bone formation, Calcium hydroxyapatite (HAp) [Ca 10 (PO 4 ) 6 (OH) 2 ] bone fill with varying composition (60% and 70%) and bone cream (35-48%), has been acquired with 15keV synchrotron X-rays. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15keV X-rays (λ=0.82666 A 0 ). Diffraction data were quantitatively analyzed using the Rietveld refinement approach, which allowed us to characterize the structure of these samples in their early stages. Hydroxyapatite, received considerable attention in medical and materials sciences, since these materials are the hard tissues, such as bone and teeth. Higher bioactivity of these samples gained reasonable interest for biological application and for bone tissue repair in oral surgery and orthopedics. The results obtained from these samples, such as phase data, crystalline size of the phases, as well as the degree of crystallinity, confirm the apatite family crystallizing in a hexagonal system, space group P6 3 /m with the lattice parameters of a=9.4328Å and c=6.8842Å (JCPDS card #09-0432). Synchrotron-based XRD patterns are relatively sharp and well resolved and can be attributed to the hexagonal crystal form of hydroxyapatite. All the samples were examined with scanning electron microscope at an accelerating voltage of 15kV. The presence of large globules of different sizes is observed, in small age groups of the rat bone (8w) and lumber vertebra (LV), as distinguished from, large age groups (56 and 78w) in all samples with different magnification, reflects an amorphous phase without significant traces of crystalline phases. Scanning electron microscopy (SEM) was used to characterize the morphology and crystalline properties of Hap, for all the samples, from 2 to 100μm resolution. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Karakteristik Beberapa Jenis Antibiotik Berdasarkan Pola Difraksi Sinar-X (XRD Dan Spektrum FTIR

    Directory of Open Access Journals (Sweden)

    Mirzan T Razzak

    2017-03-01

    Full Text Available Telah dilakukan pengukuran karakteristik difraksi sinar-x (XRD terhadap beberapa jenisantibiotik. Penelitian ini bertujuan untuk memahami karakteristik difraksi sinar-x suatuantibiotik sebagai upaya untuk identifikasi antibiotik secara cepat. Dalam penelitian ini diamatikarakteristik difraksi sinar-x dari 15 (lima belas antibiotik yang tersedia di pasaran. SpektrumXRD diukur pada sudut 2 antara 5 – 75 untuk dibandingkan dan dievaluasi mengenai bentukkristalnya. Selanjutnya diukur pula spektrum XRD dari pencampuran antibiotik dengan tepungtapioka. Pengukuran spektrum infrared dengan FTIR juga dilakukan untuk menguji konsistensihasil evaluasi spektrum XRD. Hasil penelitian menunjukkan bahwa amoxicillin dan ampicillinmempunyai struktur kristal yang sama, yaitu orthorombic primitif. Sayangnya baik XRDmaupun FTIR, tidak memberikan nilai kuantitatif pada antibiotik. Oleh sebab itu, perbedaankonsentrasi dengan pencampuran tepung tapioka tidak dapat dideteksi. Walaupun demikian,metode ini terbukti dapat digunakan untuk membedakan komposisi zat penyusun antibiotiksecara cepat dan akurat.

  14. Mineralogical Composition of the Mexican Ordinary Chondrite Type Meteorite: A Raman, Infrared and XRD Study

    Science.gov (United States)

    Ostrooumov, M.

    2016-08-01

    The Raman microprobe (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of seven mexican meteorites: Aldama, Cosina, El Pozo, Escalon, Nuevo Mercurio,Pacula, Zapotitlan Salinas.

  15. Determination of grain size by XRD profile analysis and TEM counting in nano-structured Cu

    International Nuclear Information System (INIS)

    Zhong Yong; Ping Dehai; Song Xiaoyan; Yin Fuxing

    2009-01-01

    In this work, a serial of pure copper sample with different grain sizes from nano- to micro-scale were prepared by sparkle plasma sintering (SPS) and following anneal treatment at 873 K and 1073 K, respectively. The grain size distributions of these samples were determined by both X-ray diffraction (XRD) profile analysis and transmission electronic microscope (TEM) micrograph counting. Although these two methods give similar distributions of grain size in the case of as-SPS sample with nano-scale grain size (around 10 nm), there are apparent discrepancies between the grain size distributions of the annealed samples obtained from XRD and TEM, especially for the sample annealed at 1073 K after SPS with micro-scale grain size (around 2 μm), which TEM counting provides much higher values of grain sizes than XRD analysis does. It indicates that for large grain-sized material, XRD analysis lost its validity for determination of grain size. It might be due to some small sized substructures possibly existed in even annealed (large grain-sized) samples, whereas there is no substructures in as-SPS (nanocrystalline) sample. Moreover, it has been found that the effective outer cut-off radius R e derived from XRD analysis coincides with the grain sizes given by TEM counting. The potential relationship between grain size and R e was discussed in the present work. These results might provide some new hints for deeper understanding of the physical meaning of XRD analysis and the parameters derived.

  16. Clay pigment structure characterisation as a guide for provenance determination--a comparison between laboratory powder micro-XRD and synchrotron radiation XRD.

    Science.gov (United States)

    Švarcová, Silvie; Bezdička, Petr; Hradil, David; Hradilová, Janka; Žižak, Ivo

    2011-01-01

    Application of X-ray diffraction (XRD)-based techniques in the analysis of painted artworks is not only beneficial for indisputable identification of crystal constituents in colour layers, but it can also bring insight in material crystal structure, which can be affected by their geological formation, manufacturing procedure or secondary changes. This knowledge might be helpful for art historic evaluation of an artwork as well as for its conservation. By way of example of kaolinite, we show that classification of its crystal structure order based on XRD data is useful for estimation of its provenance. We found kaolinite in the preparation layer of a Gothic wall painting in a Czech church situated near Karlovy Vary, where there are important kaolin deposits. Comparing reference kaolin materials from eight various Czech deposits, we found that these can be differentiated just according to the kaolinite crystallinity. Within this study, we compared laboratory powder X-ray micro-diffraction (micro-XRD) with synchrotron radiation X-ray diffraction analysing the same real sample. We found that both techniques led to the same results.

  17. XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite

    International Nuclear Information System (INIS)

    Reyes-Gasga, José; Martínez-Piñeiro, Esmeralda L.; Rodríguez-Álvarez, Galois; Tiznado-Orozco, Gaby E.; García-García, Ramiro

    2013-01-01

    The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI) XRD index is related to the crystal structure of the samples and the (CI) FTIR index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI) XRD value indicated that enamel is more crystalline than synthetic HAP, while (CI) FTIR indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. - Highlights: • XRD and FTIR crystallinity indices for tooth enamel and synthetic HAP were obtained. • SEM and TEM images were more correlated with (CI) XRD than with (CI) FTIR . • Regardless of the temperature, (CI) XRD and (CI) FTIR showed similar behavior. • XRD and FTIR crystallinity indices resulted in a fast and qualitative measurement

  18. XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite

    Energy Technology Data Exchange (ETDEWEB)

    Reyes-Gasga, José, E-mail: jreyes@fisica.unam.mx [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Martínez-Piñeiro, Esmeralda L., E-mail: esmemapi@gmail.com [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Rodríguez-Álvarez, Galois, E-mail: galoisborre@yahoo.com [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); Tiznado-Orozco, Gaby E., E-mail: gab0409@yahoo.com.mx [Unidad Académica de Odontología, Universidad Autónoma de Nayarit, Edificio E7, Ciudad de la Cultura “Amado Nervo”, C.P. 63190 Tepic, Nayarit (Mexico); García-García, Ramiro, E-mail: ramiro@fisica.unam.mx [Instituto de Física, UNAM, Circuito de la Investigación Científica s/n., Cd. Universitaria, Coyoacán 04510, México, D.F. (Mexico); and others

    2013-12-01

    The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI){sub XRD} index is related to the crystal structure of the samples and the (CI){sub FTIR} index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI){sub XRD} value indicated that enamel is more crystalline than synthetic HAP, while (CI){sub FTIR} indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. - Highlights: • XRD and FTIR crystallinity indices for tooth enamel and synthetic HAP were obtained. • SEM and TEM images were more correlated with (CI){sub XRD} than with (CI){sub FTIR}. • Regardless of the temperature, (CI){sub XRD} and (CI){sub FTIR} showed similar behavior. • XRD and FTIR crystallinity indices resulted in a fast and qualitative measurement.

  19. Powder-XRD and (14) N magic angle-spinning solid-state NMR spectroscopy of some metal nitrides.

    Science.gov (United States)

    Kempgens, Pierre; Britton, Jonathan

    2016-05-01

    Some metal nitrides (TiN, ZrN, InN, GaN, Ca3 N2 , Mg3 N2 , and Ge3 N4 ) have been studied by powder X-ray diffraction (XRD) and (14) N magic angle-spinning (MAS) solid-state NMR spectroscopy. For Ca3 N2 , Mg3 N2 , and Ge3 N4 , no (14) N NMR signal was observed. Low speed (νr  = 2 kHz for TiN, ZrN, and GaN; νr  = 1 kHz for InN) and 'high speed' (νr  = 15 kHz for TiN; νr  = 5 kHz for ZrN; νr  = 10 kHz for InN and GaN) MAS NMR experiments were performed. For TiN, ZrN, InN, and GaN, powder-XRD was used to identify the phases present in each sample. The number of peaks observed for each sample in their (14) N MAS solid-state NMR spectrum matches perfectly well with the number of nitrogen-containing phases identified by powder-XRD. The (14) N MAS solid-state NMR spectra are symmetric and dominated by the quadrupolar interaction. The envelopes of the spinning sidebands manifold are Lorentzian, and it is concluded that there is a distribution of the quadrupolar coupling constants Qcc 's arising from structural defects in the compounds studied. Copyright © 2015 John Wiley & Sons, Ltd.

  20. Swelling induced by alpha decay in monazite and zirconolite ceramics: A XRD and TEM comparative study

    Science.gov (United States)

    Deschanels, X.; Seydoux-Guillaume, A. M.; Magnin, V.; Mesbah, A.; Tribet, M.; Moloney, M. P.; Serruys, Y.; Peuget, S.

    2014-05-01

    Zirconolite and monazite matrices are potential ceramics for the containment of actinides (Np, Cm, Am, Pu) which are produced over the reprocessing of spent nuclear fuel. Actinides decay mainly through the emission of alpha particles, which in turn causes most ceramics to undergo structural and textural changes (amorphization and/or swelling). In order to study the effects of alpha decays on the above mentioned ceramics two parallel approaches were set up. The first involved the use of an external irradiation source, Au, which allowed the deposited recoil energy to be simulated. The second was based on short-lived actinide doping with 238Pu, (i.e. an internal source), via the incorporation of plutonium oxide into both the monazite and zirconolite structures during synthesis. In both types of irradiation experiments, the zirconolite samples became amorphous at room temperature with damage close to 0.3 dpa; corresponding to a critical dose of 4 × 1018 α g-1 (i.e. ∼1.3 × 1021 keV cm-3). Both zirconolite samples also showed the same degree of macroscopic swelling at saturation (∼6%), with ballistic processes being the predominant damaging effect. In the case of the monazite however, the macroscopic swelling and amorphization were dependent on the nature of the irradiation. Externally, (Au), irradiated samples became amorphous while also demonstrating a saturation swelling of up to 8%. In contrast to this, the swelling of the 238Pu doped samples was much smaller at ∼1%. Also, unlike the externally (Au) irradiated monazite these 238Pu doped samples remained crystalline up to 7.5 × 1018 α g-1 (0.8 dpa). XRD, TEM and swelling measurements were used to fully characterize and interpret this behavior. The low swelling and the conservation of the crystalline state of 238Pu doped monazite samples indicates that alpha annealing took place within this material.

  1. Interaction of selenite with reduced Fe and/or S species: An XRD and XAS study.

    Science.gov (United States)

    Finck, Nicolas; Dardenne, Kathy

    2016-05-01

    In this study, we investigated the interaction between selenite and either Fe((II))aq or S((-II))aq in solution, and the results were used to investigate the interaction between Se((IV))aq and FeS in suspension. The reaction products were characterized by a combination of methods (SEM, XRD and XAS) and the reaction mechanisms were identified. In a first experiment, Se((IV))aq was reduced to Se((0)) by interaction with Fe((II))aq which was oxidized to Fe((III)), but the reaction was only partial. Subsequently, some Fe((III)) produced akaganeite (β-FeOOH) and the release of proton during that reaction decreased the pH. The pH decrease changed the Se speciation in solution which hindered further Se((IV)) reduction by Fe((II))aq. In a second experiment, Se((IV))aq was quantitatively reduced to Se((0)) by S((-II))aq and the reaction was fast. Two sulfide species were needed to reduce one Se((IV)), and the observed pH increase was due to a proton consumption. For both experiments, experimental results are consistent with expectations based on the oxidation reduction potential of the various species. Upon interaction with FeS, Se((IV))aq was reduced to Se((0)) and minute amounts of pyrite were detected, a consequence of partial mackinawite oxidation at surface sulfur sites. These results are of prime importance with respect to safe deep disposal of nuclear waste which contains the long-lived radionuclide (79)Se. This study shows that after release of (79)Se((IV)) upon nuclear waste matrix corrosion, selenite can be reduced in the near field to low soluble Se((0)) by interaction with Fe((II))aq and/or S((-II))aq species. Because the solubility of Se((0)) species is significantly lower than that of Se((IV)), selenium will become much less (bio)available and its migration out of deep HLW repositories may be drastically hindered. Copyright © 2016. Published by Elsevier B.V.

  2. Characterization of crystallite morphology for doped strontium fluoride nanophosphors by TEM and XRD

    Energy Technology Data Exchange (ETDEWEB)

    O' Connell, J.H. [Centre for HRTEM, Nelson Mandela Metropolitan University, PO Box 77000, Port Elizabeth ZA6031 (South Africa); Lee, M.E., E-mail: Michael.lee@nmmu.ac.za [Centre for HRTEM, Nelson Mandela Metropolitan University, PO Box 77000, Port Elizabeth ZA6031 (South Africa); Yagoub, M.Y.A.; Swart, H.C.; Coetsee, E. [Department of Physics, University of the Free State, PO Box 339, Bloemfontein ZA9300 (South Africa)

    2016-01-01

    Crystallite morphology for Eu-doped and undoped SrF{sub 2} nanophosphors have been determined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The values for average crystallite size obtained by the application of the Scherrer equation and the full width at half maximum (FWHM) values for XRD peaks are compared to the results obtained using the hollow cone dark field (HCDF) TEM imaging technique. In the case of the TEM analysis, a bimodal crystallite size distribution was revealed with one of the distributions having a measured range of crystallite sizes which was in good agreement with the XRD data. HCDF in combination with FIB specimen preparation was found to be a promising technique for the determination of crystallite size distributions in nanophosphors which might facilitate a better understanding of their scintillation properties.

  3. Characterization of crystallite morphology for doped strontium fluoride nanophosphors by TEM and XRD

    International Nuclear Information System (INIS)

    O'Connell, J.H.; Lee, M.E.; Yagoub, M.Y.A.; Swart, H.C.; Coetsee, E.

    2016-01-01

    Crystallite morphology for Eu-doped and undoped SrF_2 nanophosphors have been determined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The values for average crystallite size obtained by the application of the Scherrer equation and the full width at half maximum (FWHM) values for XRD peaks are compared to the results obtained using the hollow cone dark field (HCDF) TEM imaging technique. In the case of the TEM analysis, a bimodal crystallite size distribution was revealed with one of the distributions having a measured range of crystallite sizes which was in good agreement with the XRD data. HCDF in combination with FIB specimen preparation was found to be a promising technique for the determination of crystallite size distributions in nanophosphors which might facilitate a better understanding of their scintillation properties.

  4. Response Time Measurements of the NIF DANTE XRD-31 X-Ray Diodes (Pre-print)

    International Nuclear Information System (INIS)

    Pellinen, Don; Griffin, Michael

    2009-01-01

    The XRD-31 is a fast, windowless X-ray vacuum photodiode developed by EG and G. It is currently the primary fast X-ray detector used to diagnose the X-rays on NIF and OMEGA on the multichannel DANTE spectrometer. The XRD-31 has a dynamic range of less than 1e-12 amps to more than 10 amps. A technique is described to measure the impulse response of the diodes to a 150 fs pulse of 200 nm laser light and a method to calculate the 'risetime' for a square pulse and compare it with the computed electron transit time from the photocathode to the anode. Measured response time for 5 XRD-31s assembled in early 2004 was 149.7 ps +-2.75 ps

  5. Definitive Mineralogical Analysis of Mars Analog Rocks Using the CheMin XRD/XRF Instrument

    Science.gov (United States)

    Blake, D. F.; Sarrazin, P.; Bish, D. L.; Feldman, S.; Chipera, S. J.; Vaniman, D. T.; Collins, S.

    2004-01-01

    Mineral identification is a critical component of Mars Astrobiological missions. Chemical or elemental data alone are not definitive because a single elemental or chemical composition or even a single bonding type can represent a range of substances or mineral assemblages. Minerals are defined as unique structural and compositional phases that occur naturally. There are about 15,000 minerals that have been described on Earth, all uniquely identifiable via diffraction methods. There are likely many minerals yet undiscovered on Earth, and likewise on Mars. If an unknown phase is identified on Mars, it can be fully characterized by structural (X-ray Diffraction, XRD) and elemental analysis (X-ray Fluorescence, XRF) without recourse to other data because XRD relies on the principles of atomic arrangement for its determinations. XRD is the principal means of identification and characterization of minerals on Earth.

  6. Stress-strain relationship and XRD line broadening in [0001] textured hexagonal polycrystalline materials

    International Nuclear Information System (INIS)

    Yokoyama, Ryouichi

    2011-01-01

    Stress analysis with X-ray diffraction (XRD) for hexagonal polycrystalline materials in the Laue classes 6/mmm and 6/m has been studied on the basis of the crystal symmetry of the constituent crystallites which was proposed by R. Yokoyama and J. Harada ['Re-evaluation of formulae for X-ray stress analysis in polycrystalline specimens with fibre texture', Journal of Applied Crystallography, Vol.42, pp.185-191 (2009)]. The relationship between the stress and strain observable by XRD in a hexagonal polycrystalline material with [0001] fibre texture was formulated in terms of the elastic compliance defined for its single crystal. As a result, it was shown that the average strains obtained in the crystallites for both symmetries of 6/mmm and 6/m are different from each other under the triaxial or biaxial stress field. Then, it turned out that the line width of XRD changes depending on the measurement direction. (author)

  7. The thermal behaviour of cuprite: An XRD-EXAFS combined approach

    International Nuclear Information System (INIS)

    Dapiaggi, M.; Tiano, W.; Artioli, G.; Sanson, A.; Fornasini, P.

    2003-01-01

    Cuprite (Cu 2 O) is a low thermal expansion material with a negative thermal expansion coefficient below room temperature. Its peculiar thermal behaviour encompasses the increase of the shear modulus with increasing temperature, and the presence of rather intense symmetry-forbidden eeo reflections below room temperature. The thermal expansion of cuprite was studied at low temperature (between 5 and 298 K) by means of high-resolution (10 -5 A) X-ray powder diffraction at European Synchrotron Radiation Facility (Grenoble, BM16) and extended X-ray absorption fine structure (EXAFS) (BM29). Negative thermal expansion is confirmed up to 200 K, by EXAFS as well as by XRD measurements, and no sign of transition was found in XRD data. The comparison between EXAFS and XRD results provides a valuable insight into vibrational behaviour of cuprite at low temperature

  8. Using of XRD in Industrial Sample Analysis and TENORM in Nuclear Malaysia

    International Nuclear Information System (INIS)

    Paulus, W.; Nurhaslinda Ee Abdullah; Meor Yusoff Meor Sulaiman

    2011-01-01

    Industrial waste such as aluminium dross and TENORM waste, oil sludge has been used as sample in this research. Determination of main elements by using X-Ray Diffraction (XRD) in Material Technology Group, Malaysian Nuclear Agency. Results shows that main elements in these samples, aluminium hydroxide (gibbsite) and quartz low, respectively. Thereby, this research shows that XRD can be considered as one of the techniques that can be used in waste characterization and furthermore, it can help researchers and engineer in the research related to waste treatment especially radioactive waste. (author)

  9. Determination of Stress Profiles in Expanded Austenite by Combining Successive Layer Removal and GI-XRD

    DEFF Research Database (Denmark)

    Fernandes, Frederico Augusto Pires; Christiansen, Thomas Lundin; Somers, Marcel A. J.

    2014-01-01

    The present work deals with the evaluation of the residual-stress profile in expanded-austenite by successive removal steps using GI-XRD. Preliminary results indicate stresses of several GPa's from 111 and 200 diffraction lines. These stresses appear largest for the 200 reflection. The strain......-free lattice parameter decayed smoothly with depth, while for the compressive stress a maximum value is observed at some depth below the surface. Additionally a good agreement was found between the nitrogen profile determined with GDOES analysis and the strain-free lattice parameter from XRD....

  10. Morphologic characterization for XRD and TEM of polyamide 6 and 66 nanocomposites with bentonite regional clay

    International Nuclear Information System (INIS)

    Leite, Amanda M.D.; Medeiros, Vanessa da N.; Maia, Larissa F.; Araujo, Edcleide M.; Lira, Helio L.

    2009-01-01

    Polyamide 6 and 66 nanocomposites with clay consisting of silicates layer from Paraiba were produced. The clay was modified being used the quaternary salt of ammonium Cetremide, this so there is a better interaction of the clay with polymeric matrix. The clay without treatment (MMT) and treated clay was evaluated by XRD that showed the insertion of the salt molecules into silicates layer. The nanocomposites were obtained from polyamide 6 and 66 were verified that these presented morphological structure composed of exfoliated/partially exfoliated, analyzed by XRD and TEM. (author)

  11. Microstructural Characterization of Water-Rich Boehmite (AlO(OH)): TEM Correlation of Apparently Divergent XRD and TGA Results

    International Nuclear Information System (INIS)

    Allard, L.F.; Anovitz, L.M.; Benezeth, P.; Coffey, D.W.; Palmer, D.A.; Porter, W.D.; Wesolowski, D.J.

    1999-01-01

    An understanding of the solid-phase thermodynamics and aqueous speciation of aluminum is critical to our ability to understand and predict processes in a wide variety of geologic and industrial settings. Boehmite (AIO(OH)) is an important phase in the system Al 2 O 3 -H 2 O that has been the subject of a number of structural and thermodynamic studies since its initial synthesis [l] and discovery in nature [2]. Unfortunately, it has long been recognized that thermogravimetric analysis (TGA) of both synthetic and natural boehmite samples (that appear well crystallized by powder XRD methods) yields significant excess water - typically losing 16-16.5 wt. % on heating as compared with a nominal expected weight loss of 15.0 wt. % [3,4]. The boehmite used in our experiments was synthesized hydrothermally from acid-washed gibbsite (Al(OH) 3 ) at 200C. Powder XRD and SEM examination showed no evidence of the presence a contaminant phase. The TGA patterns do not suggest that this is due to adsorbed water, so a structural source is likely. We therefore undertook to examine this material by TEM to clarify this phenomenon

  12. The effect of size-selective samplers (cyclones) on XRD response

    CSIR Research Space (South Africa)

    Pretorius, CJ

    2011-07-01

    Full Text Available The study evaluated five size-selective samplers used in the South African mining industry to determine how their performance affects the X-ray powder diffraction (XRD) response when respirable dust samples are analysed for quartz using direct...

  13. EPXMA survey of shelf sediments (Southern Bight, North Sea): A glance beyond the XRD-invisible

    NARCIS (Netherlands)

    De Maeyer-Worobiec, A.; Dekov, V.M.; Laane, R.W.P.M.; van Grieken, R.

    2009-01-01

    Shelf sediments of the southern North Sea, were studied with a microanalytical [electron probe X-ray microanalysis (EPXMA)] and two bulk [X-ray diffraction (XRD) and X-ray fluorescence (XRF)] techniques. The investigation proved that the promptness of the microanalytical method is combined with a

  14. Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury.

    Science.gov (United States)

    Li, Cen; Yang, Hongxia; Du, Yuzhi; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao; Wei, Lixin

    2016-01-01

    Zuotai ( gTso thal ) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100-800 nm, which commonly further aggregate into 1-30  μ m loosely amorphous particles. XRD test shows that β -HgS, S 8 , and α -HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai , and it would play a positive role in interpreting this mysterious Tibetan drug.

  15. Crystallographic Investigation of Ag (4 mol%) Doped ZnO (SZO) Thin Films by XRD

    International Nuclear Information System (INIS)

    Lwin Lwin Nwe; Sandar Dwe; Khant Khant Lin; Khin Thuzar; Than Than Win; Ko Ko Kyaw Soe

    2008-03-01

    Silver doped ZnO(SZO) thin films are prepared by sol-based method. The silver dopant concentration is 4 mol % in this case. XRD analysis carried out to determine, crystallographic properties such as lattice parameters and crystallite size of SZO thin films.

  16. Evaluation of dislocation density in copper and brass α deformed by XRD peak width analysis

    International Nuclear Information System (INIS)

    Sousa, Talita Gama de

    2014-01-01

    The determination of dislocation density in metallic materials has been available for many years in scientific environment. This is due to the fact that the dislocations are the main responsible for plastic deformation, which, thereafter, markedly influences the mechanical properties. In this work, the dislocation density was analyzed through peak broadening of Xray diffraction (XRD) using Convolutional Multiple Whole Profile (CMWP) program. The measurements obtained by XRD were compared with those obtained from images observed by transmission electronic microscopy (TEM). The materials used in this study were pure copper and brass α as alloy 268 (6 % Cu and 34 % Zn), deformed by rolling and ECA (equal channel angular extrusion) processes. The results indicate that the XRD is a powerful tool for the characterization of the microstructure in relation to the dislocation density, as they were consistent to the TEM measurements, and also showed good relationship with measurements of hardness. Furthermore, through the dislocation density it was possible to verify the influence of stacking fault energy (SFE) in the evolution of the copper samples deformation process and its alloy, and that the presence of texture in rolled samples did not impair the measurements obtained by XRD technique. (author)

  17. XRD and TEM analysis of microstructure in the welding zone of 9Cr ...

    Indian Academy of Sciences (India)

    Unknown

    XRD and TEM analysis of microstructure in the welding zone of. 9Cr–1Mo–V–Nb ... steel, which has highest Cr content in the heat-resisting. Cr–Mo ... This research provides essential ... film samples were observed under TEM and select elec-.

  18. Effect of sample moisture content on XRD-estimated cellulose crystallinity index and crystallite size

    Science.gov (United States)

    Umesh P. Agarwal; Sally A. Ralph; Carlos Baez; Richard S. Reiner; Steve P. Verrill

    2017-01-01

    Although X-ray diffraction (XRD) has been the most widely used technique to investigate crystallinity index (CrI) and crystallite size (L200) of cellulose materials, there are not many studies that have taken into account the role of sample moisture on these measurements. The present investigation focuses on a variety of celluloses and cellulose...

  19. NMR determination of solvent dependent behavior and XRD structural properties of 4-carboxy phenylboronic acid: A DFT supported study

    Science.gov (United States)

    Dikmen, Gökhan; Alver, Özgür; Parlak, Cemal

    2018-04-01

    Solvent dependent structural properties of 4-carboxy phenylboronic acid (4-cpba) were investigated by X-ray diffraction (XRD) and nuclear magnetic resonance (NMR) spectroscopic methods. The molecular structure and geometric parameters were determined by some computational methods such as B3LYP/6-31 + G(3df,p), HF/aug-cc-pvtz and MP2/6-31G(d). Detailed elucidation of the structural and spectroscopic properties of 4-cpba was carried out with 1H, HETCOR and DOSY NMR experiments. Solvent effects on the structural properties were monitored on the changes of 1H NMR spectra by using various solvents and it was observed that 4-cpba shows serious structural preferences depending on the solvent used.

  20. Fast and accurate methods for the performance testing of highly-efficient c-Si photovoltaic modules using a 10 ms single-pulse solar simulator and customized voltage profiles

    International Nuclear Information System (INIS)

    Virtuani, A; Rigamonti, G; Friesen, G; Chianese, D; Beljean, P

    2012-01-01

    Performance testing of highly efficient, highly capacitive c-Si modules with pulsed solar simulators requires particular care. These devices in fact usually require a steady-state solar simulator or pulse durations longer than 100–200 ms in order to avoid measurement artifacts. The aim of this work was to validate an alternative method for the testing of highly capacitive c-Si modules using a 10 ms single pulse solar simulator. Our approach attempts to reconstruct a quasi-steady-state I–V (current–voltage) curve of a highly capacitive device during one single 10 ms flash by applying customized voltage profiles–-in place of a conventional V ramp—to the terminals of the device under test. The most promising results were obtained by using V profiles which we name ‘dragon-back’ (DB) profiles. When compared to the reference I–V measurement (obtained by using a multi-flash approach with approximately 20 flashes), the DB V profile method provides excellent results with differences in the estimation of P max (as well as of I sc , V oc and FF) below ±0.5%. For the testing of highly capacitive devices the method is accurate, fast (two flashes—possibly one—required), cost-effective and has proven its validity with several technologies making it particularly interesting for in-line testing. (paper)

  1. Graphene oxide and reduced graphene oxide studied by the XRD, TEM and electron spectroscopy methods

    International Nuclear Information System (INIS)

    Stobinski, L.; Lesiak, B.; Malolepszy, A.; Mazurkiewicz, M.; Mierzwa, B.; Zemek, J.; Jiricek, P.; Bieloshapka, I.

    2014-01-01

    Highlights: • Graphene oxide (FL-GOc) and reduced graphene oxide (FL-RGOc): XRD, TEM, XPS, REELS. • FL-GOc: stacking nanostructure—22 × 6 nm (DxH), 0.9 nm layers separation (XRD). • FL-RGOc: stacking nanostructure—8 × 1 nm (DxH), 0.4 nm layers separation (XRD). • Reduction: oxygen group degradation, decreasing distance between graphene layers. • Number of graphene layers in stacking nanostructure: 6–7 (FL-GOc), 2–3 (FL-RGOc). - Abstract: The commercial and synthesised few-layer graphene oxide, prepared using oxidation reactions, and few-layer reduced graphene oxide samples were structurally and chemically investigated by the X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron spectroscopy methods, i.e. X-ray photoelectron spectroscopy (XPS) and reflection electron energy loss spectroscopy (REELS). The commercial graphene oxide (FL-GOc) shows a stacking nanostructure of about 22 × 6 nm average diameter by height with the distance of 0.9 nm between 6-7 graphene layers, whereas the respective reduced graphene oxide (FL-RGOc)—about 8 × 1 nm average diameter by height stacking nanostructure with the distance of 0.4 nm between 2-3 graphene layers (XRD). The REELS results are consistent with those by the XRD indicating 8 (FL-GOc) and 4 layers (FL-RGOc). In graphene oxide and reduced graphene oxide prepared from the graphite the REELS indicates 8–11 and 7–10 layers. All graphene oxide samples show the C/O ratio of 2.1–2.3, 26.5–32.1 at% of C sp 3 bonds and high content of functional oxygen groups (hydroxyl—C-OH, epoxy—C-O-C, carbonyl—C=O, carboxyl—C-OOH, water) (XPS). Reduction increases the C/O ratio to 2.8–10.3, decreases C sp 3 content to 11.4–20.3 at% and also the content of C-O-C and C=O groups, accompanied by increasing content of C-OH and C-OOH groups. Formation of additional amount of water due to functional oxygen group reduction leads to layer delamination. Removing of functional oxygen groups

  2. XRD, SEM and infrared study into the intercalation of sodium hexadecyl sulfate (SHS) into hydrocalumite.

    Science.gov (United States)

    Zhang, Ping; Wang, Tianqi; Zhang, Longlong; Wu, Daishe; Frost, Ray L

    2015-12-05

    Hydrocalumite (CaAl-LDH-Cl) interacted with a natural anionic surfactant, sodium hexadecyl sulfate (SHS), was performed using an intercalation method. To understand the intercalation behavior and characterize the resulting products, powder X-ray diffraction (XRD), scan electron microscopy (SEM) and mid-infrared (MIR) spectroscopy combined with near-infrared (NIR) spectroscopy technique were used. The XRD analysis indicated that SHS was intercalated into CaAl-LDH-Cl successfully, resulting in an expansion of the interlayer (from 0.78 nm to 2.74 nm). The bands of C-H stretching vibrations of SHS were observed in the near-infrared spectra, which indicated that the resulting products were indeed CaAl-LDH-SHS. In addition, the bands of water stretching vibrations and OH groups shifted to higher wavenumbers when SHS was intercalated into CaAl-LDH-Cl interlayer space. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. In Situ Synchrotron XRD on a Capillary Li-O2 Battery Cell

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune; Norby, Poul

    2014-01-01

    of a electrolyte filled capillary with anode and cathode in each end suspended on stainless steel wires, the oxygen in-let is placed on the cathode side of the capillary with a flushing system for oxygen in-let. In this study we present a flexible design of a capillary based Li-O2 battery with discharge and charge...... a stainless steel wire where the cathode is attached. The in situ XRD measurements show how the Li2O2 growth depend on current discharge rate and how the FWHM changes dependent on reflection and charge/discharge.Several cells were tested both ex situ and in situ, and in situ XRD for 1st discharge/charge and 2...

  4. Characterising palladium-silver and palladium-nickel alloy membranes using SEM, XRD and PIXE

    International Nuclear Information System (INIS)

    Keuler, J.N.; Lorenzen, L.; Sanderson, R.D.; Prozesky, V.; Przybylowicz, W.J.

    1999-01-01

    Palladium alloy membranes were prepared by successive electroless plating steps on an alumina-zirconia support membrane. Palladium, silver and nickel were deposited in layers and then the metal films were heat treated for 5 h in a hydrogen atmosphere at 650 deg. C. The topography of the metal coatings and cross-sections of the films (before and after heating) were characterised using scanning electron microscopy (SEM). XRD was used to determine the crystal phase of the alloy coatings. Both SEM and XRD provide only surface information and therefore micro-PIXE was used to extract depth information of the alloy coating. Concentration profiles across the thickness of the films were constructed to determine penetration of the coating into the support membrane pores during electroless plating and to investigate diffusion of coated layers during the heating step

  5. Nanosecond time measurements of single pulse

    International Nuclear Information System (INIS)

    Xing Jingyuan; Cheng Shiyuan

    1986-01-01

    This report mainly describes the principle specification of circuit design and time-interval calibrations of model SHS 500 time-to-digital converter. Its range is 12 to 500 ns, with six ranges: 50, 100, 200, 300, 400 and 500 ns. The precision of measured time-interval is 0.3% of full scale and time resolution is 0.1% of full scale

  6. Searching for Single Pulses Using Heimdall

    Science.gov (United States)

    Walsh, Gregory; Lynch, Ryan

    2018-01-01

    In radio pulsar surveys, the interstellar medium causes a frequency dependent dispersive delay of a pulsed signal across the observing band. If not corrected, this delay substantially lowers S/N and makes most pulses undetectable. The delay is proportional to an unknown dispersion measure (DM), which must be searched over with many trial values. A number of new, GPU-accelerated codes are now available to optimize this dedispersion task, and to search for transient pulsed radio emission. We report on the use of Heimdall, one such GPU-accelerated tree dedispersion utility, to search for transient radio sources in a Green Bank Telescope survey of the Cygnus Region and North Galactic Plane. The survey is carried out at central frequency of 820 MHz with a goal of finding Fast Radio Bursts, Rotating Radio Transients, young pulsars, and millisecond pulsars. We describe the the survey, data processing pipeline, and follow-up of candidate sources.

  7. X-ray diffraction (XRD) characterization of microstrain in some iron and uranium alloys

    International Nuclear Information System (INIS)

    Kimmel, G.; Dayan, D.; Frank, G.A.; Landau, A.

    1996-01-01

    The high linear attenuation coefficient of steel, uranium and uranium based alloys is associated with the small penetration depth of X-rays with the usual wavelength used for diffraction. Nevertheless, by using the proper surface preparation technique, it is possible of obtaining surfaces with bulk properties (free of residual mechanical microstrain). Taking advantage of the feasibility to obtain well prepared surfaces, extensive work has been conducted in studying XRD line broadening effects from flat polycrystalline samples of steel, uranium and uranium alloys

  8. In-situ high temperature XRD of calcium phosphate biomaterial using DEHPA as the starting material

    International Nuclear Information System (INIS)

    Meor Yusoff Meor Sulaiman; Masliana Muslim

    2009-01-01

    A process to produce calcium phosphate biomaterial was done using an organic based phosphoric acid (DEHPA) as its starting material. The gel obtained from this reaction was used to study calcium phosphate transformation using in-situ XRD with temperature ranges from room temperature to 1300 degree C. The results obtained from this analysis show the following phase transformation: Gel β-Ca 2 P 2 O 7 β-TCP + HA α-TCP + HA, β-Ca 2 P 2 O 7 forms at 400 degree C and as we heat the sample at 1000 degree C peaks belonging to β- TCP and HA appears showing the transformation of the β-Ca 2 P 2 O 7 phase. When the sample is heated up further to 1200 degree C, β-TCP is transform into α-TCP. In the cold in-situ study, XRD analysis was performed on the sample from room temperature to -140 degree C. At room the XRD diffractogram shows the sample as an amorphous material and as the temperature was further lowered sharp peaks begins to form indicating that the material had becomes crystalline. The peaks were identified to be that calcium hydrogen phosphate (Ca(H 2 PO 4 ) 2 ) and this indicates that there is no hydroxyl group removal during the cooling process. The relative crystallinity values obtained for the different cooling temperatures show a slow exponential increase on the initial cooling of 0 to -100 degree C and at further cooling temperatures resulted fast and linear process. Also unlike the in-situ XRD analysis performs at high temperature no phase transformation occurred at this low temperature. (Author)

  9. A Study on Factors Affecting Strength of Solidified Peat through XRD and FESEM Analysis

    Science.gov (United States)

    Rahman, J. A.; Napia, A. M. A.; Nazri, M. A. A.; Mohamed, R. M. S. R.; Al-Geethi, A. S.

    2018-04-01

    Peat is soft soil that often causes multiple problems to construction. Peat has low shear strength and high deformation characteristics. Thus, peat soil needs to be stabilized or treated. Study on peat stabilization has been conducted for decades with various admixtures and mixing formulations. This project intends to provide an overview of the solidification of peat soil and the factors that affecting the strength of solidified peat soil. Three types of peats which are fabric, hemic and sapric were used in this study to understand the differences on the effect. The understanding of the factors affecting strength of solidified peat in this study is limited to XRD and FESEM analysis only. Peat samples were collected at Pontian, Johor and Parit Raja, Johor. Peat soil was solidified using fly ash, bottom ash and Portland cement with two mixing formulation following literature review. The solidified peat were cured for 7 days, 14 days, 28 days and 56 days. All samples were tested using Unconfined Compressive Strength Test (UCS), X-ray diffraction (XRD) and Field Emission Scanning Electron Microscope (FESEM). The compressive strength test of solidified peat had shown consistently increase of sheer strength, qu for Mixing 1 while decrease of its compressive strength value for Mixing 2. All samples were tested and compared for each curing days. Through XRD, it is found that all solidified peat are dominated with pargasite and richterite. The highest qu is Fabric Mixing 1(FM1) with the value of 105.94 kPa. This sample were proven contain pargasite. Samples with high qu were observed to be having fly ash and bottom ash bound together with the help of pargasite. Sample with decreasing strength showed less amount of pargasite in it. In can be concluded that XRD and FESEM findings are in line with UCS values.

  10. Study the oxidation kinetics of uranium using XRD and Rietveld method

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Yanzhi; Guan Weijun; Wang Qinguo; Wang Xiaolin; Lai Xinchun; Shuai Maobing, E-mail: yanzhizh@163.com [China Academy of Engineering Physics, PO Box 919-71, Mianyang, Sichuan, 621900 (China)

    2010-03-15

    The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50{approx}300deg. C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO{sub 2} was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO{sub 2} can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

  11. Mineralogical composition of the meteorite El Pozo (Mexico): a Raman, infrared and XRD study.

    Science.gov (United States)

    Ostrooumov, Mikhail; Hernández-Bernal, Maria del Sol

    2011-12-01

    The Raman (RMP), infrared (IR) and XRD analysis have been applied to the examination of mineralogical composition of El Pozo meteorite (an ordinary chondrite L5 type; village Valle of Allende, founded in State of Chihuahua, Mexico: 26°56'N and 105°24'W, 1998). RMP measurements in the range of 100-3500 cm(-1) revealed principal characteristic bands of the major minerals: olivine, two polymorph modifications of pyroxene (OPx and CPx) and plagioclase. Some bands of the minor minerals (hematite and goethite) were also identified. All these minerals were clearly distinguished using IR and XRD techniques. XRD technique has shown the presence of some metallic phases such as kamacite and taenite as well as troilite and chromite. These minerals do not have characteristic Raman spectra because Fe-Ni metals have no active modes for Raman spectroscopy and troilite is a weak Raman scatterer. Raman mapping microspectroscopy was a key part in the investigation of El Pozo meteorite's spatial distribution of the main minerals because these samples are structurally and chemically complex and heterogeneous. The mineral mapping by Raman spectroscopy has provided information for a certain spatial region on which a spatial distribution coexists of the three typical mineral assemblages: olivine; olivine+orthopyroxene; and orthopyroxene. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. Validation of enhanced stabilization of municipal solid waste under controlled leachate recirculation using FTIR and XRD.

    Science.gov (United States)

    Sethi, Sapna; Kothiyal, N C; Nema, Arvind K

    2012-07-01

    Leachate recirculation at neutral PH accompanied with buffer/nutrients addition has been used successfully in earlier stabilization of municipal solid waste in bioreactor landfills. In the present study, efforts were made to enhance the stabilization rate of municipal solid waste (MSW) and organic solid waste (OSW) in simulated landfill bioreactors by controlling the pH of recirculated leachate towards slightly alkaline side in absence of additional buffer and nutrients addition. Enhanced stabilization in waste samples was monitored with the help of analytical tools like Fourier Transform Infrared Spectroscopy (FTIR) and X-Ray Diffraction (XRD). Predominance of bands assigned to inorganic compounds and comparatively lower intensities of bands for organic compounds in the FTIR spectra of waste samples degraded with leachate recirculation under controlled pH confirmed higher rate of biodegradation and mineralization of waste than the samples degraded without controlled leachate recirculation. XRD spectra also confirmed to a greater extent of mineralization in the waste samples degraded under leachate recirculation with controlled pH. Comparison of XRD spectra of two types of wastes pointed out higher degree of mineralization in organic solid waste as compared to municipal solid waste.

  13. [Study on the vibrational spectra and XRD characters of Huanglong jade from Longling County, Yunnan Province].

    Science.gov (United States)

    Pei, Jing-cheng; Fan, Lu-wei; Xie, Hao

    2014-12-01

    Based on the conventional test methods, the infrared absorption spectrum, Raman spectrum and X-ray diffraction (XRD) were employed to study the characters of the vibration spectrum and mineral composition of Huanglong jade. The testing results show that Huanglong jade shows typical vibrational spectrum characteristics of quartziferous jade. The main infrared absorption bands at 1162, 1076, 800, 779, 691, 530 and 466 cm(-1) were induced by the asymmetric stretching vibration, symmetrical stretching vibration and bending vibration of Si-O-Si separately. Especially the absorption band near 800 cm(-1) is split, which indicates that Huanglong jade has good crystallinity. In Raman spectrum, the main strong vibration bands at 463 and 355 cm(-1) were attributed to bending vibration of Si-O-Si. XRD test confirmed that Quartz is main mineral composition of Huanglong jade and there is a small amount of hematite in red color samples which induced the red color of Huanglong jade. This is the first report on the infrared, Raman and XRD spectra feature of Huanglong jade. It will provide a scientific basis for the identification, naming and other research for huanglong jade.

  14. Matching 4.7-Å XRD spacing in amelogenin nanoribbons and enamel matrix.

    Science.gov (United States)

    Sanii, B; Martinez-Avila, O; Simpliciano, C; Zuckermann, R N; Habelitz, S

    2014-09-01

    The recent discovery of conditions that induce nanoribbon structures of amelogenin protein in vitro raises questions about their role in enamel formation. Nanoribbons of recombinant human full-length amelogenin (rH174) are about 17 nm wide and self-align into parallel bundles; thus, they could act as templates for crystallization of nanofibrous apatite comprising dental enamel. Here we analyzed the secondary structures of nanoribbon amelogenin by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) and tested if the structural motif matches previous data on the organic matrix of enamel. XRD analysis showed that a peak corresponding to 4.7 Å is present in nanoribbons of amelogenin. In addition, FTIR analysis showed that amelogenin in the form of nanoribbons was comprised of β-sheets by up to 75%, while amelogenin nanospheres had predominantly random-coil structure. The observation of a 4.7-Å XRD spacing confirms the presence of β-sheets and illustrates structural parallels between the in vitro assemblies and structural motifs in developing enamel. © International & American Associations for Dental Research.

  15. XRD and FTIR crystallinity indices in sound human tooth enamel and synthetic hydroxyapatite.

    Science.gov (United States)

    Reyes-Gasga, José; Martínez-Piñeiro, Esmeralda L; Rodríguez-Álvarez, Galois; Tiznado-Orozco, Gaby E; García-García, Ramiro; Brès, Etienne F

    2013-12-01

    The crystallinity index (CI) is a measure of the percentage of crystalline material in a given sample and it is also correlated to the degree of order within the crystals. In the literature two ways are reported to measure the CI: X-ray diffraction and infrared spectroscopy. Although the CI determined by these techniques has been adopted in the field of archeology as a structural order measure in the bone with the idea that it can help e.g. in the sequencing of the bones in chronological and/or stratigraphic order, some debate remains about the reliability of the CI values. To investigate similarities and differences between the two techniques, the CI of sound human tooth enamel and synthetic hydroxyapatite (HAP) was measured in this work by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), at room temperature and after heat treatment. Although the (CI)XRD index is related to the crystal structure of the samples and the (CI)FTIR index is related to the vibration modes of the molecular bonds, both indices showed similar qualitative behavior for heat-treated samples. At room temperature, the (CI)XRD value indicated that enamel is more crystalline than synthetic HAP, while (CI)FTIR indicated the opposite. Scanning (SEM) and transmission (TEM) images were also used to corroborate the measured CI values. © 2013.

  16. Study the oxidation kinetics of uranium using XRD and Rietveld method

    Science.gov (United States)

    Zhang, Yanzhi; Guan, Weijun; Wang, Qinguo; Wang, Xiaolin; Lai, Xinchun; Shuai, Maobing

    2010-03-01

    The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50~300°C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO2 was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO2 can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

  17. Measurement of 2-5 keV x-ray emission from laser-target interactions by using fluor-MCP and CsI-XRD detectors

    International Nuclear Information System (INIS)

    Lee, P.H.Y.; Tirsell, K.G.; Leipelt, G.R.; Laird, W.B.

    1981-01-01

    For inertial confinement fusion plasma diagnostics, x-ray diode (XRD) detectors using conventional cathodes are not sensitive enough to measure x-rays above approx. 1.5 keV. However, for laser driver fusion targets, x-rays in the range of 2 to 5 keV are important because of their mobility in the target. We have successfully used fluor-microchannel plate (MCP) detectors to obtain absolute x-ray measurements in the 2 to 5 keV range. Recent data obtained from experiments on the Shiva laser system are presented. In addition, designs for a variety of channels in the range using fluor-MCP and CsI-XRD's above 1.5 keV will be discussed

  18. JST Thesaurus Headwords and Synonyms: XRD [MeCab user dictionary for science technology term[Archive

    Lifescience Database Archive (English)

    Full Text Available MeCab user dictionary for science technology term XRD 名詞 一般 * * * * X線回折 Xセンカイセツ エックスセンカイセツ Thesaurus2015 200906089250080619 C PA11/PA08 UNKNOWN_1 XRD

  19. [Analysis of XRD spectral characteristics of soil clay mineral in two typical cultivated soils].

    Science.gov (United States)

    Zhang, Zhi-Dan; Luo, Xiang-Li; Jiang, Hai-Chao; Li, Qiao; Shen, Cong-Ying; Liu, Hang; Zhou, Ya-Juan; Zhao, Lan-Po; Wang, Ji-Hong

    2014-07-01

    The present paper took black soil and chernozem, the typical cultivated soil in major grain producing area of Northeast, as the study object, and determinated the soil particle composition characteristics of two cultivated soils under the same climate and location. Then XRD was used to study the composition and difference of clay mineral in two kinds of soil and the evolutionary mechanism was explored. The results showed that the two kinds of soil particles were composed mainly of the sand, followed by clay and silt. When the particle accumulation rate reached 50%, the central particle size was in the 15-130 microm interval. Except for black soil profile of Shengli Xiang, the content of clay showed converse sequence to the central particle in two soils. Clay accumulated under upper layer (18.82%) in black soil profile while under caliche layer (17.41%) in chernozem profile. Clay content was the least in parent material horizon except in black profile of Quanyanling. Analysis of clay XRD atlas showed that the difference lied in not only the strength of diffraction peak, but also in the mineral composition. The main contents of black soil and chernozem were both 2 : 1 clay, the composition of black soil was smectite/illite mixed layer-illite-vermiculite and that of chernozem was S/I mixture-illite-montmorillonite, and both of them contained little kaolinite, chlorite, quartz and other primary mineral. This paper used XRD to determine the characteristics of clay minerals comprehensively, and analyzed two kinds of typical cultivated soil comparatively, and it was a new perspective of soil minerals study.

  20. Composition and microstructure of MTA and Aureoseal Plus: XRF, EDS, XRD and FESEM evaluation.

    Science.gov (United States)

    Cianconi, L; Palopoli, P; Campanella, V; Mancini, M

    2016-12-01

    The aim of this study was to determine the chemical composition and the phases' microstructure of Aureoseal Plus (OGNA, Italy) and ProRoot MTA (Dentsply Tulsa Dental, USA) and to compare their characteristics. Study Design: Comparing Aureoseal Plus and ProRoot MTA microstructure by means of several analyses type. The chemical analysis of the two cements was assessed following the UNI EN ISO 196-2 norm. X-Ray fluorescence (XRF) was used to determine the element composition. The crystalline structure was analysed quantitatively using x-ray diffraction (XRD). Powders morphology was evaluated using a scanning electron microscope (SEM) with backscattering detectors, and a field emission scanning electron microscope (FESEM). Elemental analysis was performed by energy dispersive x-ray analysis (EDS). The semi-quantitative XRF analysis showed the presence of heavy metal oxides in both cements. The XRD spectra of the two cements reported the presence of dicalcium silicate, tricalcium silicate, tricalcium aluminate, tetracalcium aluminoferrite, bismuth oxide and gypsum. SEM analysis showed that ProRoot MTA powder is less coarse and more homogeneous than Aureoseal. Both powders are formed by particles of different shapes: round, prismatic and oblong. The EDS analysis showed that some ProRoot MTA particles, differently from Aureoseal, contain Ca, Si, Al and Fe. Oblong particles in ProRoot and Aureoseal are rich of bismuth. The strong interest in developing new Portland cement-based endodontic sealers will create materials with increased handling characteristics and physicochemical properties. A thorough investigation on two cement powders was carried out by using XRF, XRD, SEM and EDS analysis. To date there was a lack of studies on Aureoseal Plus. This cement is similar in composition to ProRoot MTA. Despite that it has distinctive elements that could improve its characteristics, resulting in a good alternative to MTA.

  1. Quantitative XRD analysis: tools to investigate link between hydrous strain and clay mineral CEC

    International Nuclear Information System (INIS)

    Oueslati, W.; Ammar, M.; Ben Rhaiem, H.; Ben Haj Amara, A.

    2012-01-01

    Document available in extended abstract form only. This work aims at examining, by quantitative XRD analysis, the effect of an applied hydrous strain in the cationic exchange process of a di-octahedral smectite (Na-rich montmorillonite SWy-2). The hydrous constraint was created by a continuous, in situ, hydration-dehydration cycles using a variation of the %RH rate. Respectively, The starting, the intermediate and the final stressed samples was deposed in contact with saturated Me 2+ (i.e. Cd 2+ , Co 2+ , Zn 2+ and Ni 2+ ) chloride solutions respectively in order to examine the effect of the retained materials stress on the CEC of the host materials. An XRD profile modelling approach is adopted to describe all structural changes created by the environmental evolution of the %RH rate. This investigation allowed us to determine several structural parameters related to the nature, abundance, size, position and organization of exchangeable cation and water molecule in the inter-lamellar space along the c* axis. The obtained qualitative results show a considerable change in the hydration behaviour, versus the number of hydration - dehydration cycle, from homogeneous '2W' to heterogeneous '1W-2W' hydration state indicating an interstratified hydration phases and due probably to a new organization of the inter-lamellar space content. Quantitatively, the theoretical Mixed Layer Structure MLS suggest the coexistence of more one 'crystallite' species. Which are saturated by more than one exchangeable cations, indicating a partial saturation of all exchangeable sites. Using optimum structural parameter values, deduced from XRD modelling profile approach, some equations which described the evolution of exchangeable cation amount versus the applied hydrous strain were derived. (authors)

  2. Influence of smectite suspension structure on sheet orientation in dry sediments: XRD and AFM applications.

    Science.gov (United States)

    Zbik, Marek S; Frost, Ray L

    2010-06-15

    The structure-building phenomena within clay aggregates are governed by forces acting between clay particles. Measurements of such forces are important to understand in order to manipulate the aggregate structure for applications such as dewatering of mineral processing tailings. A parallel particle orientation is required when conducting XRD investigation on the oriented samples and conduct force measurements acting between basal planes of clay mineral platelets using atomic force microscopy (AFM). To investigate how smectite clay platelets were oriented on silicon wafer substrate when dried from suspension range of methods like SEM, XRD and AFM were employed. From these investigations, we conclude that high clay concentrations and larger particle diameters (up to 5 microm) in suspension result in random orientation of platelets in the substrate. The best possible laminar orientation in the clay dry film, represented in the XRD 001/020 intensity ratio of 47 was obtained by drying thin layers from 0.02 wt.% clay suspensions of the natural pH. Conducted AFM investigations show that smectite studied in water based electrolytes show very long-range repulsive forces lower in strength than electrostatic forces from double-layer repulsion. It was suggested that these forces may have structural nature. Smectite surface layers rehydrate in water environment forms surface gel with spongy and cellular texture which cushion approaching AFM probe. This structural effect can be measured in distances larger than 1000 nm from substrate surface and when probe penetrate this gel layer, structural linkages are forming between substrate and clay covered probe. These linkages prevent subsequently smooth detachments of AFM probe on way back when retrieval. This effect of tearing new formed structure apart involves larger adhesion-like forces measured in retrieval. It is also suggested that these effect may be enhanced by the nano-clay particles interaction. 2010 Elsevier Inc. All

  3. Micro-XRD and temperature-modulated DSC investigation of nickel-titanium rotary endodontic instruments.

    Science.gov (United States)

    Alapati, Satish B; Brantley, William A; Iijima, Masahiro; Schricker, Scott R; Nusstein, John M; Li, Uei-Ming; Svec, Timothy A

    2009-10-01

    Employ Micro-X-ray diffraction and temperature-modulated differential scanning calorimetry to investigate microstructural phases, phase transformations, and effects of heat treatment for rotary nickel-titanium instruments. Representative as-received and clinically used ProFile GT and ProTaper instruments were principally studied. Micro-XRD analyses (Cu Kalpha X-rays) were performed at 25 degrees C on areas of approximately 50 microm diameter near the tip and up to 9 mm from the tip. TMDSC analyses were performed from -80 to 100 degrees C and back to -80 degrees C on segments cut from instruments, using a linear heating and cooling rate of 2 degrees C/min, sinusoidal oscillation of 0.318 degrees C, and period of 60s. Instruments were also heat treated 15 min in a nitrogen atmosphere at 400, 500, 600 and 850 degrees C, and analyzed. At all Micro-XRD analysis regions the strongest peak occurred near 42 degrees , indicating that instruments were mostly austenite, with perhaps some R-phase and martensite. Tip and adjacent regions had smallest peak intensities, indicative of greater work hardening, and the intensity at other sites depended on the instrument. TMDSC heating and cooling curves had single peaks for transformations between martensite and austenite. Austenite-finish (A(f)) temperatures and enthalpy changes were similar for as-received and used instruments. Heat treatments at 400, 500 and 600 degrees C raised the A(f) temperature to 45-50 degrees C, and heat treatment at 850 degrees C caused drastic changes in transformation behavior. Micro-XRD provides novel information about NiTi phases at different positions on instruments. TMDSC indicates that heat treatment might yield instruments with substantial martensite and improved clinical performance.

  4. Spectral studies of 2-pyrazoline derivatives: structural elucidation through single crystal XRD and DFT calculations.

    Science.gov (United States)

    Chinnaraja, D; Rajalakshmi, R; Srinivasan, T; Velmurugan, D; Jayabharathi, J

    2014-04-24

    A series of biologically active N-thiocarbamoyl pyrazoline derivatives have been synthesized using anhydrous potassium carbonate as the catalyst. All the synthesized compounds were characterized by FT-IR, (1)H NMR, (13)C NMR spectral studies, LCMS, CHN Analysis and X-ray diffraction analysis (compound 7). In order to supplement the XRD parameters, molecular modelling was carried out by Gaussian 03W. From the optimized structure, the energy, dipolemoment and HOMO-LUMO energies of all the systems were calculated. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. The XRD Amorphous Component in John Klein Drill Fines at Yellowknife Bay, Gale Crater, Mars

    Science.gov (United States)

    Morris, Richard V.; Ming,, Douglas W.; Blake, David; Vaniman, David; Bish, David L; Chipera, Steve; Downs, Robert; Morrison, Shaunna; Gellert, Ralf; Campbell, Iain; hide

    2013-01-01

    Drill fines of mudstone (targets John Klein and Cumberland) from the Sheepbed unit at Yel-lowknife Bay were analyzed by MSL payload elements including the Chemistry and Mineralogy (CheMin), APXS (Alpha Particle X-Ray Spectrometer), and Sample Analysis at Mars (SAM) instruments. CheMin XRD results show a variety of crystalline phases including feldspar, pyroxene, olivine, oxides, oxyhydroxides, sulfates, sulfides, a tri-octahedral smectite, and XRD amorphous material. The drill fines are distinctly different from corresponding analyses of the global soil (target Rocknest) in that the mudstone samples contained detectable phyllosilicate. Here we focus on John Klein and combine CheMin and APXS data to calculate the chemical composition and concentration of the amorphous component. The chemical composition of the amorphous plus smectite component for John Klein was calculated by subtracting the abundance-weighted chemical composition of the individual XRD crystalline components from the bulk composition of John Kline as measured by APXS. The chemical composition of individual crystalline components was determined either by stoichiometry (e.g., hematite and magnetite) or from their unit cell parameters (e.g., feldspar, olivine, and pyroxene). The chemical composition of the amorphous + smectite component (approx 71 wt.% of bulk sample) and bulk chemical composition are similar. In order to calculate the chemical composition of the amorphous component, a chemical composition for the tri-octahedral smectite must be assumed. We selected two tri-octahedral smectites with very different MgO/(FeO + Fe2O3) ratios (34 and 1.3 for SapCa1 and Griffithite, respectively). Relative to bulk sample, the concentration of amorphous and smectite components are 40 and 29 wt.% for SapCa1 and 33 and 36 wt.% for Griffithite. The amount of smectite was calculated by requiring the MgO concentration to be approx 0 wt.% in the amorphous component. Griffithite is the preferred smectite because

  6. Analytical electron microscopy of Mg-SiO smokes - A comparison with infrared and XRD studies

    Science.gov (United States)

    Rietmeijer, F. J. M.; Nuth, J. A.; Mackinnon, I. D. R.

    1986-01-01

    Analytical electron microscopy conducted for Mg-SiO smokes (experimentally obtained from samples previously characterized by IR spectroscopy) indicates that the microcrystallinity content of unannealed smokes increases with increased annealing for up to 30 hr. The growth of forsterite microcrystallites in the initially nonstoichiometric smokes may give rise to the contemporaneous growth of the SiO polymorph tridymite and MgO; after 4 hr of annealing, these react to form enstatite. It is suggested that XRD analysis and IR spectroscopy should be conducted in conjunction with detailed analytical electron microscopy for the detection of emerging crystallinity in vapor-phase condensates.

  7. Early Medieval ceramics from the Viile Tecii archaeological site (Romania: an optical and XRD study

    Directory of Open Access Journals (Sweden)

    Corina Ionescu

    2007-10-01

    Full Text Available Mineralogical and petrographic studies of Early Medieval potshards exhumed in the Viile Tecii archaeological site (North Transylvania, Romania show a ceramic body composed of a microcrystalline to amorphous matrix, various clasts and voids. The microscopical features and XRD patterns indicate that illitic-kaolinitic clays were used as raw materials, together with quartzitic sands as tempering material. The ceramic vessels were obtained with the potter’s wheel, but the fabric is only slightly oriented, due either to the fast modeling or to the coarseness of the clayish paste. The thermal alteration of mineral phases points to relatively high firing-temperatures, between 800 and 900°C.

  8. XRD analysis and microstructure of milled and sintered V, W, C, and Co powders

    CSIR Research Space (South Africa)

    Bolokang, AS

    2011-01-01

    Full Text Available on the starting compositions of pure elements, their lattice coherency according to Hume-Rothery rules on crystal structure and atomic size, and enough milling time that provides adequate kinetics. Keywords ? X-ray analysis; ? (V,W)C; ? Co15W8C6...-1 International Journal of Refractory Metals and Hard Materials Volume 29, Issue 1, January 2011, Pages 108?111 XRD analysis and microstructure of milled and sintered V, W, C, and Co powders ? A.S. Bolokang ? M.J. Phasha ? C. Oliphant ? D. Motaung ? a...

  9. XRD, lead equivalent and UV-VIS properties study of Ce and Pr lead silicate glasses

    International Nuclear Information System (INIS)

    Alias, Nor Hayati; Abdullah, Wan Shafie Wan; Isa, Norriza Mohd; Isa, Muhammad Jamal Md; Zali, Nurazila Mat; Abdullah, Nuhaslinda Ee; Muhammad, Azali

    2014-01-01

    In this work, Cerium (Ce) and Praseodymium (Pr) containing lead silicate glasses were produced with 2 different molar ratios low (0.2 wt%) and high (0.4wt%). These types of glasses can satisfy the characteristics required for radiation shielding glasses and minimize the lead composition in glass. The radiation shielding properties of the synthesized glasses is explained in the form of lead equivalent study. The XRD diffraction and UV-VIS analysis were performed to observe the structural changes of the synthesis glasses at 1.5 Gy gamma radiation exposures

  10. Effect of the weather in the aging of asphalts by XRD

    Energy Technology Data Exchange (ETDEWEB)

    Cardoso, Edson da R.; Braz, Delson; Lopes, Ricardo T., E-mail: ecardoso@lin.ufrj.b [Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Programa de Engenharia Nuclear; Motta, Laura M.G. da, E-mail: Laura@coc.ufrj.b [Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Programa de Construcao Civil/Geotecnia; Barroso, Regina C., E-mail: cely@uerj.b [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Inst. de Fisica

    2009-07-01

    Asphalt is a sticky, black and highly viscous liquid or semi-solid that is presented in most crude petroleum and in some natural deposits. As is well known, asphalt has been the preferential choice in pavement construction since excellent utility of pavement, however, as other organic substances, it is also subjected to aging phenomena evolving with time. Asphalt aging is one of the principal factors causing deterioration of asphalt pavements. The photodegradation of asphalts must be considered in the study of the performance of asphalt pavement, especially in geographical regions where high solar radiation intensity occurs. It has an important influence in asphalt aging in tropical places as Brazil. Many methods have been applied to simulate aging of bitumen. It was just a simulation but not real aging asphalt. In this study we submitted the asphalt to the weather as sun and rain. Periodically, during 430 days, the XRD profiles were done and the results analyzed. The scattering measurements were carried out in 0-20 reflection geometry using a powder diffractometer Shimadzu XRD-6000. Scans were typically done from 8 deg to 28 deg every 0.05 deg. The parameters FWHM and peak centroid were analyzed. From 0 until 180 days the aging was faster. The peaks were marked and analyzed with the pass of time. The crystallinity of asphalt increase with weather exposition. Some angles of profiles changed the position indicating change of atomics plans. (author)

  11. Structure and surface morphology studies of cerium oxide system using XRD and SEM analysis

    International Nuclear Information System (INIS)

    Ahmad Jais Alimin; Farid Nasir Ani; Wan Azelee Wan Abu Bakar

    2000-01-01

    Conventional Precious Group Materials (PGM) catalyst systems have been using CeO 2 as an Oxygen Storage Capacity component in the catalyst washcoat. Due to the limitations of the PGM catalyst, researches are now focusing on improving or replacing this conventional system. In a previous work, the potential of a copper-ceria (Cu-Ce) oxide as a catalyst system has been identified. In this paper, the morphology and characterisation of Cu-Ce oxides analysed using XRD and SEM will be described. The Cu-Ce samples were prepared at a fixed ratio under temperatures of 400 o C and 800 o C. XRD diffractograms showed CeO 2 is in a cubic phase at 400 o C and 800 o C. At 800 o C, the CuO particle is visible, presumably has incorporated with the lattice structure of ceria, indicating an absent of solid state condition between copper and ceria. Analysis by SEM revealed significant increase in particle sizes with increasing calcination temperatures. (Author)

  12. Effects of acid treatment on the clay palygorskite: XRD, surface area, morphological and chemical composition

    Energy Technology Data Exchange (ETDEWEB)

    Xavier, Katiane Cruz Magalhaes; Santos, Maria do Socorro Ferreira dos; Santos, Maria Rita Morais Chaves; Oliveira, Marilia Evelyn Rodrigues; Osajima, Josy Antevelli; Silva Filho, Edson Cavalcanti da [Universidade Federal do Piaui (UFPI), Teresina, PI (Brazil); Carvalho, Maria Wilma Nunes Cordeiro, E-mail: edsonfilho@ufpi.edu.br [Universidade Federal de Campina Grande (UFCG), PB (Brazil)

    2014-08-15

    The palygorskite is an aluminum-magnesium silicate that has a fibrous morphology. Their physicochemical characteristics are the result of high surface area, porosity and thermal resistance which make it an attractive adsorbent. Its adsorption capacity can be increased through chemical reactions and/or heat treatments. The objective of this work is to verify the effects of acid activation on the palygorskite, treated with HCl at 90 °C at concentrations of 2, 4 and 6 mol L{sup -1} in 2 and 4 hours, with clay/acid solution ratio 1 g 10 mL{sup -1} and characterized by techniques: XRF, XRD and surface area. A significant increase in specific surface area was observed in the sample treated with HCl at the concentration 6 mol L{sup -1}. The changes were more pronounced at stricter concentrations of acidity, with decreasing intensity of reflection of the clay indicated in the XRD. These changes were confirmed in the XRF with the leaching of some oxides and with increasing concentration of SiO{sub 2}. (author)

  13. Effect of the weather in the aging of asphalts by XRD

    International Nuclear Information System (INIS)

    Cardoso, Edson da R.; Braz, Delson; Lopes, Ricardo T.; Motta, Laura M.G. da; Barroso, Regina C.

    2009-01-01

    Asphalt is a sticky, black and highly viscous liquid or semi-solid that is presented in most crude petroleum and in some natural deposits. As is well known, asphalt has been the preferential choice in pavement construction since excellent utility of pavement, however, as other organic substances, it is also subjected to aging phenomena evolving with time. Asphalt aging is one of the principal factors causing deterioration of asphalt pavements. The photodegradation of asphalts must be considered in the study of the performance of asphalt pavement, especially in geographical regions where high solar radiation intensity occurs. It has an important influence in asphalt aging in tropical places as Brazil. Many methods have been applied to simulate aging of bitumen. It was just a simulation but not real aging asphalt. In this study we submitted the asphalt to the weather as sun and rain. Periodically, during 430 days, the XRD profiles were done and the results analyzed. The scattering measurements were carried out in 0-20 reflection geometry using a powder diffractometer Shimadzu XRD-6000. Scans were typically done from 8 deg to 28 deg every 0.05 deg. The parameters FWHM and peak centroid were analyzed. From 0 until 180 days the aging was faster. The peaks were marked and analyzed with the pass of time. The crystallinity of asphalt increase with weather exposition. Some angles of profiles changed the position indicating change of atomics plans. (author)

  14. The use of micro-XRD for the study of glaze color decorations

    Energy Technology Data Exchange (ETDEWEB)

    Pradell, T.; Molina, G. [Universitat Politecnica de Catalunya, Dpt. Fisica i Enginyeria Nuclear, Castelldefels (Spain); Molera, J.; Pla, J. [Universitat de Vic, GRTD, Escola Politecnica Superior, Vic (Spain); Labrador, A. [BM16-ESRF, LLS, BP 220, Grenoble Cedex (France); Lund University, MAX IV Laboratory, Lund (Sweden)

    2013-04-15

    The compounds responsible for the colors and decorations in glass and glazed ceramics include: coloring agents (transition-metal ions), pigments (micro- and nanoprecipitates of compounds that either do not dissolve or recrystallize in the glassy matrix) and opacifiers (microcrystalline compounds with high light scattering capability). Their composition, structure and range of stability are highly dependent not only on the composition but also on the procedures followed to obtain them. Chemical composition of the colorants and crystallites may be obtained by means of SEM-EDX and WDX. Synchrotron radiation micro-X-ray diffraction (SR-micro-XRD) has a small beam size adequate (10 to 50 microns footprint size) to obtain the structural information of crystalline compounds and high brilliance, optimal for determining the crystallites even when present in low amounts. In addition, in glass decorations the crystallites often appear forming thin layers (from 10 to 100 micrometers thick) and they show a depth-dependent composition and crystal structure. Their nature and distribution across the glass/glaze decorations gives direct information on the technology of production and stability and may be related to the color and appearance. A selection of glass and glaze coloring agents and decorations are studied by means of SR-micro-XRD and SEM-EDX including: manganese brown, antimony yellow, red copper lusters and cobalt blue. The selection includes Medieval (Islamic, and Hispano Moresque) and Renaissance tin-glazed ceramics from the 10th to the 17th century AD. (orig.)

  15. FTIR, XRD and DSC studies of nanochitosan, cellulose acetate and polyethylene glycol blend ultrafiltration membranes.

    Science.gov (United States)

    Vinodhini, P Angelin; K, Sangeetha; Thandapani, Gomathi; P N, Sudha; Jayachandran, Venkatesan; Sukumaran, Anil

    2017-11-01

    In the present work, a series of novel nanochitosan/cellulose acetate/polyethylene glycol (NCS/CA/PEG) blend flat sheet membranes were fabricated in different ratios (1:1:1, 1:1:2, 2:1:1, 2:1:2, 1:2:1, 2:2:1) in a polar solvent of N,N'-dimethylformamide (DMF) using the most popular phase inversion method. Nanochitosan was prepared by the ionotropic gelation method and its average particle size has been analyzed using Dynamic Light Scattering (DLS) method. The effect of blending of the three polymers was investigated using FTIR and XRD studies. FTIR results confirmed the formation of well-blended membranes and the XRD analysis revealed enhanced amorphous nature of the membrane ratio 2:1:2. DSC study was conducted to find out the thermal behavior of the blend membranes and the results clearly indicated good thermal stability and single glass transition temperature (T g ) of all the prepared membranes. Asymmetric nature and rough surface morphology was confirmed using SEM analysis. From the results it was evident that the blending of the polymers with higher concentration of nanochitosan can alter the nature of the resulting membranes to a greater extent and thus amorphous membranes were obtained with good miscibility and compatibility. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Morphological, chemical and structural characterisation of deciduous enamel: SEM, EDS, XRD, FTIR and XPS analysis.

    Science.gov (United States)

    Zamudio-Ortega, C M; Contreras-Bulnes, R; Scougall-Vilchis, R J; Morales-Luckie, R A; Olea-Mejía, O F; Rodríguez-Vilchis, L E

    2014-09-01

    The purpose of this study was to characterise the enamel surface of sound deciduous teeth in terms of morphology, chemical composition, structure and crystalline phases. The enamel of 30 human deciduous teeth was examined by: Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS), X-ray Powder Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and X-ray Photoelectron Spectroscopy (XPS). Chemical differences between incisors and canines were statistically evaluated using the Mann-Whitney U test (p ≤ 0.05). Three enamel patterns were observed by SEM: 'mostly smooth with some groves', 'abundant microporosities' and 'exposed prisms'. The average Ca/P molar ratios were 1.37 and 1.03 by EDS and XPS, respectively. The crystallite size determined by XRD was 210.82 ± 16.78 Å. The mean ratio between Ca bonded to phosphate and Ca bonded to hydroxyl was approximately 10:1. The enamel of sound deciduous teeth showed two main patterns: 'mostly smooth with some groves' and 'abundant microporosities'. 'Exposed prisms' was a secondary pattern. There were slight variations among the Ca/P molar ratios found by EDS and XPS, suggesting differences in the mineral content from the enamel surface to the interior. The crystalline phases found in enamel were hydroxyapatite and carbonate apatite, with major type B than type A carbonate incorporation.

  17. Trace elemental analysis of Indian natural moonstone gems by PIXE and XRD techniques.

    Science.gov (United States)

    Venkateswara Rao, R; Venkateswarulu, P; Kasipathi, C; Sivajyothi, S

    2013-12-01

    A selected number of Indian Eastern Ghats natural moonstone gems were studied with a powerful nuclear analytical and non-destructive Proton Induced X-ray Emission (PIXE) technique. Thirteen elements, including V, Co, Ni, Zn, Ga, Ba and Pb, were identified in these moonstones and may be useful in interpreting the various geochemical conditions and the probable cause of their inceptions in the moonstone gemstone matrix. Furthermore, preliminary XRD studies of different moonstone patterns were performed. The PIXE technique is a powerful method for quickly determining the elemental concentration of a substance. A 3MeV proton beam was employed to excite the samples. The chemical constituents of moonstones from parts of the Eastern Ghats geological formations of Andhra Pradesh, India were determined, and gemological studies were performed on those gems. The crystal structure and the lattice parameters of the moonstones were estimated using X-Ray Diffraction studies, trace and minor elements were determined using the PIXE technique, and major compositional elements were confirmed by XRD. In the present work, the usefulness and versatility of the PIXE technique for research in geo-scientific methodology is established. © 2013 Elsevier Ltd. All rights reserved.

  18. XRD- and infrared-probed anisotropic thermal expansion properties of an organic semiconducting single crystal.

    Science.gov (United States)

    Mohanraj, J; Capria, E; Benevoli, L; Perucchi, A; Demitri, N; Fraleoni-Morgera, A

    2018-01-17

    The anisotropic thermal expansion properties of an organic semiconducting single crystal constituted by 4-hydroxycyanobenzene (4HCB) have been probed by XRD in the range 120-300 K. The anisotropic thermal expansion coefficients for the three crystallographic axes and for the crystal volume have been determined. A careful analysis of the crystal structure revealed that the two different H-bonds stemming from the two independent, differently oriented 4HCB molecules composing the unit cell have different rearrangement patterns upon temperature variations, in terms of both bond length and bond angle. Linearly Polarized Mid InfraRed (LP-MIR) measurements carried out in the same temperature range, focused on the O-H bond spectral region, confirm this finding. The same LP-MIR measurements, on the basis of a semi-empirical relation and of geometrical considerations and assumptions, allowed calculation of the -CNH-O- hydrogen bond length along the a and b axes of the crystal. In turn, the so-calculated -CNH-O- bond lengths were used to derive the thermal expansion coefficients along the corresponding crystal axes, as well as the volumetric one, using just the LP-MIR data. Reasonable to good agreement with the same values obtained from XRD measurements was obtained. This proof-of-principle opens interesting perspectives about the possible development of a rapid, low cost and industry-friendly assessment of the thermal expansion properties of organic semiconducting single crystals (OSSCs) involving hydrogen bonds.

  19. XRD, TEM, and thermal analysis of Arizona Ca-montmorillonites modified with didodecyldimethylammonium bromide.

    Science.gov (United States)

    Sun, Zhiming; Park, Yuri; Zheng, Shuilin; Ayoko, Godwin A; Frost, Ray L

    2013-10-15

    An Arizona SAz-2 calcium montmorillonite was modified by a typical dialkyl cationic surfactant (didodecyldimethylammonium bromide, abbreviated to DDDMA) through direct ion exchange. The obtained organoclays were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), high-resolution thermogravimetric analysis (HR-TG), and infrared emission spectroscopy (IES). The intercalation of surfactants greatly increased the basal spacing of the interlayers and the conformation arrangement of the loaded surfactant were assessed based on the XRD and TEM measurements. This work shows that the dialkyl surfactant can be directly intercalated into the montmorillonite without first undergoing Na(+) exchange. Moreover, the thermal stability of organoclays and the different arrangements of the surfactant molecules intercalated in the SAz-2 Ca-montmorillonite were determined by a combination of TG and IES techniques. The detailed conformational ordering of different intercalated surfactants under different conditions was also studied. The surfactant molecule DDDMA has proved to be thermally stable even at 400°C which indicates that the prepared organoclay is stable to significantly high temperatures. This study offers new insights into the structure and thermal stabilities of SAz-2 Ca-montmorillonite modified with DDDMA. The experimental results also confirm the potential applications of organic SAz-2 Ca-montmorillonites as adsorbents and polymer-clay nanocomposites. Copyright © 2013 Elsevier Inc. All rights reserved.

  20. Modeling and measurements of XRD spectra of extended solids under high pressure

    Science.gov (United States)

    Batyrev, I. G.; Coleman, S. P.; Stavrou, E.; Zaug, J. M.; Ciezak-Jenkins, J. A.

    2017-06-01

    We present results of evolutionary simulations based on density functional calculations of various extended solids: N-Si and N-H using variable and fixed concentration methods of USPEX. Predicted from the evolutionary simulations structures were analyzed in terms of thermo-dynamical stability and agreement with experimental X-ray diffraction spectra. Stability of the predicted system was estimated from convex-hull plots. X-ray diffraction spectra were calculated using a virtual diffraction algorithm which computes kinematic diffraction intensity in three-dimensional reciprocal space before being reduced to a two-theta line profile. Calculations of thousands of XRD spectra were used to search for a structure of extended solids at certain pressures with best fits to experimental data according to experimental XRD peak position, peak intensity and theoretically calculated enthalpy. Comparison of Raman and IR spectra calculated for best fitted structures with available experimental data shows reasonable agreement for certain vibration modes. Part of this work was performed by LLNL, Contract DE-AC52-07NA27344. We thank the Joint DoD / DOE Munitions Technology Development Program, the HE C-II research program at LLNL and Advanced Light Source, supported by BES DOE, Contract No. DE-AC02-05CH112.

  1. The chaotic points and XRD analysis of Hg-based superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Aslan, Oe [Anatuerkler Educational Consultancy and Trading Company, Orhan Veli Kanik Cad., 6/1, Kavacik 34810 Beykoz, Istanbul (Turkey); Oezdemir, Z Gueven [Physics Department, Yildiz Technical University, Davutpasa Campus, Esenler 34210, Istanbul (Turkey); Keskin, S S [Department of Environmental Eng., University of Marmara, Ziverbey, 34722, Istanbul (Turkey); Onbasli, Ue, E-mail: ozdenaslan@yahoo.co [Physics Department, University of Marmara, Ridvan Pasa Cad. 3. Sok. 85/12 Goztepe, Istanbul (Turkey)

    2009-03-01

    In this article, high T{sub c} mercury based cuprate superconductors with different oxygen doping rates have been examined by means of magnetic susceptibility (magnetization) versus temperature data and X-ray diffraction pattern analysis. The under, optimally and over oxygen doping procedures have been defined from the magnetic susceptibility versus temperature data of the superconducting sample by extracting the Meissner critical transition temperature, T{sub c} and the paramagnetic Meissner temperature, T{sub PME}, so called as the critical quantum chaos points. Moreover, the optimally oxygen doped samples have been investigated under both a.c. and d.c. magnetic fields. The related a.c. data for virgin(uncut) and cut samples with optimal doping have been obtained under a.c. magnetic field of 1 Gauss. For the cut sample with the rectangular shape, the chaotic points have been found to occur at 122 and 140 K, respectively. The Meissner critical temperature of 140 K is the new world record for the high temperature oxide superconductors under normal atmospheric pressure. Moreover, the crystallographic lattice parameters of superconducting samples have a crucial importance in calculating Josephson penetration depth determined by the XRD patterns. From the XRD data obtained for under and optimally doped samples, the crystal symmetries have been found in tetragonal structure.

  2. Radiometric, SEM and XRD investigation of the Chituc black sands, southern Danube Delta, Romania

    International Nuclear Information System (INIS)

    Margineanu, R.M.; Blebea-Apostu, Ana-Maria; Celarel, Aurelia; Gomoiu, Claudia-Mariana; Costea, C.; Dumitras, Delia; Ion, Adriana; Duliu, O.G.

    2014-01-01

    The black sand of the Chituc marine sand bank, northern of the city of Navodari (Romania), presents anomalous high radioactivity. Field measurements recorded in some places dose rate up to 200 nSv/h, significantly overpassing the average value of 44 ± 20 nSv/h along the entire Southern sector of Romanian Black Sea shore. Gamma ray spectrometry performed on both Slanic-Prahova Underground Low Background Laboratory and Geological Institute of Romania Radiometric Facilities showed with clarity the dominance of 228 Ac radioisotope in the 50 microns fraction together with the 226 Ra and traces of 40 K. No significant amount of anthropogenic 137 Cs was identified. Based on radiometric as well as on SEM–EDAX and XRD determinations we come to the conclusion that the evidenced radioactivity could be attributed to both uranium and thorium series in the zircon and monazite fractions and to a lesser extent to potassium in the feldspars. - Highlights: • High background radioactivity (up to 200 nSv/h) evidenced. • Radiometric measurements showed a maximum radioactivity of U and Th confined to 50–100 μm fraction. • XRD and SEM–EDAX data revealed the presence of k-feldspars, ilmenite, zircone, monazite and garnets

  3. Lupeol and its esters: NMR, powder XRD data and in vitro evaluation of cancer cell growth

    Directory of Open Access Journals (Sweden)

    Aline Teixeira Maciel e Silva

    2018-02-01

    Full Text Available ABSTRACT The triterpene lupeol (1 and some of its esters are secondary metabolites produced by species of Celastraceae family, which have being associated with cytotoxic activity. We report herein the isolation of 1, the semi-synthesis of eight lupeol esters and the evaluation of their in vitro activity against nine strains of cancer cells. The reaction of carboxylic acids with 1 and DIC/DMAP was used to obtain lupeol stearate (2, lupeol palmitate (3 lupeol miristate (4, and the new esters lupeol laurate (5, lupeol caprate (6, lupeol caprilate (7, lupeol caproate (8 and lupeol 3’,4’-dimethoxybenzoate (9, with high yields. Compounds 1-9 were identified using FT-IR, 1H, 13C-NMR, CHN analysis and XRD data and were tested in vitro for proliferation of human cancer cell activity. In these assays, lupeol was inactive (GI50> 250µg/mL while lupeol esters 2 -4 and 7 - 9 showed a cytostatic effect. The XRD method was a suitable tool to determine the structure of lupeol and its esters in solid state. Compound 3 showed a selective growth inhibition effect on erythromyeloblastoid leukemia (K-562 cells in a concentration-dependent way. Lupeol esters 4 and 9 showed a selective cytostatic effect with low GI50 values representing promising prototypes for the development of new anticancer drugs.

  4. Determination of equilibrium humidities using temperature and humidity controlled X-ray diffraction (RH-XRD)

    International Nuclear Information System (INIS)

    Linnow, Kirsten; Steiger, Michael

    2007-01-01

    Confined growth of crystals in porous building materials is generally considered to be a major cause of damage. We report on the use of X-ray diffraction under controlled conditions of temperature and relative humidity (RH-XRD) for the investigation of potentially deleterious phase transition reactions. An improved procedure based on rate measurements is used for the accurate and reproducible determination of equilibrium humidities of deliquescence and hydration reactions. The deliquescence humidities of NaCl (75.4 ± 0.5% RH) and Ca(NO 3 ) 2 .4H 2 O (50.8 ± 0.7% RH) at 25 deg. C determined with this improved RH-XRD technique are in excellent agreement with available literature data. Measurement of the hydration of anhydrous Ca(NO 3 ) 2 to form Ca(NO 3 ) 2 .2H 2 O revealed an equilibrium humidity of 10.2 ± 0.3%, which is also in reasonable agreement with available data. In conclusion, dynamic X-ray diffraction measurements are an appropriate method for the accurate and precise determination of equilibrium humidities with a number of interesting future applications

  5. Moessbauer and XRD study of pulse plated Fe-P and Fe-Ni thin layers

    Energy Technology Data Exchange (ETDEWEB)

    Miko, Annamaria [Bay Zoltan Institute for Material Science (Hungary); Kuzmann, Erno, E-mail: kuzmann@para.chem.elte.hu [Eoetvoes Lorand University, Research Group for Nuclear Methods in Structural Chemistry, Hungarian Academy of Sciences, Department of Nuclear Chemistry (Hungary); Lakatos-Varsanyi, Magda [Bay Zoltan Institute for Material Science (Hungary); Kakay, Attila [Research Institute for Solid State Physics and Optics (Hungary); Nagy, Ferenc [Eoetvoes Lorand University, Research Group for Nuclear Methods in Structural Chemistry, Hungarian Academy of Sciences, Department of Nuclear Chemistry (Hungary); Varga, Lajos Karoly [Research Institute for Solid State Physics and Optics (Hungary)

    2005-09-15

    {sup 57}Fe conversion electron Moessbauer spectroscopy, X-ray diffraction, electrochemical and magnetic measurements were used to study pulse electroplated Fe-P and Ni-Fe coatings. XRD and {sup 57}Fe CEMS measurements revealed the amorphous character of the novel pulse plated Fe-P alloys. CEM spectra indicated significant differences in the short range order and in the magnetic anisotropy between the Fe-P deposits pulse plated at medium long deposition time (t{sub on} = 2 ms), with short relaxation time (t{sub off} = 9 ms) and low current density (I{sub p} = 0.05 Acm{sup -2}) or at short deposition time (t{sub on} = 1 ms) with long relaxation time (t{sub off} = 250 ms) and high current density (I{sub p} = 1.0 Acm{sup -2}). The broad peaks centred around the fcc reflections in XRD of the pulse plated Ni-22 wt.% Fe deposit reflected a microcrystalline Ni-Fe alloy with a very fine, 5-8 nm, grain size. The CEM spectrum of the pulse plated Ni-22 wt.% Fe coating corresponded to a highly disordered solid solution alloy containing a minute amount of ferrihydrite. Extreme favourable soft magnetic properties were observed with these Ni-Fe and Fe-P pulse plated thin layers.

  6. Moessbauer and XRD study of pulse plated Fe-P and Fe-Ni thin layers

    International Nuclear Information System (INIS)

    Miko, Annamaria; Kuzmann, Erno; Lakatos-Varsanyi, Magda; Kakay, Attila; Nagy, Ferenc; Varga, Lajos Karoly

    2005-01-01

    57 Fe conversion electron Moessbauer spectroscopy, X-ray diffraction, electrochemical and magnetic measurements were used to study pulse electroplated Fe-P and Ni-Fe coatings. XRD and 57 Fe CEMS measurements revealed the amorphous character of the novel pulse plated Fe-P alloys. CEM spectra indicated significant differences in the short range order and in the magnetic anisotropy between the Fe-P deposits pulse plated at medium long deposition time (t on = 2 ms), with short relaxation time (t off = 9 ms) and low current density (I p = 0.05 Acm -2 ) or at short deposition time (t on = 1 ms) with long relaxation time (t off = 250 ms) and high current density (I p = 1.0 Acm -2 ). The broad peaks centred around the fcc reflections in XRD of the pulse plated Ni-22 wt.% Fe deposit reflected a microcrystalline Ni-Fe alloy with a very fine, 5-8 nm, grain size. The CEM spectrum of the pulse plated Ni-22 wt.% Fe coating corresponded to a highly disordered solid solution alloy containing a minute amount of ferrihydrite. Extreme favourable soft magnetic properties were observed with these Ni-Fe and Fe-P pulse plated thin layers.

  7. Insight into the Am-O Phase Equilibria: A Thermodynamic Study Coupling High-Temperature XRD and CALPHAD Modeling.

    Science.gov (United States)

    Epifano, Enrica; Guéneau, Christine; Belin, Renaud C; Vauchy, Romain; Lebreton, Florent; Richaud, Jean-Christophe; Joly, Alexis; Valot, Christophe; Martin, Philippe M

    2017-07-03

    In the frame of minor actinide transmutation, americium can be diluted in UO 2 and (U, Pu)O 2 fuels burned in fast neutron reactors. The first mandatory step to foresee the influence of Am on the in-reactor behavior of transmutation targets or fuel is to have fundamental knowledge of the Am-O binary system and, in particular, of the AmO 2-x phase. In this study, we coupled HT-XRD (high-temperature X-ray diffraction) experiments with CALPHAD thermodynamic modeling to provide new insights into the structural properties and phase equilibria in the AmO 2-x -AmO 1.61+x -Am 2 O 3 domain. Because of this approach, we were able for the first time to assess the relationships between temperature, lattice parameter, and hypostoichiometry for fcc AmO 2-x . We showed the presence of a hyperstoichiometric existence domain for the bcc AmO 1.61+x phase and the absence of a miscibility gap in the fcc AmO 2-x phase, contrary to previous representations of the phase diagram. Finally, with the new experimental data, a new CALPHAD thermodynamic model of the Am-O system was developed, and an improved version of the phase diagram is presented.

  8. XRD and SEM study on the phase separation and crystallization behavior for an amorphous Cu+ conductor

    International Nuclear Information System (INIS)

    Yang Yuan; Hou Jianguo; Yu Wenhai

    1990-01-01

    The X-ray diffraction (XRD) and scanning electron microscopy (SEM) study was carried out for an amorphous Cu + conductor 0.4 CuI-0.3 Cu 2 O-0.3 P 2 O 5 with the simultaneous conductivity measurement in the isothermal heat treament process. The results indicated that the initial amorphous material was phase-separated. In the course of time the separated amorphous phase disappeared, the crystalline γ-CuI and Cu 2 P 2 O 7 formed in sequence and grew up gradually. The correlation of the phase separation and crystallization behavior with the conductivity anomaly confirmed again the interface effect between different phases in amorphous fast ionic conductors and its universality

  9. Investigation of synthetic spider silk crystallinity and alignment via electrothermal, pyroelectric, literature XRD, and tensile techniques.

    Science.gov (United States)

    Munro, Troy; Putzeys, Tristan; Copeland, Cameron G; Xing, Changhu; Lewis, Randolph V; Ban, Heng; Glorieux, Christ; Wubbenhorst, Michael

    2017-04-01

    The processes used to create synthetic spider silk greatly affect the properties of the produced fibers. This paper investigates the effect of process variations during artificial spinning on the thermal and mechanical properties of the produced silk. Property values are also compared to the ones of the natural dragline silk of the N. clavipes spider, and to unprocessed (as-spun) synthetic silk. Structural characterization by scanning pyroelectric microscopy is employed to provide insight into the axial orientation of the crystalline regions of the fiber and is supported by XRD data. The results show that stretching and passage through liquid baths induce crystal formation and axial alignment in synthetic fibers, but with different structural organization than natural silks. Furthermore, an increase in thermal diffusivity and elastic modulus is observed with decreasing fiber diameter, trending towards properties of natural fiber. This effect seems to be related to silk fibers being subjected to a radial gradient during production.

  10. XRD analysis of undoped and Fe doped TiO2 nanoparticles by Williamson Hall method

    International Nuclear Information System (INIS)

    Bharti, Bandna; Barman, P. B.; Kumar, Rajesh

    2015-01-01

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

  11. XRD total scattering of the CZTS nanoparticle absorber layer for the thin film solar cells

    DEFF Research Database (Denmark)

    Symonowicz, Joanna; Jensen, Kirsten M. Ø.; Engberg, Sara Lena Josefin

    Cu2ZnSnS4 (CZTS) thin film solar cells are cheap, non-toxic and present an efficiency up to 9,2% [1]. They can be easily manufactured by the deposition of the nanoparticle ink as a thin film followed by a thermal treatment to obtain large grains [2]. Therefore, CZTS has the potential...... to revolutionize the solar energy market. However, to commercialize CZTS nanoparticle thin films, the efficiency issues must yet be resolved. In order to do so, it is vital to understand in detail their nanoscale atomic structure. CZTS crystallize in the kesterite structure, where Cu and Zn is distributed between......-ray Diffraction data with X-ray total scattering with Pair Distribution Function analysis. Powder neutron diffraction will furthermore allow characterization of the cation disorder on the metal sites in the kesterite structure. The nanoparticle ink is also characterized by XRD, EDS, and Raman spectroscopy...

  12. Different β-alanine dimeric forms in trifluoromethanesulfonic acid salts. XRD and vibrational studies

    Science.gov (United States)

    Wołoszyn, Łukasz; Ilczyszyn, Maria M.

    2018-03-01

    Two new crystalline salts: β-alaninium trifluoromethanesulfonate (β-AlaOTf) and bis(β-alanine) trifluoromethanesulfonate (β-2AlaOTf) were obtained. The former one contains diprotonated β-alanine dimer, the latter one monoprotonated β-alanine dimer. Both compounds were studied by single crystal XRD, vibrational (IR and Raman) spectroscopy and calorimetric method. The quantum-mechanical calculations (DFT/B3LYP/6-311 ++G(2d,2p)) for the diprotonated dimer were carried out. The β-AlaOTf salt crystallizes in the P 1 bar space group of triclinic system (Z = 2), the β-2AlaOTf in the P21/m space group of monoclinic system (Z = 2). The vibrational data for the studied compounds are discussed in relation to their crystal structure, and provide insight into the character of hydrogen bonds and β-alanine protonation. The studied crystals do not exhibit phase transitions in the solid state.

  13. Crystal imperfection studies of pure and silicon substituted hydroxyapatite using Raman and XRD.

    Science.gov (United States)

    Zou, Shuo; Huang, Jie; Best, Serena; Bonfield, William

    2005-12-01

    Hydroxyapatite (HA) is important in biomedical applications because of its chemical similarity to the mineral content of bone and its consequent bioactivity. Silicon substitution into the hydroxyapatite crystal lattice was found to enhance its bioactivity both in vitro and in vivo [1, 2]. However, the mechanism for the enhancement is still not well understood. In this paper, the crystal imperfections introduced by silicon substitution were studied using XRD and Raman spectroscopy. It was found that silicon substitution did not introduce microstrain, but deceased the crystal size in the hk0 direction. Three new vibration modes and peak broadening were observed in Raman spectra following silicon incorporation. The imperfections introduced by silicon substitution may play a role in enhancing bioactivity. A phenomenological relationship between the width of the PO4 v1 peak and crystal size was established.

  14. Spectroscopic, DFT, and XRD Studies of Hydrogen Bonds in N-Unsubstituted 2-Aminobenzamides.

    Science.gov (United States)

    Mphahlele, Malose Jack; Maluleka, Marole Maria; Rhyman, Lydia; Ramasami, Ponnadurai; Mampa, Richard Mokome

    2017-01-04

    The structures of the mono- and the dihalogenated N -unsubstituted 2-aminobenzamides were characterized by means of the spectroscopic (¹H-NMR, UV-Vis, FT-IR, and FT-Raman) and X-ray crystallographic techniques complemented with a density functional theory (DFT) method. The hindered rotation of the C(O)-NH₂ single bond resulted in non-equivalence of the amide protons and therefore two distinct resonances of different chemical shift values in the ¹H-NMR spectra of these compounds were observed. 2-Amino-5-bromobenzamide ( ABB ) as a model confirmed the presence of strong intramolecular hydrogen bonds between oxygen and the amine hydrogen. However, intramolecular hydrogen bonding between the carbonyl oxygen and the amine protons was not observed in the solution phase due to a rapid exchange of these two protons with the solvent and fast rotation of the Ar-NH₂ single bond. XRD also revealed the ability of the amide unit of these compounds to function as a hydrogen bond donor and acceptor simultaneously to form strong intermolecular hydrogen bonding between oxygen of one molecule and the NH moiety of the amine or amide group of the other molecule and between the amine nitrogen and the amide hydrogen of different molecules. DFT calculations using the B3LYP/6-311++G(d,p) basis set revealed that the conformer ( A ) with oxygen and 2-amine on the same side predominates possibly due to the formation of a six-membered intramolecular ring, which is assisted by hydrogen bonding as observed in the single crystal XRD structure.

  15. Reduction of mixed Mn-Zr oxides: in situ XPS and XRD studies.

    Science.gov (United States)

    Bulavchenko, O A; Vinokurov, Z S; Afonasenko, T N; Tsyrul'nikov, P G; Tsybulya, S V; Saraev, A A; Kaichev, V V

    2015-09-21

    A series of mixed Mn-Zr oxides with different molar ratios Mn/Zr (0.1-9) have been prepared by coprecipitation of manganese and zirconium nitrates and characterized by X-ray diffraction (XRD) and BET methods. It has been found that at concentrations of Mn below 30 at%, the samples are single-phase solid solutions (MnxZr1-xO2-δ) based on a ZrO2 structure. X-ray photoelectron spectroscopy (XPS) measurements showed that manganese in these solutions exists mainly in the Mn(4+) state on the surface. An increase in Mn content mostly leads to an increase in the number of Mn cations in the structure of solid solutions; however, a part of the manganese cations form Mn2O3 and Mn3O4 in the crystalline and amorphous states. The reduction of these oxides with hydrogen was studied by a temperature-programmed reduction technique, in situ XRD, and near ambient pressure XPS in the temperature range from 100 to 650 °C. It was shown that the reduction of the solid solutions MnxZr1-xO2-δ proceeds via two stages. During the first stage, at temperatures between 100 and 500 °C, the Mn cations incorporated into the solid solutions MnxZr1-xO2-δ undergo partial reduction. During the second stage, at temperatures between 500 and 700 °C, Mn cations segregate on the surface of the solid solution. In the samples with more than 30 at% Mn, the reduction of manganese oxides was observed: Mn2O3 → Mn3O4 → MnO.

  16. Thermal decomposition of dolomite under CO2: insights from TGA and in situ XRD analysis.

    Science.gov (United States)

    Valverde, Jose Manuel; Perejon, Antonio; Medina, Santiago; Perez-Maqueda, Luis A

    2015-11-28

    Thermal decomposition of dolomite in the presence of CO2 in a calcination environment is investigated by means of in situ X-ray diffraction (XRD) and thermogravimetric analysis (TGA). The in situ XRD results suggest that dolomite decomposes directly at a temperature around 700 °C into MgO and CaO. Immediate carbonation of nascent CaO crystals leads to the formation of calcite as an intermediate product of decomposition. Subsequently, decarbonation of this poorly crystalline calcite occurs when the reaction is thermodynamically favorable and sufficiently fast at a temperature depending on the CO2 partial pressure in the calcination atmosphere. Decarbonation of this dolomitic calcite occurs at a lower temperature than limestone decarbonation due to the relatively low crystallinity of the former. Full decomposition of dolomite leads also to a relatively low crystalline CaO, which exhibits a high reactivity as compared to limestone derived CaO. Under CO2 capture conditions in the Calcium-Looping (CaL) process, MgO grains remain inert yet favor the carbonation reactivity of dolomitic CaO especially in the solid-state diffusion controlled phase. The fundamental mechanism that drives the crystallographic transformation of dolomite in the presence of CO2 is thus responsible for its fast calcination kinetics and the high carbonation reactivity of dolomitic CaO, which makes natural dolomite a potentially advantageous alternative to limestone for CO2 capture in the CaL technology as well as SO2in situ removal in oxy-combustion fluidized bed reactors.

  17. Spectroscopic, DFT, and XRD Studies of Hydrogen Bonds in N-Unsubstituted 2-Aminobenzamides

    Directory of Open Access Journals (Sweden)

    Malose Jack Mphahlele

    2017-01-01

    Full Text Available The structures of the mono- and the dihalogenated N-unsubstituted 2-aminobenzamides were characterized by means of the spectroscopic (1H-NMR, UV-Vis, FT-IR, and FT-Raman and X-ray crystallographic techniques complemented with a density functional theory (DFT method. The hindered rotation of the C(O–NH2 single bond resulted in non-equivalence of the amide protons and therefore two distinct resonances of different chemical shift values in the 1H-NMR spectra of these compounds were observed. 2-Amino-5-bromobenzamide (ABB as a model confirmed the presence of strong intramolecular hydrogen bonds between oxygen and the amine hydrogen. However, intramolecular hydrogen bonding between the carbonyl oxygen and the amine protons was not observed in the solution phase due to a rapid exchange of these two protons with the solvent and fast rotation of the Ar–NH2 single bond. XRD also revealed the ability of the amide unit of these compounds to function as a hydrogen bond donor and acceptor simultaneously to form strong intermolecular hydrogen bonding between oxygen of one molecule and the NH moiety of the amine or amide group of the other molecule and between the amine nitrogen and the amide hydrogen of different molecules. DFT calculations using the B3LYP/6-311++G(d,p basis set revealed that the conformer (A with oxygen and 2-amine on the same side predominates possibly due to the formation of a six-membered intramolecular ring, which is assisted by hydrogen bonding as observed in the single crystal XRD structure.

  18. Data from the Mars Science Laboratory CheMin XRD/XRF Instrument

    Science.gov (United States)

    Vaniman, David; Blake, David; Bristow, Tom; DesMarais, David; Achilles, Cherie; Anderson, Robert; Crips, Joy; Morookian, John Michael; Spanovich, Nicole; Vasavada, Ashwin; hide

    2013-01-01

    The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity uses a Co tube source and a CCD detector to acquire mineralogy from diffracted primary X-rays and chemical information from fluoresced X-rays. CheMin has been operating at the MSL Gale Crater field site since August 5, 2012 and has provided the first X-ray diffraction (XRD) analyses in situ on a body beyond Earth. Data from the first sample collected, the Rocknest eolian soil, identify a basaltic mineral suite, predominantly plagioclase (approx.An50), forsteritic olivine (approx.Fo58), augite and pigeonite, consistent with expectation that detrital grains on Mars would reflect widespread basaltic sources. Minor phases (each XRD. This amorphous component is attested to by a broad rise in background centered at approx.27deg 2(theta) (Co K(alpha)) and may include volcanic glass, impact glass, and poorly crystalline phases including iron oxyhydroxides; a rise at lower 2(theta) may indicate allophane or hisingerite. Constraints from phase chemistry of the crystalline components, compared with a Rocknest bulk composition from the APXS instrument on Curiosity, indicate that in sum the amorphous or poorly crystalline components are relatively Si, Al, Mg-poor and enriched in Ti, Cr, Fe, K, P, S, and Cl. All of the identified crystalline phases are volatile-free; H2O, SO2 and CO2 volatile releases from a split of this sample analyzed by the SAM instrument on Curiosity are associated with the amorphous or poorly ordered materials. The Rocknest eolian soil may be a mixture of local detritus, mostly crystalline, with a regional or global set of dominantly amorphous or poorly ordered components. The Rocknest sample was targeted by MSL for "first time analysis" to demonstrate that a loose deposit could be scooped, sieved to <150 microns, and delivered to instruments in the body of the rover. A drilled sample of sediment in outcrop is anticipated. At the time of writing this abstract, promising outcrops are

  19. XRD monitoring of α self-irradiation in uranium-americium mixed oxides.

    Science.gov (United States)

    Horlait, Denis; Lebreton, Florent; Roussel, Pascal; Delahaye, Thibaud

    2013-12-16

    The structural evolution under (241)Am self-irradiation of U(1-x)Am(x)O(2±δ) transmutation fuels (with x ≤ 0.5) was studied by X-ray diffraction (XRD). Samples first underwent a preliminary heat treatment performed under a reducing atmosphere (Ar/H2(4%)) aiming to recover the previously accumulated structural defects. Over all measurements (carried out over up to a full year and for integrated doses up to 1.5 × 10(18) α-decay events·g(-1)), only fluorite U(1-x)Am(x)O(2±δ) solid solutions were observed. Within a few days after the end of the heat treatment, each of the five studied samples was slowly oxidized as a consequence of their move to air atmosphere, which is evidenced by XRD by an initial sharp decrease of the unit cell parameter. For the compounds with x ≤ 0.15, this oxidation occurred without any phase transitions, but for U0.6Am0.4O(2±δ) and U0.5Am0.5O(2±δ), this process is accompanied by a transition from a first fluorite solid solution to a second oxidized one, as the latter is thermodynamically stable in ambient conditions. In the meantime and after the oxidation process, (241)Am α self-irradiation caused a structural swelling up to ∼0.8 vol %, independently of the sample composition. The kinetic constants of swelling were also determined by regression of experimental data and are, as expected, dependent on x and thus on the dose rate. The normalization of these kinetic constants by sample α-activity, however, leads to very close swelling rates among the samples. Finally, evolutions of microstrain and crystallite size were also monitored, but for the considered dose rates and cumulated doses, α self-irradiation was found, within the limits of the diffractometer used, to have almost no impact on these characteristics. Microstrain was found to be influenced instead by the americium content in the materials (i.e., by the impurities associated with americium starting material and the increase of cationic charge heterogeneity with

  20. Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

    Science.gov (United States)

    Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

    2004-01-01

    A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

  1. Synthesis, XRD, TEM, EPR, and Optical Absorption Spectral Studies of CuZnO2 Nanocompound

    Directory of Open Access Journals (Sweden)

    T. Ravindra Reddy

    2014-01-01

    Full Text Available Synthesis of nano CuZnO2 compound is carried out by thermal decomposition method. The crystalline phase of the material is characterized by XRD. The calculated unit cell constants are a=3.1 Å and c=3.4786 Å and are of tetragonal structure. The unit cell constants are different from wurtzite (hexagonal which indicate that a nanocompound is formed. Further TEM images reveal that the metal ion is in tetragonal structure with oxygen ligands. The prepared CuZnO2 is then characterized for crystallite size analysis by employing transmission electron microscopy (TEM. The size is found to be 100 nm. Uniform bright rings are noticed in the TEM picture suggesting that the nanocrystals have preferential instead of random orientations. The selected-area electron diffraction (SAED pattern clearly indicates the formation of CuO-ZnO nanocompound. The nature of bonding is studied by electron paramagnetic resonance (EPR. The covalency character is about 0.74 and thus the compound is electrically less conductive. Optical absorption spectral studies suggest that Cu(II is placed in tetragonal elongation crystal field. The spin-orbit coupling constant, λ, is calculated using the EPR and optical absorption spectral results suggest some covalent bond between metal and ligand. Near infrared (NIR spectra are due to hydroxyl and water fundamentals.

  2. {mu}-XRF/{mu}-RS vs. SR {mu}-XRD for pigment identification in illuminated manuscripts

    Energy Technology Data Exchange (ETDEWEB)

    Snickt, G. van der; Nolf, W. de; Vekemans, B.; Janssens, K. [University of Antwerp, Department of Chemistry, Antwerp (Belgium)

    2008-07-15

    For the non-destructive identification of pigments and colorants in works of art, in archaeological and in forensic materials, a wide range of analytical techniques can be used. Bearing in mind that every method holds particular limitations, two complementary spectroscopic techniques, namely confocal {mu}-Raman spectroscopy ({mu}-RS) and {mu}-X-ray fluorescence spectroscopy ({mu}-XRF), were joined in one instrument. The combined {mu}-XRF and {mu}-RS device, called PRAXIS unites both complementary techniques in one mobile setup, which allows {mu}- and in situ analysis. {mu}-XRF allows one to collect elemental and spatially-resolved information in a non-destructive way on major and minor constituents of a variety of materials. However, the main disadvantages of {mu}-XRF are the penetration depth of the X-rays and the fact that only elements and not specific molecular combinations of elements can be detected. As a result {mu}-XRF is often not specific enough to identify the pigments within complex mixtures. Confocal Raman microscopy ({mu}-RS) can offer a surplus as molecular information can be obtained from single pigment grains. However, in some cases the presence of a strong fluorescence background limits the applicability. In this paper, the concrete analytical possibilities of the combined PRAXIS device are evaluated by comparing the results on an illuminated sheet of parchment with the analytical information supplied by synchrotron radiation {mu}-X-ray diffraction (SR {mu}-XRD), a highly specific technique. (orig.)

  3. Mössbauer, XRD, and Complex Thermal Analysis of the Hydration of Cement with Fly Ash

    Directory of Open Access Journals (Sweden)

    Vili Lilkov

    2013-01-01

    Full Text Available Hydration of cement with and without fly ash is studied with Mössbauer spectroscopy, XRD, and thermal analysis. Iron in cement is present as Fe3+-ions and occupies two octahedral positions, with close isomer shifts and quadrupole splittings. Iron in fly ash is present as Fe2+ and Fe3+, and the Mössbauer spectra display three doublets—two for Fe3+ in octahedral coordination and one for Fe2+. A third doublet was registered in the hydrating plain cement pastes after the 5th day, due to Fe3+ in tetrahedral coordination in the structure of the newly formed monosulphate aluminate. In cement pastes with fly ash, the doublet of tetrahedral iron is formed earlier because the quantity of ettringite and portlandite is low and more monosulphate crystallizes. No Fe(OH3 phase forms during hydration of C4AF. The fly ash displays pozzolanic properties, which lead to lowering of the portlandite quantity in the cement mixtures and increasing of the high temperature products.

  4. Size distribution of magnetic iron oxide nanoparticles using Warren-Averbach XRD analysis

    Science.gov (United States)

    Mahadevan, S.; Behera, S. P.; Gnanaprakash, G.; Jayakumar, T.; Philip, J.; Rao, B. P. C.

    2012-07-01

    We use the Fourier transform based Warren-Averbach (WA) analysis to separate the contributions of X-ray diffraction (XRD) profile broadening due to crystallite size and microstrain for magnetic iron oxide nanoparticles. The profile shape of the column length distribution, obtained from WA analysis, is used to analyze the shape of the magnetic iron oxide nanoparticles. From the column length distribution, the crystallite size and its distribution are estimated for these nanoparticles which are compared with size distribution obtained from dynamic light scattering measurements. The crystallite size and size distribution of crystallites obtained from WA analysis are explained based on the experimental parameters employed in preparation of these magnetic iron oxide nanoparticles. The variation of volume weighted diameter (Dv, from WA analysis) with saturation magnetization (Ms) fits well to a core shell model wherein it is known that Ms=Mbulk(1-6g/Dv) with Mbulk as bulk magnetization of iron oxide and g as magnetic shell disorder thickness.

  5. XRD, TEM, IR, Raman and NMR Spectroscopy of In Situ Crystallization of Lithium Disilicate Glass

    Science.gov (United States)

    Fuss, T.; Mogus-Milankovic, A.; Ray, C. S.; Lesher, C. E.; Youngman, R.; Day, D. E.

    2006-01-01

    The structure of a Li2O-2SiO2 (LS2) glass was investigated as a function of pressure and temperature up to 6 GPa and 750 C respectively, using XRD, TEM, IR, Raman and NMR spectroscopy. Glass densified at 6 GPa has an average Si-O-Si bond angle approx.7deg lower than that found in glass processed at 4.5 GPa. At 4.5 GPa, lithium disilicate crystallizes from the glass, while at 6 GPa a new high pressure form of lithium metasilicate crystallizes. The new phase, while having lithium metasilicate crystal symmetry, contains at least 4 different Si sites. NMR results for 6 GPa sample indicate the presence of Q4 species with (Q(sup 4))Si-O-Si(Q(sup 4)) bond angles of approx.157deg. This is the first reported occurrence of Q(sup 4) species with such large bond angles in alumina free alkali silicate glass. No five- or six- coordinated Si are found.

  6. Different β-alanine dimeric forms in trifluoromethanesulfonic acid salts. XRD and vibrational studies.

    Science.gov (United States)

    Wołoszyn, Łukasz; Ilczyszyn, Maria M

    2018-03-15

    Two new crystalline salts: β-alaninium trifluoromethanesulfonate (β-AlaOTf) and bis(β-alanine) trifluoromethanesulfonate (β-2AlaOTf) were obtained. The former one contains diprotonated β-alanine dimer, the latter one monoprotonated β-alanine dimer. Both compounds were studied by single crystal XRD, vibrational (IR and Raman) spectroscopy and calorimetric method. The quantum-mechanical calculations (DFT/B3LYP/6-311++G(2d,2p)) for the diprotonated dimer were carried out. The β-AlaOTf salt crystallizes in the P1¯ space group of triclinic system (Z=2), the β-2AlaOTf in the P2 1 /m space group of monoclinic system (Z=2). The vibrational data for the studied compounds are discussed in relation to their crystal structure, and provide insight into the character of hydrogen bonds and β-alanine protonation. The studied crystals do not exhibit phase transitions in the solid state. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Synchrotron Radiation XRD Analysis of Indialite in Y-82094 Ungrouped Carbonaceous Chondrite

    Science.gov (United States)

    Mikouchi, T.; Hagiya, K.; Sawa, N.; Kimura, M.; Ohsumi, K.; Komatsu, M.; Zolensky, M.

    2016-01-01

    Y-82094 is an ungrouped type 3.2 carbonaceous chondrite, with abundant chondrules making 78 vol.% of the rock. Among these chondrules, an unusual porphyritic Al-rich magnesian chondrule is reported that consists of a cordierite-like phase, Al-rich orthopyroxene, cristobalite, and spinel surrounded by an anorthitic mesostasis. The reported chemical formula of the cordierite-like phase is Na(0.19)Mg(1.95)Fe(0.02)Al(3.66)Si(5.19)O18, which is close to stoichiometric cordierite (Mg2Al3[AlSi5O18]). Although cordierite can be present in Al-rich chondrules, it has a high temperature polymorph (indialite) and it is therefore necessary to determine whether it is cordierite or indialite in order to better constrain its formation conditions. In this abstract we report on our synchrotron radiation X-ray diffraction (SR-XRD) study of the cordierite-like phase in Y-82094.

  8. In situ synchrotron XRD analysis of the kinetics of spodumene phase transitions.

    Science.gov (United States)

    L Moore, Radhika; Mann, Jason P; Montoya, Alejandro; Haynes, Brian S

    2018-04-25

    The phase transition by thermal activation of natural α-spodumene was followed by in situ synchrotron XRD in the temperature range 896 to 940 °C. We observed both β- and γ-spodumene as primary products in approximately equal proportions. The rate of the α-spodumene inversion is first order and highly sensitive to temperature (apparent activation energy ∼800 kJ mol-1). The γ-spodumene product is itself metastable, forming β-spodumene, with the total product mass fraction ratio fγ/fβ decreasing as the conversion of α-spodumene continues. We found the relationship between the product yields and the degree of conversion of α-spodumene to be the same at all temperatures in the range studied. A model incorporating first order kinetics of the α- and γ-phase inversions with invariant rate constant ratio describes the results accurately. Theoretical phonon analysis of the three phases indicates that the γ phase contains crystallographic instabilities, whilst the α and β phases do not.

  9. A 4-(o-chlorophenyl)-2-aminothiazole: Microwave assisted synthesis, spectral, thermal, XRD and biological studies

    Science.gov (United States)

    Rajmane, S. V.; Ubale, V. P.; Lawand, A. S.; Nalawade, A. M.; Karale, N. N.; More, P. G.

    2013-11-01

    A 4-(o-chlorophenyl)-2-aminothiazole (CPAT) has been synthesized by reacting o-chloroacetophenone, iodine and thiourea under microwave irradiation as a green chemistry approach. The reactions proceed selectively and within a couple of minutes giving high yields of the products. The compound was characterized by elemental, spectral (UV-visible, IR, NMR and GC-MS), XRD and thermal analyses. The TG curve of the compound was analyzed to calculate various kinetic parameters (n, E, Z, ΔS and ΔG) by using Coats-Redfern (C.R.), MacCallum-Tanner (M.T.) and Horowitz-Metzger (H.M.) method. The compound was tested for the evaluation of antibacterial activity against B. subtilis and E. coli and antifungal activity against A. niger and C. albicans. The compound was evaluated for their in vitro nematicidal activity on plant parasitic nematode Meloidogyne javanica and molluscicidal activity on fresh water helminthiasis vector snail Lymnea auricularia. The compound is biologically active in very low concentration. X-ray diffraction study suggests a triclinic crystal system for the compound.

  10. Application of XRF and XRD in the study of ceramics and pottery

    International Nuclear Information System (INIS)

    Meor Yusoff Meor Sulaiman

    2004-01-01

    Ceramic artefacts are made from clay-based mineral and their elemental and mineral compositions tend to vary from one locality to another. The elemental and mineral composition data's besides able to verify the originality of the artifact also helps in regard to provenance, fabrication technology and also manufacturing technique. X-ray fluorescence XRF is a non-destructive technique to identify and quantify elements ranging from sodium (atomic number = 11 to uranium atomic number = 92). The paper also looks into recent advances of this technique in the study of ceramics and pottery. Microfocus XRF, besides able to do qualitative and quantitative elemental analysis, it also can perform accurate elemental mapping. Another aspect there is important in this study is the capability to do in-situ analysis. With the recent introduction of the peltiered-cooled silicon detector, in-situ analysis had become more easily available. X-ray diffraction (XRD) analysis on the other hand, helps to identify correctly the different mineral composition present in the ceramic artifact. This could also help in identifying the type of clay that is used in the manufacturing of these ceramic artifacts as well as its origin. Both x-ray techniques complement each other and are very important tool in the archaeological study of ceramic and pottery samples. (Author)

  11. EXAFS and XRD studies of nanocrystalline cerium oxide: the effect of preparation method on the microstructure

    International Nuclear Information System (INIS)

    Savin, S.L.P.; Chadwick, A.V.; Smith, M.E.; O'Dell, L.A.

    2007-01-01

    There is considerable interest in nanocrystalline materials due to their unusual properties, such as enhanced ionic conductivity in the case of nanocrystalline ionic solids. This has potential commercial applications, particularly for oxide ion conductors. However, a detailed knowledge of the microstructure is important in fully understanding the novel properties exhibited by nanocrystalline materials. The final microstructure of a material is dependent on the preparation method used, for example, sol-gel and ball-milling methods are commonly used in the preparation of nanocrystalline oxides. Additionally, there is a problem in maintaining the materials in nanocrystalline form when they are subjected to elevated temperatures. We have been exploring strategies to restrict the growth of nanocrystalline oxides and have found that adding a small amount of an inert material, e.g. SiO 2 or Al 2 O 3 , is particularly effective. We will report XRD and EXAFS studies of nanocrystalline ceria prepared by sol-gel, sol-gel pinned and ball-milling methods and the effect of preparation method on the final microstructure. (copyright 2007 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  12. Multielemental analyses of isomorphous Indian garnet gemstones by XRD and external pixe techniques.

    Science.gov (United States)

    Venkateswarulu, P; Srinivasa Rao, K; Kasipathi, C; Ramakrishna, Y

    2012-12-01

    Garnet gemstones were collected from parts of Eastern Ghats geological formations of Andhra Pradesh, India and their gemological studies were carried out. Their study of chemistry is not possible as they represent mixtures of isomorphism nature, and none of the individual specimens indicate independent chemistry. Hence, non-destructive instrumental methodology of external PIXE technique was employed to understand their chemistry and identity. A 3 MeV proton beam was employed to excite the samples. In the present study geochemical characteristics of garnet gemstones were studied by proton induced X-ray emission. Almandine variety of garnet is found to be abundant in the present study by means of their chemical contents. The crystal structure and the lattice parameters were estimated using X-Ray Diffraction studies. The trace and minor elements are estimated using PIXE technique and major compositional elements are confirmed by XRD studies. The technique is found very useful in characterizing the garnet gemstones. The present work, thus establishes usefulness and versatility of the PIXE technique with external beam for research in Geo-scientific methodology. Copyright © 2012 Elsevier Ltd. All rights reserved.

  13. Characterization of Serpentine Samples from the Coast Range Ophiolite Microbial Observatory with μ-FTIR and XRD. ­­

    Science.gov (United States)

    Sousa, A.; Cardace, D.

    2017-12-01

    Serpentinizing systems hold much promise as potentially habitable environments in diverse planetary settings. They involve abundant and simple ingredients (i.e., the mineral olivine, liquid water), support subsurface microbial communities on Earth (Crespo-Medina et al. 2014; Suzuki et al. 2014; Kelley et al. 2005) and are thought to occur elsewhere in our solar system such as Mars (Schulte et al. 2006; Ehlmann et al. 2010)and possibly ocean worlds (Waite et al. 2017; Vance 2009). Although geochemical and microbial data collection continues in serpentinizing systems, the identification and resolution of potential biosignatures in serpentinites are not yet clear. Specifically, the micro-scale mineralogical contexts in which cell fragments or biofilm residues may be formed and preserved is lacking. Here we report preliminary transmission and reflection mode μ-FTIR spectral maps and XRD diffractograms, obtained with instruments relevant to robotic exploration missions (Blake et al. 2012; Igisu et al. 2009; Leroi et al. 2009). Samples analyzed include ultramafic rock and constituent mineral standards (e.g., olivine) and rocks collected from near surface sites associated with the NASA Astrobiology Institute-funded initiative, the Coast Range Ophiolite Microbial Observatory (CROMO), in Lower Lake, CA (Cardace et al. 2013). These new results provide co-registered, complementary data on astrobiologically important rock and mineral phases related to serpentinization (Crespo-Medina et al. 2014; Twing et al. 2017). Future work will leverage this data set in microbial colonization experiments aimed at parsing background organic loads in serpentinites from surficial/fracture-localized modern biofilm signatures.

  14. Novel XRD technique and equipment for in-situ monitoring of phase transformations in lithium batteries during cycling

    International Nuclear Information System (INIS)

    Nikolov, J.; Howlett, P.

    2002-01-01

    Full text: Safe, rechargeable batteries utilising a lithium metal electrode have not been realised due to phenomena, which occur on the lithium surface during the cycling of a battery. Lithium ion conduction inhomogeneities through the surface film give rise to uneven deposition of lithium, which can result in short circuits. The large potential increase in energy density that the use of the lithium electrode represents makes the nature of the surface film of interest to battery researchers. The lithium surface is highly reactive, particularly in the case of electrodes with a rough surface deposit. This presents difficulties to researchers hoping to obtain representative measurements of the lithium surface and requires the use of environmental sample chambers and in-situ techniques. X-ray diffraction techniques have been used to probe changes in cathode materials (typically transition metal oxides) for lithium batteries, but to our knowledge has not been successfully used to study changes taking place on the lithium surface during cycling. We present early results from work we have undertaken to develop a technique for characterising the surface film on lithium battery electrodes. The instrumentation was set-up as follows. An XRD was fitted with an INEL CPS 120 position sensitive detector (PSD), multilayer mirror and environmental chamber. The latter was specially developed in our laboratory for the purpose of these experiments. The lithium cells were sealed in laminated foil. Cycled and uncycled cells were investigated. Different radiation sources were used (Cu, Co and Cr). The in-situ measurements aiming at monitoring the phase transitions of cycled/uncycled cells at different angles (including grazing angles) in time were carried out in both transmission and reflection mode. Copyright (2002) Australian X-ray Analytical Association Inc

  15. [Study of the phase transformation of TiO2 with in-situ XRD in different gas].

    Science.gov (United States)

    Ma, Li-Jing; Guo, Lie-Jin

    2011-04-01

    TiO2 sample was prepared by sol-gel method from chloride titanium. The phase transformation of the prepared TiO2 sample was studied by in-situ XRD and normal XRD in different gas. The experimental results showed that the phase transformation temperatures of TiO2 were different under in-situ or normal XRD in different kinds of gas. The transformation of amorphous TiO2 to anatase was controlled by kinetics before 500 degrees C. In-situ XRD showed that the growth of anatase was inhibited, but the transformation of anatase to rutile was accelerated under inactive nitrogen in contrast to air. Also better crystal was obtained under hydrogen than in argon. These all showed that external oxygen might accelerate the growth of TiO2, but reduced gas might partly counteract the negative influence of lack of external oxygen. The mechanism of phase transformation of TiO2 was studied by in-situ XRD in order to control the structure in situ.

  16. Transmission X-ray Diffraction (XRD) Patterns Relevant to the MSL Chemin Amorphous Component: Sulfates And Silicates

    Science.gov (United States)

    Morris, R. V.; Rampe, E. B.; Graff, T. G.; Archer, P. D., Jr.; Le, L.; Ming, D. W.; Sutter, B.

    2015-01-01

    The Mars Science Laboratory (MSL) CheMin instrument on the Curiosity rover is a transmission X-ray diffractometer (Co-Kalpha radiation source and a approx.5deg to approx.52deg 2theta range) where the analyzed powder samples are constrained to have discrete particle diameters XRD amorphous component. Estimates of amorphous component abundance, based on the XRD data itself and on mass-balance calculations using APXS data crystalline component chemistry derived from XRD data, martian meteorites, and/or stoichiometry [e.g., 6-9], range from approx.20 wt.% to approx.50 wt.% of bulk sample. The APXSbased calculations show that the amorphous component is rich in volatile elements (esp. SO3) and is not simply primary basaltic glass, which was used as a surrogate to model the broad band in the RN CheMin pattern. For RN, the entire volatile inventory (except minor anhydrite) is assigned to the amorphous component because no volatile-bearing crystalline phases were reported within detection limits [2]. For JK and CB, Fesaponite, basanite, and akaganeite are volatile-bearing crystalline components. Here we report transmission XRD patterns for sulfate and silicate phases relevant to interpretation of MSL-CheMin XRD amorphous components.

  17. Correlation of index tests with smectite content determined with XRD in bentonite and smectite rich clays

    International Nuclear Information System (INIS)

    Kumpulainen, Sirpa; Kiviranta, Leena; Korkeakoski, Petri

    2012-01-01

    Document available in extended abstract form only. Various index tests are used by bentonite producers and users to assess the amount of swelling minerals in bentonites and smectite rich clays. Index tests are meant to provide relative fast and inexpensive way of testing the amount of swelling minerals, and their performance should not require sophisticated equipment. Such index tests are e.g. methylene blue absorption test, liquid limit and swelling index test (free swelling). In order to select appropriate index test to control the quality of buffer and backfill materials to be used in nuclear waste end disposal in Finland, results from various index tests were correlated with the smectite content determined with XRD and Rietveld refinement. Tests evaluated were: water absorption capacity (WAC) based on DIN 18132, swelling index (SI) based on ASTM D 5890-06, cation exchange capacity (CEC) based on Cu(II)-trien adsorption by Meier and Kahr (1999) and Ammann et al. (2005), liquid limit (LL) based on CEN ISO/TS 17892- 12:2004, methylene blue absorption (MB) based on SFS-EN 933-9, and specific surface area based on absorption of ethylene glycol monoethyl ether (EGME) described by Cerato and Lutenegger (2002). The number of samples tested was 6-25 (exact number of samples was dependent on the test method), and included natural Na-bentonites, natural Ca-bentonites, sodium activated Ca-bentonites and smectite rich clays from Wyoming/USA, Milos/Greece, Gujarat/India and Friedland/Germany. Smectite content in samples was determined after Kiviranta and Kumpulainen (2011) by x-ray diffraction (XRD), optical microscopy, chemical analyses, and full-pattern fitting with the Rietveld method using Siroquant software. Exchangeable cation composition was determined after Belyayeva (1967) and Jackson (1975). In order to achieve correlation of index test results with smectite content, water absorption capacity, liquid limit, and swelling index methods required additional information

  18. Potato Starch/Montmorillonite-Based Nanocomposites: Water Sensitivity, Mechanical and Thermal Properties and XRD Profile Study

    Directory of Open Access Journals (Sweden)

    Ronak Gholami

    2013-06-01

    Full Text Available Studies were carried out on the effect of adding different percentages of montmorillonite (3, 5, 7 and 9% of starch weight on the physical properties of potato starch-MMT nanocomposites. Heat resistance and mechanical properties of films were measured by differential scanning calorimetry (DSC and tensile test. Nanoparticles distribution in polymer matrix was investigated using X-ray diffraction test (XRD. For investigation of water vapor resistance of film samples, moisture sorption and water vapor permeability (WVP were measured. The results showed that the distribution of nanoparticles in the polymer matrix was exfoliated. WVP in pure starch films was 2.62×10-7 g/mhPa and with the addition of 9% MMT it was reduced to 1.43×10-7 g/mhPa. With the addition of nanoclay from zero to 9%, the ultimate tensile strength of nanocomposite samples was increased from 5.9 to 6.63 MPa and strain-to-break was decreased from 34.82 to 26.83%. But the rising trend was not significant for nanocomposite samples containing low concentrations of nanoclay (0-7%. The main reasons for the enhancement of mechanical properties due to the addition of nanoclay were to establish hydrogen bonding between polymer chains and clay layers, filling the empty spaces and increase the crystalline domains. Investigation of thermal resistance of nanocomposite samples showed that they have higher thermal resistance and melting point in comparison with pure starch films. With the addition of nanoclay from zero to 9%, the melting point of film samples was increased from 218 to 232.1°C. With the addition of nanoclay, probably the mobility of amylopectin chains decreased and crystalline domains increased. Also, with increasing nanoclay content, the glass transition temperature of nanocomposite samples was increased. This result corresponded to shrinkage in free volume and thus reduction in the polymer chains mobility in amorphous regions.

  19. Studying the melting behavior of coal, biomass, and coal/biomass ash using viscosity and heated stage XRD data

    DEFF Research Database (Denmark)

    Arvelakis, Stelios; Folkedahl, B.; Dam-Johansen, Kim

    2006-01-01

    by the cocombustion tests appeared to be somewhat different compared to that of the laboratory-prepared ash samples. The heated stage XRD data provide useful information regarding the reactions among the various ash compounds and the phase transformations during the heating and cooling of the ash samples and helped...... a high-temperature rotational viscometer and a hot stage XRD. The produced data were used to calculate the operating temperature of a pilot-scale entrained flow reactor during the cocombustion of biomass/ coal samples in order to ensure the slag flow and to avoid corrosion of the walls due to liquid slag...

  20. The identification of carbide phases by XRD analysis as the method of assess the extent of the steel damage after long time in service

    Directory of Open Access Journals (Sweden)

    I. Pietryka

    2010-07-01

    Full Text Available After long time in service in contact in a superheated steam mechanical properties of materials decrease. Experiments revealed that the XRD analysis of electrocemically separated carbide phase is a rapid and informative method of evaluation the service condition of steel. Mechanical properties of ferritic and bainitic low-alloy steels are caused by many factors like: chemical composition, quantity and the kind of microstructural constituent, the precipitation hardening, substructure of matrix and index of matrix lattice defects. In this paper the results of investigations 13CrMo4-5 steel was shown. The material for research was taken from thermal power plant elements. Material A was after 150.000 hours of work as the pressure chamber in which was the temperature 530-580oC and the pressure was 12 MPa. Material B was after 250000 hours of work as the pipeline of superheated steam. The temperature in this case was 530oC but the pressure was 12 MPa as well. The mechanical properties after long time service and changes in fine structure were tested. Parameters of carbide phase electrochemical separation in electrolytes solutions are presented in this work.The most relevant electrolyte and the far better conditions of extraction process were chosen taking into consideration the time needed to get considerable amount of carbide phase constituents. The identification of carbide phases was the special goal of this work. Identification of electrochemically separated carbide phases by means of the XRD analysis was used.

  1. Studying the melting behaviour of fly ash from the incineration of MSW using viscosity and heated stage XRD data

    DEFF Research Database (Denmark)

    Arvelakis, Stelios; Folkedahl, B.; Frandsen, F. J.

    2008-01-01

    , by use of a high-temperature rotational viscometer in order to determine the rheology of the ash material, and by a hot-stage XRD in order to identify phase changes and transformations during the heating and cooling of the ash samples. Knowledge of the ash melting properties as well as phase changes...

  2. XRF, XRD and SEM facilities in the School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia

    International Nuclear Information System (INIS)

    Azmi Rahmat

    1996-01-01

    The School has acquired excellent facilities for elemental analysis by XRF and EDX and phase analysis by XRD. The type of research work carried out in the School is described. The school also assists the local industries in trying to solve their problems fully utilizing these facilities along with other testing units

  3. Phase evaluation of YSZ upon doping with Ta"5"+, Ti"4"+ and Ca"2"+ with combined Raman and XRD analysis

    International Nuclear Information System (INIS)

    Bhattacharya, A.; Shklover, V.; Wermelinger, T.

    2012-01-01

    To improve the phase stability of 7YSZ (7 wt%-Y_2O_3-doped ZrO_2), it has been doped with larger (Ca"2"+) and smaller (Ti"4"+ or Ta"5"+) ions. Complementary Raman and XRD studies of these stabilized systems have been performed. The tetragonal symmetry of the Ta"5"+-ion-doped YSZ sample and the Ti"4"+-doped YSZ sample, and the cubic symmetry of Ca"2"+-doped YSZ have been confirmed both by means of XRD and Raman analyses. Raman scattering measurements show shifts of characteristic peaks when the YSZ is doped with Ta"5"+, Ti"4"+ and Ca"2"+ cations. The peak shift increased with increasing dopant concentration in the ZrO_2 lattice. The Ta-doped YSZ sample heat-treated below 1500 C contained some YTaO_4 phase, which was confirmed by means of XRD as well as by Raman spectroscopy. The effect of Ca"2"+ ion doping on the Raman peak shift was much higher than that of Y"3"+ ion doping. In this work it has been highlighted that Raman spectroscopy is a useful tool complementing XRD, for qualitative comparison of the doping effect on the lattice parameters of ZrO_2.

  4. XRD Investigation of the relaxation of InAsP layers grown by CBE on (100) InP

    NARCIS (Netherlands)

    Marschner, T.H.; Leijs, M.R.; Vonk, H.; Wolter, J.H.

    1998-01-01

    We present X-ray diffraction (XRD) investigations of the influence of the substrate off-orientation on the relaxation of InAsP layers grown on InP by chemical beam epitaxy (CBE). Our measurements show that with beginning relaxation the As-concentration increases drastically and stays constant if the

  5. XRD Analysis of Nanocrystalline Anatase Powders Prepared by Various Chemical Routes: Correlations between Micro-structure and Crystal Structure Parameters

    Czech Academy of Sciences Publication Activity Database

    Matěj, Z.; Matějová, Lenka; Kužel, R.

    2013-01-01

    Roč. 28, Suppl. 2 (2013), s. 161-183 ISSN 0885-7156 Grant - others:UK(CZ) UNCE 204023/2012; MŠk(CZ) GAP108/11/1539 Institutional support: RVO:67985858 Keywords : anatase * crystallite size * lattice parameters * XRD * vacancies * anisotropy Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.586, year: 2013

  6. Study of the thermal transformations of Co- and Fe-exchanged zeolites A and X by 'in situ' XRD under reducing atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Ronchetti, Silvia, E-mail: silvia.ronchetti@polito.it [Dipartimento di Scienza dei Materiali e Ingegneria Chimica, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy); Turcato, Elisa Aurelia; Delmastro, Alessandro [Dipartimento di Scienza dei Materiali e Ingegneria Chimica, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy); Esposito, Serena; Ferone, Claudio; Pansini, Michele [Laboratorio Materiali del Dipartimento di Meccanica, Strutture, Ambiente e Territorio, Facolta di Ingegneria dell' Universita di Cassino, Via G. Di Biasio 43, 03043 Cassino (Italy); Onida, Barbara; Mazza, Daniele [Dipartimento di Scienza dei Materiali e Ingegneria Chimica, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy)

    2010-06-15

    'In situ' high temperature X-ray diffraction under reducing atmosphere is used for the first time to study the thermal stability and transformations of Co- and Fe-exchanged A and X zeolites. TG-DTA and 'ex situ' XRD characterization were also carried out. The temperature of incipient crystallization of metallic phase was found to be 700 {sup o}C in Fe-zeolites and 800 {sup o}C in Co-zeolites. Moreover, ex situ X-ray experiments, after thermal treatment both under inert and reducing atmosphere, revealed the formation of ceramic phases upon the thermal collapse of the zeolitic framework. Metal nanoparticles were obtained by reduction and the size of metal clusters was found to range between 24 and 40 nm.

  7. Some critical aspects of FT-IR, TGA, powder XRD, EDAX and SEM studies of calcium oxalate urinary calculi.

    Science.gov (United States)

    Joshi, Vimal S; Vasant, Sonal R; Bhatt, J G; Joshi, Mihir J

    2014-06-01

    Urinary calculi constitute one of the oldest afflictions of humans as well as animals, which are occurring globally. The calculi vary in shape, size and composition, which influence their clinical course. They are usually of the mixed-type with varying percentages of the ingredients. In medical management of urinary calculi, either the nature of calculi is to be known or the exact composition of calculi is required. In the present study, two selected calculi were recovered after surgery from two different patients for detailed examination and investigated by using Fourier-Transform infrared spectroscopy (FT-IR), thermo-gravimetric analysis (TGA), powder X-ray diffraction (XRD), scanning electron microscopy and energy dispersive analysis of X-rays (EDAX) techniques. The study demonstrated that the nature of urinary calculi and presence of major phase in mixed calculi could be identified by FT-IR, TGA and powder XRD, however, the exact content of various elements could be found by EDAX only.

  8. In-situ XRD and EDS method study on the oxidation behaviour of Ni-Cu sulphide ore.

    Science.gov (United States)

    Li, Guangshi; Cheng, Hongwei; Xiong, Xiaolu; Lu, Xionggang; Xu, Cong; Lu, Changyuan; Zou, Xingli; Xu, Qian

    2017-06-12

    The oxidation mechanism of sulfides is the key issue during the sulphide-metallurgy process. In this study, the phase transformation and element migration were clearly demonstrated by in-situ laboratory-based X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS), respectively. The reaction sequence and a four-step oxidation mechanism were proposed and identified. The elemental distribution demonstrated that at a low temperature, the Fe atoms diffused outward and the Ni/Cu atoms migrated toward the inner core, whereas the opposite diffusion processes were observed at a higher temperature. Importantly, the unique visual presentation of the oxidation behaviour provided by the combination of in-situ XRD and EDS might be useful for optimising the process parameters to improve the Ni/Cu extraction efficiency during Ni-Cu sulphide metallurgy.

  9. X-Ray Diffraction (XRD) Characterization Methods for Sigma=3 Twin Defects in Cubic Semiconductor (100) Wafers

    Science.gov (United States)

    Park, Yeonjoon (Inventor); Kim, Hyun Jung (Inventor); Skuza, Jonathan R. (Inventor); Lee, Kunik (Inventor); King, Glen C. (Inventor); Choi, Sang Hyouk (Inventor)

    2017-01-01

    An X-ray defraction (XRD) characterization method for sigma=3 twin defects in cubic semiconductor (100) wafers includes a concentration measurement method and a wafer mapping method for any cubic tetrahedral semiconductor wafers including GaAs (100) wafers and Si (100) wafers. The methods use the cubic semiconductor's (004) pole figure in order to detect sigma=3/{111} twin defects. The XRD methods are applicable to any (100) wafers of tetrahedral cubic semiconductors in the diamond structure (Si, Ge, C) and cubic zinc-blend structure (InP, InGaAs, CdTe, ZnSe, and so on) with various growth methods such as Liquid Encapsulated Czochralski (LEC) growth, Molecular Beam Epitaxy (MBE), Organometallic Vapor Phase Epitaxy (OMVPE), Czochralski growth and Metal Organic Chemical Vapor Deposition (MOCVD) growth.

  10. Leonardo da Vinci's drapery studies: characterization of lead white pigments by µ-XRD and 2D scanning XRF

    Science.gov (United States)

    Gonzalez, Victor; Calligaro, Thomas; Pichon, Laurent; Wallez, Gilles; Mottin, Bruno

    2015-11-01

    This work focuses on the composition and microstructure of the lead white pigment employed in a set of paintworks, using a combination of µ-XRD and 2D scanning XRF, directly applied on five drapery studies attributed to Leonardo da Vinci (1452-1519) and conserved in the Département des Arts Graphiques, Musée du Louvre and in the Musée des Beaux- Arts de Rennes. Trace elements present in the composition as well as in the lead white highlights were imaged by 2D scanning XRF. Mineral phases were determined in a fully noninvasive way using a special µ-XRD diffractometer. Phase proportions were estimated by Rietveld refinement. The analytical results obtained will contribute to differentiate lead white qualities and to highlight the artist's technique.

  11. Characterization of ash pond ashes from 3rd thermal power plant by SEM/EDX and XRD methods

    OpenAIRE

    A Minjigmaa; Ts Zolzaya; E Bayanjargal; B Davaabal; J Temuujin

    2014-01-01

      Coal combustion by products from ash pond of 3rdthermal power plant of Ulaanbaatar city have been collected in 2010 and 2013 years. The ash samples have been characterized by XRD, XRF and SEM-EDX methods in order to evaluate their chemical and mineralogical composition changes with disposed times. The mineralogical composition of ash varies with time though the chemical composition of the ashes were close each other. Possibly, inefficient operating condition of the TPS shows influence on th...

  12. AFM and XRD characterization of silver nanoparticles films deposited on the surface of DGEBA epoxy resin by ion sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Andrade, Jose Elisandro de; Machado, Rogerio; Macedo, Marcelo Andrade; Cunha, Frederico Guilherme Carvalho [Clinica de Medicina Nuclear e Radiologia de Maceio (MedRadiUS), Radiology and Imaging Diagnosis at Universidade Federal de Alagoas (UFAL), Maceio, AL (Brazil)

    2012-07-01

    In this work, silver atoms were deposited by ion sputtering on the surface of diglycidyl ether of bisphenol A (DGEBA) epoxy resin cured at 150 deg C for 6 hours in air. The films of DGEBA and its precursors were characterized by Raman spectroscopy to identify the main functional groups and their relationship with the deposited silver atoms. Silver thin films of 5, 10, 15 and 20 nm were deposited on the epoxy resin at room temperature. Both the initial film of DGEBA and the subsequent silver thin film were analyzed by Atomic Force Microscopy (AFM) in the non-contact mode. Silver thin films were also analyzed using X-ray diffraction (XRD) at room temperature. The AFM results showed the formation of silver crystallites on the surface of DGEBA at very low coverage whereas XRD indicated that most of them had their main axis aligned to the normal of the surface. An increase in the coverage led to an increase in the grain size as indicated by AFM. However, XRD results indicated that the crystallite size remained almost constant while the appearance of peaks corresponding to other crystalline orientations suggests the coalescence of the original crystallites and an increase in size of the more dense planes, namely [111]. (author)

  13. AFM and XRD characterization of silver nanoparticles films deposited on the surface of DGEBA epoxy resin by ion sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Andrade, Jose Elisandro de; Machado, Rogerio; Macedo, Marcelo Andrade [Universidade Federal de Sergipe (UFSE), Aracaju, SE (Brazil). Programa de Pos-graduacao em Fisica; Cunha, Frederico Guilherme Carvalho [Universidade Federal de Sergipe (UFSE), Aracaju, SE (Brazil). Programa de Pos-graduacao em Ciencia e Engenharia de Materiais

    2012-07-01

    In this work, silver atoms were deposited by ion sputtering on the surface of diglycidyl ether of bisphenol A (DGEBA) epoxy resin cured at 150 Degree-Sign C for 6 hours in air. The films of DGEBA and its precursors were characterized by Raman spectroscopy to identify the main functional groups and their relationship with the deposited silver atoms. Silver thin films of 5, 10, 15 and 20 nm were deposited on the epoxy resin at room temperature. Both the initial film of DGEBA and the subsequent silver thin film were analyzed by Atomic Force Microscopy (AFM) in the non-contact mode. Silver thin films were also analyzed using X-ray diffraction (XRD) at room temperature. The AFM results showed the formation of silver crystallites on the surface of DGEBA at very low coverage whereas XRD indicated that most of them had their main axis aligned to the normal of the surface. An increase in the coverage led to an increase in the grain size as indicated by AFM. However, XRD results indicated that the crystallite size remained almost constant while the appearance of peaks corresponding to other crystalline orientations suggests the coalescence of the original crystallites and an increase in size of the more dense planes, namely [111]. (author)

  14. [NIR and XRD analysis of drill-hole samples from Zhamuaobao iron-graphite deposit, Inner Mongolia].

    Science.gov (United States)

    Li, Ying-kui; Cao, Jian-jin; Wu, Zheng-quan; Dai, Dong-le; Lin, Zu-xu

    2015-01-01

    The author analyzed the 4202 drill-hole samples from Zhamuaobao iron-graphite deposit by using near infrared spectroscopy(NIR) and X-ray diffraction(XRD) measuring and testing techniques, and then compared and summarized the results of two kinds of testing technology. The results indicate that some difference of the mineral composition exists among different layers, the lithology from upper to deeper is the clay gravel layer of tertiary and quaternary, mudstone, mica quartz schist, quartz actinolite scarn, skarnization marble, iron ore deposits, graphite deposits and mica quartz schist. The petrogenesis in different depth also shows difference, which may indicate the geological characteristic to some extent. The samples had mainly undergone such processes as oxidization, carbonation, chloritization and skarn alteration. The research results can not only improve the geological feature of the mining area, but also have great importance in ore exploration, mining, mineral processing and so on. What's more, as XRD can provide preliminary information about the mineral composition, NIR can make further judgement on the existence of the minerals. The research integrated the advantages of both NIR and XRD measuring and testing techniques, put forward a method with two kinds of modern testing technology combined with each other, which may improve the accuracy of the mineral composition identification. In the meantime, the NIR will be more wildly used in geography on the basis of mineral spectroscopy.

  15. AFM and XRD characterization of silver nanoparticles films deposited on the surface of DGEBA epoxy resin by ion sputtering

    Directory of Open Access Journals (Sweden)

    José Elisandro de Andrade

    2013-01-01

    Full Text Available In this work, silver atoms were deposited by ion sputtering on the surface of diglycidyl ether of bisphenol A (DGEBA epoxy resin cured at 150 °C for 6 hours in air. The films of DGEBA and its precursors were characterized by Raman spectroscopy to identify the main functional groups and their relationship with the deposited silver atoms. Silver thin films of 5, 10, 15 and 20 nm were deposited on the epoxy resin at room temperature. Both the initial film of DGEBA and the subsequent silver thin film were analyzed by Atomic Force Microscopy (AFM in the non-contact mode. Silver thin films were also analyzed using X-ray diffraction (XRD at room temperature. The AFM results showed the formation of silver crystallites on the surface of DGEBA at very low coverage whereas XRD indicated that most of them had their main axis aligned to the normal of the surface. An increase in the coverage led to an increase in the grain size as indicated by AFM. However, XRD results indicated that the crystallite size remained almost constant while the appearance of peaks corresponding to other crystalline orientations suggests the coalescence of the original crystallites and an increase in size of the more dense planes, namely [111].

  16. Phosphorus Sorption Characteristics in Aluminum-based Water Treatment Residuals Reacted with Dairy Wastewater: 1. Isotherms, XRD, and SEM-EDS Analysis.

    Science.gov (United States)

    Zohar, Iris; Massey, Michael S; Ippolito, James A; Litaor, M Iggy

    2018-05-01

    We examined P sorption characteristics in Al-based water treatment residuals (Al-WTR) generated from slightly alkaline surface water and in an organic residual composite (WW-Al/O-WTR), produced by using the Al-WTR to treat organic-rich and high P concentration dairy wastewater. Solids from both residuals were examined using scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and X-ray diffraction (XRD), and exposed to P additions of 0 to 4000 mg L in a sorption experiment. The Al-WTR removed ∼97% of the added P, whereas WW-Al/O-WTR removed only 78% of the added P in the addition range of 0 to 100 mg P L. With P additions of ≥100 mg L, the removal rate declined to XRD indicated that the major mineral was calcite, with some silica and poorly crystalline Al hydroxides. Analysis by SEM-EDS, which used three-element overlay maps of the residual surfaces, indicated that P was sparsely sorbed on both calcic and Al (hydr)oxide surfaces, along with a few clusters, even at low P concentrations of the treated waters. Ternary clusters of P, Al, and Ca were more abundant on the WW-Al/O-WTR. Carbon distribution suggested that organic substances covered Al surfaces. Sorption of P onto WW-Al/O-WTR may be reversible due to relatively weak Ca-P and Al-P bonds induced by the slight alkaline nature and in the presence of organic moieties, enhancing the WW-Al/O-WTR potential to act as a P source, rather than a P sink, in agricultural applications. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  17. Characterizing the Phyllosilicates and Amorphous Phases Found by MSL Using Laboratory XRD and EGA Measurements of Natural and Synthetic Materials

    Science.gov (United States)

    Rampe, Elizabeth B.; Morris, Richard V.; Chipera, Steve; Bish, David L.; Bristow, Thomas; Archer, Paul Douglas; Blake, David; Achilles, Cherie; Ming, Douglas W.; Vaniman, David; hide

    2013-01-01

    The Curiosity Rover landed on the Peace Vallis alluvial fan in Gale crater on August 5, 2012. A primary mission science objective is to search for past habitable environments, and, in particular, to assess the role of past water. Identifying the minerals and mineraloids that result from aqueous alteration at Gale crater is essential for understanding past aqueous processes at the MSL landing site and hence for interpreting the site's potential habitability. X-ray diffraction (XRD) data from the CheMin instrument and evolved gas analyses (EGA) from the SAM instrument have helped the MSL science team identify phases that resulted from aqueous processes: phyllosilicates and amorphous phases were measure in two drill samples (John Klein and Cumberland) obtained from the Sheepbed Member, Yellowknife Bay Fm., which is believed to represent a fluvial-lacustrine environment. A third set of analyses was obtained from scoop samples from the Rocknest sand shadow. Chemical data from the APXS instrument have helped constrain the chemical compositions of these secondary phases and suggest that the phyllosilicate component is Mg-enriched and the amorphous component is Fe-enriched, relatively Si-poor, and S- and H-bearing. To refine the phyllosilicate and amorphous components in the samples measured by MSL, we measured XRD and EGA data for a variety of relevant natural terrestrial phyllosilicates and synthetic mineraloids in laboratory testbeds of the CheMin and SAM instruments. Specifically, Mg-saturated smectites and vermiculites were measured with XRD at low relative humidity to understand the behavior of the 001 reflections under Mars-like conditions. Our laboratory XRD measurements suggest that interlayer cation composition affects the hydration state of swelling clays at low RH and, thus, the 001 peak positions. XRD patterns of synthetic amorphous materials, including allophane, ferrihydrite, and hisingerite were used in full-pattern fitting (FULLPAT) models to help

  18. CCD-Based XRD/XRF for Determining Environmental Mineralogy on Mars

    Science.gov (United States)

    Vaniman, D. T.; Bish, D. L.; Blake, D. F.; Chipera, S. J.

    2000-01-01

    Health effects from Martian dusts will be a concern for any manned Mars missions. Nuisance dusts plagued the Apollo astronauts, but dusts of more hazardous mineralogy, in habitats occupied by Mars astronauts weakened by a long-duration mission, may be more than a nuisance. Chemical hazards in Martian regolith attributable to S, Cl, Br, Cd, and Pb are known or strongly suspected to be present, but terrestrial studies of the health effects of dusts indicate that accurate determination of mineralogy is a critical factor in evaluating inhalation hazards. Mineral inhalation hazards such as the Group-I carcinogenic zeolite erionite, which is demonstrated to cause mesothelioma, cannot be identified by chemical analysis alone. Studies of palagonite analogs raise the possibility that erionite may occur on Mars. In addition to health effects concerns, environmental mineralogy has significant importance in resource extraction, groundwater use, and sustained agriculture. The high sulfur and chlorine content of Martian regolith will affect all of these uses, but the nature of mineralogic reservoirs for S and Cl will determine their uptake and concentration in extracted groundwater and in agricultural applications of regolith. Wet chemistry experiments planned for the Mars Environmental Compatibility Assessment (MECA) will define some of the consequences of water/soil interaction, but an understanding of the mineralogic basis for water-rock reactions is needed to understand the mechanisms of reaction and to apply the results of a few experiments to larger scales and different conditions.

  19. Characterisation of annealed Fe/Ag bilayers by RBS and XRD

    Energy Technology Data Exchange (ETDEWEB)

    Tunyogi, A., E-mail: tunyogi@rmki.kfki.h [KFKI Research Institute for Particle and Nuclear Physics, H-1525 Budapest, P.O. Box 49 (Hungary); Tancziko, F.; Bogdan, Cs. [KFKI Research Institute for Particle and Nuclear Physics, H-1525 Budapest, P.O. Box 49 (Hungary); Horvath, Z.E. [Research Institute for Technical Physics and Materials Science, H-1525 Budapest, P.O. Box 49 (Hungary); Szilagyi, E. [KFKI Research Institute for Particle and Nuclear Physics, H-1525 Budapest, P.O. Box 49 (Hungary)

    2010-06-15

    Recently Fe/Ag thin films have been intensively investigated due to their special magnetic properties. To study the stability of the Fe-Ag interfaces very long time experiments are necessary at room temperature. To enhance the processes which take place at interfaces, high temperature annealing can be used. A detailed annealing experiment was carried out on Si-covered Fe/Ag (Ag grown on Fe) and Ag/Fe (Fe grown on Ag) polycrystalline bilayers, which were deposited on Si(1 1 1) substrates by MBE method. Heat treatments of various duration and temperature were applied in UHV conditions. Rutherford backscattering spectrometry and X-ray diffractometry were used to determine the effects of the heat treatments. In case of Fe/Ag samples, formation of iron-silicide phases was observed between the Fe layer and Si substrate, and the silver and the silicon capping layer were also completely mixed with each other. In case of the Ag/Fe samples the silver moved to the sample surface through the iron layers, while iron shifted to the substrate and mixed with silicon.

  20. XRD and neutron diffraction analyses of heat treated U-Mo/Al dispersion fuel

    Energy Technology Data Exchange (ETDEWEB)

    Nam, Ji Min; Kim, Woo Jeong; Ryu, Ho Jin; Lee, Kyu Hong; Park, Jong Man [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2012-10-15

    High density U Mo alloys are regarded as promising candidates for advanced research reactor fuel because they have shown stable irradiation performance when compared to other uranium alloys and compounds. However, interaction layer formation between the U Mo alloys and Al matrix degrades the irradiation performance of U Mo dispersion fuel. Therefore, addition of Ti in U Mo alloys, addition of Si in Al matrix and silicide or nitride coating on the surface of U Mo particles have been proposed in order to inhibit the interaction layer growth. In order to analyze the mechanisms of interaction layer growth inhibition by adding Ti in U Mo alloys or Si in Al matrix, accurate phase characterization of the interaction layers is required. While previous studies using X ray diffraction have been reported, laboratory X ray diffraction method has limitations such as low resolution and small measurement volume. Neutron diffraction method can be a more accurate analysis when compared with X ray diffraction method due to the large penetration depth of neutron. In this study, X ray diffraction and neutron diffraction experiments have been performed by using the laboratory X ray diffractometer and high resolution powder diffractometer (HRPD) of the HANARO research reactor in KAERI.

  1. Sample environment for in situ synchrotron XRD measurements for CO2 interaction with subsurface materials

    Science.gov (United States)

    Elbakhshwan, M.; Gill, S.; Weidner, R.; Ecker, L.

    2017-12-01

    Sequestration of CO2 in geological formations requires a deep understanding of its interaction with the cement-casing components in the depleted oil and gas wells. Portland cement is used to seal the wellbores; however it tends to interact with the CO2. Therefore it is critical to investigate the wellbore integrity over long term exposure to CO2. Studies showed that, CO2 leakage is due to the flow through the casing-cement microannulus, cement-cement fractures, or the cement-caprock interface. The objective of this work is to gain a better understanding of the dissolution process of the cement-casing in the CO2 flow channels alongside with the carbonation reactions at the interfaces using XRF, XANES and X-ray tomography techniques. In this study, a synthetic wellbore system, consisting of cement with an embedded rectangular length of steel casing that had grooves to accommodate fluid flow, was used to investigate the casing-cement microannulus through core-flood experiments. The objective of this work is to gain a better understanding of the dissolution process of the cement-casing in the CO2 flow channels alongside with the carbonation reactions at the interfaces using a sample environment designed and built for in situ X-ray diffraction in the National Synchrotron Light Source II (NSLS II). The formation of carbonate phases at cement -fluid and cement-steel/fluid interfaces will be monitored in real time. Samples may be exposed to super critical CO2 at pressures above 1100 psi and temperatures around 50°C. The reaction cell is built from hastealloy to provide corrosion resistance, while the experimental temperature and pressure are controlled with thermocouples and pressure vessel.

  2. Investigation of CaO-CO₂ reaction kinetics by in-situ XRD using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Biasin, A.; Segre, C. U.; Salviulo, G.; Zorzi, F.; Strumendo, M. [Padova; (IIT)

    2015-02-05

    In this work, in-situ synchrotron radiation x-ray powder diffraction (SR-XRPD), performed at the Advanced Photon Source (APS) facilities of the Argonne National Laboratory, was applied to investigate the CaO–CO2 reaction. A set of CO2 absorption experiments were conducted in a high temperature reaction capillary with a controlled atmosphere (CO2 partial pressure of 1 bar), in the temperature range between 450 °C and 750 °C using CaO based sorbents obtained by calcination of commercial calcium carbonate. The evolution of the crystalline phases during CO2 uptake by the CaO solid sorbents was monitored for a carbonation time of 20 min as a function of the carbonation temperature and of the calcination conditions. The Rietveld refinement method was applied to estimate the calcium oxide conversion during the reaction progress and the average size of the initial (at the beginning of carbonation) calcium oxide crystallites. The measured average initial carbonation rate (in terms of conversion time derivative) of 0.280 s-1 (±13.2% standard deviation) is significantly higher than the values obtained by thermo-gravimetric analysis and reported thus far in the literature. Additionally, a dependence of the conversion versus time curves on the initial calcium oxide crystallite size was observed and a linear relationship between the initial CaO crystallite size and the calcium oxide final conversion was identified.

  3. Mössbauer and XRD studies of Roman amphorae buried in the sea for two millennia

    Science.gov (United States)

    Wagner, F. E.; Wagner, U.; Häusler, W.; Costa, B. F. O.; Blot, J.-Y.; Silva, A. J. M.; Bombico, S.

    2016-12-01

    During the years 2004-2007 many Roman amphora sherds were found in the sea near Cortiçais, off the southern coast of the Peniche peninsula on the Atlantic coast of Portugal. The amphorae are of the Haltern 70 type and stem from a shipwreck that has been dated to the time of the emperor Augustus, between about 15 BC and 15 AD. They were produced in the Roman Province of Baetica in the south of Spain and used to transport wine and other staple foods by sea to other Roman settlements. We have studied several fragments of these amphorae by 57Fe Mössbauer spectroscopy and X-ray diffraction in order to look for changes in the ceramic material caused by two millennia of exposure to sea water. For comparison Mössbauer data on a Haltern 70 type amphora handle excavated on land at the site of Castro do Vieito in the north of Portugal were used. The fragments on which we report here are a body sherd and two handles. The sherds show a visible layer structure. The different layers were studied separately. The Mössbauer spectra of the buff surface layers indicate that up to about 60 % of the iron is present as very fine goethite particles, which are superparamagnetic at RT but exhibit magnetically split spectra at 4.2 K. Their blocking temperature is around or even below 50 K. The goethite is too fine grained to be detected by X-ray diffraction. Re-firing experiments confirm the presence of goethite, which is found to convert to hematite between 300 and 600 ∘C. The results show that the iron in the silicate matrix of the ceramic material converts to goethite under the prolonged influence of the sea water, mainly in the outermost several millimetres and apparently depending on the nature of the ceramic material.

  4. Mössbauer and XRD studies of Roman amphorae buried in the sea for two millennia

    Energy Technology Data Exchange (ETDEWEB)

    Wagner, F. E., E-mail: fwagner@tum.de; Wagner, U.; Häusler, W. [Technical University of Munich, Physics Department E15 (Germany); Costa, B. F. O. [University of Coimbra, CFisUC, Physics Department (Portugal); Blot, J.-Y. [Universidade Nova de Lisboa, CHAMFCSH (Portugal); Silva, A. J. M. [University of Coimbra, FCT/Centro de Estudos Arqueológicos das Universidades de Coimbra e do Porto (Portugal); Bombico, S. [University of Evora, CIDEHUS (Portugal)

    2016-12-15

    During the years 2004–2007 many Roman amphora sherds were found in the sea near Cortiçais, off the southern coast of the Peniche peninsula on the Atlantic coast of Portugal. The amphorae are of the Haltern 70 type and stem from a shipwreck that has been dated to the time of the emperor Augustus, between about 15 BC and 15 AD. They were produced in the Roman Province of Baetica in the south of Spain and used to transport wine and other staple foods by sea to other Roman settlements. We have studied several fragments of these amphorae by {sup 57}Fe Mössbauer spectroscopy and X-ray diffraction in order to look for changes in the ceramic material caused by two millennia of exposure to sea water. For comparison Mössbauer data on a Haltern 70 type amphora handle excavated on land at the site of Castro do Vieito in the north of Portugal were used. The fragments on which we report here are a body sherd and two handles. The sherds show a visible layer structure. The different layers were studied separately. The Mössbauer spectra of the buff surface layers indicate that up to about 60 % of the iron is present as very fine goethite particles, which are superparamagnetic at RT but exhibit magnetically split spectra at 4.2 K. Their blocking temperature is around or even below 50 K. The goethite is too fine grained to be detected by X-ray diffraction. Re-firing experiments confirm the presence of goethite, which is found to convert to hematite between 300 and 600 {sup ∘}C. The results show that the iron in the silicate matrix of the ceramic material converts to goethite under the prolonged influence of the sea water, mainly in the outermost several millimetres and apparently depending on the nature of the ceramic material.

  5. Mössbauer and XRD studies of Roman amphorae buried in the sea for two millennia

    International Nuclear Information System (INIS)

    Wagner, F. E.; Wagner, U.; Häusler, W.; Costa, B. F. O.; Blot, J.-Y.; Silva, A. J. M.; Bombico, S.

    2016-01-01

    During the years 2004–2007 many Roman amphora sherds were found in the sea near Cortiçais, off the southern coast of the Peniche peninsula on the Atlantic coast of Portugal. The amphorae are of the Haltern 70 type and stem from a shipwreck that has been dated to the time of the emperor Augustus, between about 15 BC and 15 AD. They were produced in the Roman Province of Baetica in the south of Spain and used to transport wine and other staple foods by sea to other Roman settlements. We have studied several fragments of these amphorae by "5"7Fe Mössbauer spectroscopy and X-ray diffraction in order to look for changes in the ceramic material caused by two millennia of exposure to sea water. For comparison Mössbauer data on a Haltern 70 type amphora handle excavated on land at the site of Castro do Vieito in the north of Portugal were used. The fragments on which we report here are a body sherd and two handles. The sherds show a visible layer structure. The different layers were studied separately. The Mössbauer spectra of the buff surface layers indicate that up to about 60 % of the iron is present as very fine goethite particles, which are superparamagnetic at RT but exhibit magnetically split spectra at 4.2 K. Their blocking temperature is around or even below 50 K. The goethite is too fine grained to be detected by X-ray diffraction. Re-firing experiments confirm the presence of goethite, which is found to convert to hematite between 300 and 600 "∘C. The results show that the iron in the silicate matrix of the ceramic material converts to goethite under the prolonged influence of the sea water, mainly in the outermost several millimetres and apparently depending on the nature of the ceramic material.

  6. [Research on characteristics of soil clay mineral evolution in paddy field and dry land by XRD spectrum].

    Science.gov (United States)

    Zhang, Zhi-dan; Li, Qiao; Luo, Xiang-li; Jiang, Hai-chao; Zheng, Qing-fu; Zhao, Lan-po; Wang, Ji-hong

    2014-08-01

    The present paper took the typical saline-alkali soil in Jilin province as study object, and determinated the soil clay mineral composition characteristics of soil in paddy field and dry land. Then XRD spectrum was used to analyze the evolutionary mechanism of clay mineral in the two kinds of soil. The results showed that the physical and chemical properties of soil in paddy field were better than those in dry land, and paddy field would promote the weathering of mineral particles in saline-alkali soil and enhance the silt content. Paddy field soil showed a strong potassium-removal process, with a higher degree of clay mineral hydration and lower degree of illite crystallinity. Analysis of XRD spectrum showed that the clay mineral composition was similar in two kinds of soil, while the intensity and position of diffraction peak showed difference. The evolution process of clay mineral in dry land was S/I mixture-->vermiculite, while in paddy field it was S/I mixture-->vermiculite-->kaolinite. One kind of hydroxylated 'chlorite' mineral would appear in saline-alkali soil in long-term cultivated paddy field. Taking into account that the physical and chemical properties of soil in paddy field were better then those in dry land, we could know that paddy field could help much improve soil structure, cultivate high-fertility soil and improve saline-alkali soil. This paper used XRD spectrum to determine the characteristics of clay minerals comprehensively, and analyzed two'kinds of land use comparatively, and was a new perspective of soil minerals study.

  7. XRD and HRTEM characterization of mechanosynthesized Ti{sub 0.9}W{sub 0.1}C cermet

    Energy Technology Data Exchange (ETDEWEB)

    Bandyopadhyay, S. [Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India); Dutta, H. [Department of Physics, Vivekananda College, Burdwan 713103, West Bengal (India); Pradhan, S.K., E-mail: skp_bu@yahoo.com [Department of Physics, The University of Burdwan, Golapbag, Burdwan 713104, West Bengal (India)

    2013-12-25

    Highlights: •Cubic Ti{sub 0.9}W{sub 0.1}C is formed after 50 min of milling of α-Ti, W and graphite powders. •Nanocrystalline Ti{sub 0.9}W{sub 0.1}C with particle size ∼11 nm is obtained after 8 h milling. •Average particle size of Ti{sub 0.9}W{sub 0.1}C from XRD analysis and HRTEM is very close. •Formation of Ti{sub 0.9}W{sub 0.1}C is hindered as compared with TiC. -- Abstract: Elemental powder mixture of titanium, tungsten and graphite is milled by high energy planetary ball mill at a fixed ball to powder mass ratio (BPMR) for different duration to produce nanosized particles of Ti{sub 0.9}W{sub 0.1}C hard metal. Microstructure characterization in terms of lattice imperfections and phase quantification of ball-milled samples has been done primarily by analyzing the XRD pattern and employing Rietveld method of structure and microstructure refinement. After 8 h of ball-milling full formation of Ti{sub 0.9}W{sub 0.1}C is noticed without any contamination of other phase or milling media. TEM study of 8 h ball-milled sample gives direct supportive evidence of structural and microstructural evaluation by XRD pattern analysis. A comparative study of microstructural changes between TiC and Ti{sub 0.9}W{sub 0.1}C helps to understand the effect of addition of W as solute in Ti–C metal matrix.

  8. Evaluation of the physical stability and local crystallization of amorphous terfenadine using XRD-DSC and micro-TA

    International Nuclear Information System (INIS)

    Yonemochi, Etsuo; Hoshino, Takafumi; Yoshihashi, Yasuo; Terada, Katsuhide

    2005-01-01

    It is very difficult to follow rapid changes in polymorphic transformation and crystallization and to estimate the species recrystallized from the amorphous form. The aim of this study was to clarify the structural changes of amorphous terfenadine and to evaluate the polymorphs crystallized from amorphous samples using XRD-DSC and an atomic force microscope with a thermal probe (micro-TA). Amorphous samples were prepared by grinding or rapid cooling of the melt. The rapid structural transitions of samples were followed by the XRD-DSC system. On the DSC trace of the quenched terfenadine, two exotherms were observed, while only one exothermic peak was observed in the DSC scan of a ground sample. From the in situ data obtained by the XRD-DSC system, the stable form of terfenadine was recrystallized during heating of the ground amorphous sample, whereas the metastable form was recrystallized from the quenched amorphous sample and the crystallized polymorph changed to the stable form. Obtained data suggested that recrystallized species could be related to the homogeneity of samples. When the stored sample surface was scanned by atomic force microscopy (AFM), heterogeneous crystallization was observed. By using micro-TA, melting temperatures at various points were measured, and polymorph forms I and II were crystallized in each region. The percentages of the crystallized form I stored at 120 and 135 deg C were 47 and 79%, respectively. This result suggested that increasing the storage temperature increased the crystallization of form I, the stable form, confirming the temperature dependency of the crystallized form. The crystallization behavior of amorphous drug was affected by the annealing temperature. Micro-TA would be useful for detecting the inhomogeneities in polymorphs crystallized from amorphous drug

  9. Astrobiological Significance of Definitive Mineralogical Analysis of Martian Surface Samples Using the CheMin XRD/XRF Instrument

    Science.gov (United States)

    Feldman, S. M.; Blake, D. F.; Sarrazin, P.; Bish, D. L.; Chipera, S. J.; Vaniman, D. T.; Collins, S.

    2004-01-01

    The search for evidence of habitability, or of extant or extinct life on Mars, will initially be a search for evidence of past or present conditions supportive of life. The three key requirements for the emergence of life are thought to be liquid water; a suitable energy source; and chemical building blocks. CheMin is a miniaturized XRD/XRF (X-Ray diffraction / X-ray fluorescence) instrument which has been developed for definitive mineralogic analysis of soils and rocks on the Martian surface. The CheMin instrument can provide information that is highly relevant to each of these habitability requirements as summarized below.

  10. Operando XRD studies as a tool for determination of transport parameters of mobile ions in electrode materials

    Science.gov (United States)

    Kondracki, Łukasz; Kulka, Andrzej; Świerczek, Konrad; Ziąbka, Magdalena; Molenda, Janina

    2017-11-01

    In this work a detailed operando XRD investigations of structural properties of LixMn2O4 manganese spinel are shown to be a complementary, successful method of determination of diffusion coefficient D and surface exchange coefficient k in the working electrode. Kinetics of lithium ions transport are estimated on the basis of rate of structural changes of the cathode material during a relaxation stage after a high current charge, i.e. during structural relaxation of the material. The presented approach seems to be applicable as a complementary method of determination of transport coefficients for all intercalation-type electrode materials.

  11. Structural, electronic and optical properties of monoclinic Na2Ti3O7 from density functional theory calculations: A comparison with XRD and optical absorption measurements

    International Nuclear Information System (INIS)

    Araújo-Filho, Adailton A.; Silva, Fábio L.R.; Righi, Ariete; Silva, Mauricélio B. da; Silva, Bruno P.; Caetano, Ewerton W.S.; Freire, Valder N.

    2017-01-01

    Powder samples of bulk monoclinic sodium trititanate Na 2 Ti 3 O 7 were prepared carefully by solid state reaction, and its monoclinic P2 1 /m crystal structure and morphology were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM), respectively. Moreover, the sodium trititanate main energy band gap was estimated as E g =3.51±0.01 eV employing UV–Vis spectroscopy, which is smaller than the measured 3.70 eV energy gap published previously by other authors. Aiming to achieve a better understanding of the experimental data, density functional theory (DFT) computations were performed within the local density and generalized gradient approximations (LDA and GGA, respectively) taking into account dispersion effects through the scheme of Tkatchenko and Scheffler (GGA+TS). Optimal lattice parameters, with deviations relative to measurements Δa=−0.06 Å, Δb=0.02 Å, and Δc=−0.09 Å, were obtained at the GGA level, which was then used to simulate the sodium trititanate electronic and optical properties. Indirect band transitions have led to a theoretical gap energy value of about 3.25 eV. Our results, however, differ from pioneer DFT results with respect to the specific Brillouin zone vectors for which the indirect transition with smallest energy value occurs. Effective masses for electrons and holes were also estimated along a set of directions in reciprocal space. Lastly, our calculations revealed a relatively large degree of optical isotropy for the Na 2 Ti 3 O 7 optical absorption and complex dielectric function. - Graphical abstract: Monoclinic sodium trititanate Na2Ti3O7 was characterized by experiment and dispersion-corrected DFT calculations. An indirect gap of 3.5 eV is predicted, with heavy electrons and anisotropic holes ruling its conductivity. - Highlights: • Monoclinic Na2Ti3O7 was characterized by experiment (XRD, SEM, UV–Vis spectroscopy). • DFT GGA+TS optimized geometry and optoelectronic properties were

  12. Structure determination of electrodeposited zinc-nickel alloys: thermal stability and quantification using XRD and potentiodynamic dissolution

    International Nuclear Information System (INIS)

    Fedi, B.; Gigandet, M.P.; Hihn, J-Y; Mierzejewski, S.

    2016-01-01

    Highlights: • Quantification of zinc-nickel phases between 1,2% and 20%. • Coupling XRD to partial potentiodynamic dissolution. • Deconvolution of anodic stripping curves. • Phase quantification after annealing. - Abstract: Electrodeposited zinc-nickel coatings obtained by electrodeposition reveal the presence of metastable phases in various quantities, thus requiring their identification, a study of their thermal stability, and, finally, determination of their respective proportions. By combining XRD measurement with partial potentiodynamic dissolution, anodic peaks were indexed to allow their quantification. Quantification of electrodeposited zinc-nickel alloys approximately 10 μm thick was thus carried out on nickel content between 1.2% and 20%, and exhibited good accuracy. This method was then extended to the same set of alloys after annealing (250 °C, 2 h), thus bringing the structural organization closer to its thermodynamic equilibrium. The result obtained ensures better understanding of crystallization of metastable phases and of phase proportion evolution in a bi-phasic zinc-nickel coating. Finally, the presence of a monophase γ and its thermal stability in the 12% to 15% range provides important information for coating anti-corrosion behavior.

  13. The Crystal Structure of Micro- and Nanopowders of ZnS Studied by EPR of Mn2+ and XRD.

    Science.gov (United States)

    Nosenko, Valentyna; Vorona, Igor; Grachev, Valentyn; Ishchenko, Stanislav; Baran, Nikolai; Becherikov, Yurii; Zhuk, Anton; Polishchuk, Yuliya; Kladko, Vasyl; Selishchev, Alexander

    2016-12-01

    The crystal structure of micro- and nanopowders of ZnS doped with different impurities was analyzed by the electron paramagnetic resonance (EPR) of Mn 2+ and XRD methods. The powders of ZnS:Cu, ZnS:Mn, ZnS:Co, and ZnS:Eu with the particle sizes of 5-7 μm, 50-200 nm, 7-10 μm, and 5-7 nm, respectively, were studied. Manganese was incorporated in the crystal lattice of all the samples as uncontrolled impurity or by doping. The Mn 2+ ions were used as EPR structural probes. It is found that the ZnS:Cu has the cubic structure, the ZnS:Mn has the hexagonal structure with a rhombic distortion, the ZnS:Co is the mixture of the cubic and hexagonal phases in the ratio of 1:10, and the ZnS:Eu has the cubic structure and a distorted cubic structure with stacking defects in the ratio 3:1. The EPR technique is shown to be a powerful tool in the determination of the crystal structure for mixed-polytype ZnS powders and powders with small nanoparticles. It allows observation of the stacking defects, which is revealed in the XRD spectra.

  14. Synthesis of metal complexes involving Schiff base ligand with methylenedioxy moiety: spectral, thermal, XRD and antimicrobial studies.

    Science.gov (United States)

    Sundararajan, M L; Jeyakumar, T; Anandakumaran, J; Karpanai Selvan, B

    2014-10-15

    Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), Fe(III), Co(II), Mn(II) Hg(II), and Ag(I) have been synthesized from Schiff base ligand, prepared by the condensation of 3,4-(methylenedioxy)aniline and 5-bromo salicylaldehyde. All the compounds have been characterized by using elemental analysis, molar conductance, FT-IR, UV-Vis, (1)H NMR, (13)C NMR, mass spectra, powder XRD and thermal analysis (TG/DTA) technique. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The FT-IR, (1)H NMR, (13)C NMR and UV-Vis spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. Mass spectral data further support the molecular mass of the compounds and their structure. Powder XRD indicates the crystalline state and morphology of the ligand and its metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. Melting point supports the thermal stability of all the compounds. The in vitro antimicrobial effects of the synthesized compounds were tested against five bacterial and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more biological activity than the Schiff base. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Investigation of composition and structure of spongy and hard bone tissue using FTIR spectroscopy, XRD and SEM

    Science.gov (United States)

    Al-Akhras, M.-Ali H.; Hasan Qaseer, M. K.; Albiss, B. A.; Alebrhim, M. Anwar; Gezawa, Umar S.

    2018-02-01

    Valuable structural and chemical features can be obtained for spongy and hard bone by infrared spectroscopy and X-ray diffraction. A better understanding of chemical and structural differences between spongy and hard bone is a very important contributor to bone quality. Our data according to IR data showed that the collagen cross-links occurred to be higher in spongy bone, and crystallinity was lower in spongy bone. Deconvolution of the infrared band near 870 cm-1 reveals evidence for A2-type carbonate substitution on hydroxyapatite of spongy bone in addition to the A and B type carbonate substitution that are also found in hard bone. IR and XRD data confirmed the results of each other since full width at half maximum of 002-apatite pattern of XRD showed that the crystallinity was lower in spongy bone. The microstructure was examined by using scanning electron microscope and the result showed that the lattice of thin threads in spongy bone and is less dense than hard bone.

  16. Moessbauer, TEM/SAED and XRD investigation on waste dumps of the Valea lui Stan gold mines

    Energy Technology Data Exchange (ETDEWEB)

    Constantinescu, Serban Grigore, E-mail: sconst@infim.ro [National Institute of Materials Physics, Bucharest-Magurele (Romania); Udubasa, Sorin S.; Udubasa, Gheorghe [University of Bucharest, Fac. of Geology and Geophysics (Romania); Kuncser, Victor; Popescu-Pogrion, Nicoleta; Mercioniu, Ionel; Feder, Marcel [National Institute of Materials Physics, Bucharest-Magurele (Romania)

    2012-03-15

    The complementary investigation techniques, Moessbauer spectroscopy, transmission electron microscopy with selected area electron diffraction (TEM/SAED), X-ray diffraction (XRD) have been used to investigate the fate of the Valea lui Stan, Romania, gold-ore nanoscale-minerals during the long time of residence in the waste dumps. The preliminary investigations showed such waste dumps to contain significant amount of metals which cannot be identified by conventional methods. An intense research activity started up in order to evaluate the possibilities to recycle Valea lui Stan waste dumps and to recover metals by chemical or phytoextraction procedures. The waste dumps naturally show different mineral constituents with clay minerals as major phases, observed by XRD-technique. Although the waste dumps materials have whitish-yellowish colours, MOeSSBAUER technique evidences the presence of the finely dispersed iron bearing minerals. The authors are focusing to inspect and analyze Fe-compounds in the samples collected from Valea lui Stan's waste dumps in order to identify the magnetic phases by Moessbauer technique.

  17. Evaluation of the charge-sharing effects on spot intensity in XRD setup using photon-counting pixel detectors

    International Nuclear Information System (INIS)

    Nilsson, H.-E.; Mattsson, C.G.; Norlin, B.; Froejdh, C.; Bethke, K.; Vries, R. de

    2006-01-01

    In this study, we examine how charge loss due to charge sharing in photon-counting pixels detectors affects the recording of spot intensity in an X-ray diffraction (XRD) setup. In the photon-counting configuration, the charge from photons that are absorbed at the boarder of a pixel will be shared between two pixels. If the threshold is high enough, these photons will not be counted whereas if it is low enough, they will be counted twice. In an XRD setup, the intensity and position of various spots should be recorded. Thus, the intensity measure will be affected by the setting of the threshold. In this study, we used a system level Monte Carlo simulator to evaluate the variations in the intensity signals for different threshold settings and spot sizes. The simulated setup included an 8keV mono-chromatic source (providing a Gaussian shaped spot) and the MEDIPIX2 photon-counting pixel detector (55 μm x 55 μm pixel size with 300μm silicon) at various detector biases. Our study shows that the charge-sharing distortion can be compensated by numerical post processing and that high resolution in both charge distribution and position can be achieved

  18. Effect of water molecule distribution on the quantitative XRD analysis in the case of Na-montmorillonite exchanged Cu2+

    International Nuclear Information System (INIS)

    Oueslati, W.; Meftah, M.; Ben Rhaiem, H.; Ben Haj Amara, A.

    2010-01-01

    Document available in extended abstract form only. Several theoretical models are proposed to describe hydration process for Wyoming-montmorillonite clay exchanged Na + or Cu 2+ . They propose some theoretical distribution and disposition for water molecule in the inter-lamellar space in the case of homogeneous and inter-stratified hydration states. For example, Ben Brahim et al. (1983a) studied the interlayer structure (atomic positions of interlayer cations) and associated H 2 O molecules of Na-saturated montmorillonite and beidellite samples. Moore and Hower (1986) studied ordered structures composed of mono-hydrated and collapsed interlayers in montmorillonite, and Cuadros (1996) estimated the H 2 O content of smectite as a function of the interlayer cation. Using similar approach, Ferrage et al (2005b) proposed a discreet distribution of water molecule layer in the same z coordinate of the exchangeable cation with inhomogeneous distribution. This heterogeneity was attributed to the surface charge. The main objective of this study is to characterize the structural changes in the theoretical XRD profile, induced by different water molecule distribution, used to simulate experimental XRD patterns in the case of Na-montmorillonite exchanged Cu 2+ . This problem was achieved by quantitative XRD analysis using an indirect method based on the comparison of the experimental 001 reflections obtained from oriented films patterns with those calculated from structural models. The starting materials were Ca-montmorillonite originated from bentonites of Wyoming (USA). The XRD patterns were obtained by reflection setting with a D8 ADVANCE Bruker installation using Cu-Kα radiation and equipped with solid state detector. Intensities were measured at an interval of 2Θ 0.04 deg. and 40-50 s counting time per step. The diffracted intensity was calculated according to the matrix formalism detailed by Drits and Tchoubar, (1990). The fitting strategies was detailed by Ferrage et

  19. Comparative investigation of Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD) in the determination of cotton fiber crystallinity.

    Science.gov (United States)

    Liu, Yongliang; Thibodeaux, Devron; Gamble, Gary; Bauer, Philip; VanDerveer, Don

    2012-08-01

    Despite considerable efforts in developing curve-fitting protocols to evaluate the crystallinity index (CI) from X-ray diffraction (XRD) measurements, in its present state XRD can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous fraction in a sample. The greatest barrier to establishing quantitative XRD is the lack of appropriate cellulose standards, which are needed to calibrate the XRD measurements. In practice, samples with known CI are very difficult to prepare or determine. In a previous study, we reported the development of a simple algorithm for determining fiber crystallinity information from Fourier transform infrared (FT-IR) spectroscopy. Hence, in this study we not only compared the fiber crystallinity information between FT-IR and XRD measurements, by developing a simple XRD algorithm in place of a time-consuming and subjective curve-fitting process, but we also suggested a direct way of determining cotton cellulose CI by calibrating XRD with the use of CI(IR) as references.

  20. XRD analysis of strained Ge-SiGe heterostructures on relaxed SiGe graded buffers grown by hybrid epitaxy on Si(0 0 1) substrates

    International Nuclear Information System (INIS)

    Franco, N.; Barradas, N.P.; Alves, E.; Vallera, A.M.; Morris, R.J.H.; Mironov, O.A.; Parker, E.H.C.

    2005-01-01

    Ge/Si 1-x Ge x inverted modulation doped heterostructures with Ge channel thickness of 16 and 20 nm were grown by a method of hybrid epitaxy followed by ex situ annealing at 650 deg. C for p-HMOS application. The thicker layers of the virtual substrate (6000 nm graded SiGe up to x = 0.6 and 1000 nm uniform composition with x = 0.6) were produced by ultrahigh vacuum chemical vapor deposition (UHV-CVD) while the thinner, Si(2 nm)-SiGe(20 nm)-Ge-SiGe(15 nm + 5 nm B-doped + 20 nm) active layers were grown by low temperature solid-source (LT-SS) MBE at T = 350 deg. C. As-grown and annealed samples were measured by X-ray diffraction (XRD). Reciprocal space maps (RSMs) allowed us to determine non-destructively the precise composition (∼1%) and strain of the Ge channel, along with similar information regarding the other layers that made up the whole structure. Layer thickness was determined with complementary high-resolution Rutherford backscattering (RBS) experiments

  1. Characterization of explosives by x-ray diffraction and neutron scattering techniques: phase transformation study by synchrotron radiation XRD of forensically sourced ammonium nitrate pills

    International Nuclear Information System (INIS)

    Connor, B.O.; Blagojevic, N.

    2009-01-01

    Under direction of the Australian Department of Prime Minister and Cabinet ANSTO has commenced a three-year project with the title Characterisation of Explosives by XRD and Neutron Scattering Techniques. The initial focus is on Ammonium Nitrate (AN) based explosives with the intention to investigate all important energetic materials currently used in improvised explosives devices (IED) by various combative groups. The principal objective of the project is to use laboratory x-ray, synchrotron radiation (SR) and neutron scattering fingerprinting to establish associations between the diffraction pattern information and the manufacturing sources of AN and other energetic materials. Laboratory and SR experiments, at room temperature, of commercial AN show that the phase structure is principally AN-IV. Our earlier work observed other phases such as previously unreported transformation of AN-IV to AN-II, again at room temperature. Our interest is to also characterise added phase stabiliser material, solid-solution altered AN as well as desiccant and moisture barrier coatings. This prospect points strongly to the possibility of fingerprinting the materials for inferring source-association relations. The enhanced pattern definition achievable using powder SR diffraction is expected to improve the crystal structure characterisation of the materials. Other properties such as temperature dependent phase transformation and strain anisotropy as well as trace elemental impurities will provide information to further define association linkages. (Author)

  2. Real-Time XRD Studies of Li-O2 Electrochemical Reaction in Nonaqueous Lithium-Oxygen Battery.

    Science.gov (United States)

    Lim, Hyunseob; Yilmaz, Eda; Byon, Hye Ryung

    2012-11-01

    Understanding of electrochemical process in rechargeable Li-O2 battery has suffered from lack of proper analytical tool, especially related to the identification of chemical species and number of electrons involved in the discharge/recharge process. Here we present a simple and straightforward analytical method for simultaneously attaining chemical and quantified information of Li2O2 (discharge product) and byproducts using in situ XRD measurement. By real-time monitoring of solid-state Li2O2 peak area, the accurate efficiency of Li2O2 formation and the number of electrons can be evaluated during full discharge. Furthermore, by observation of sequential area change of Li2O2 peak during recharge, we found nonlinearity of Li2O2 decomposition rate for the first time in ether-based electrolyte.

  3. Combined XRD and Raman studies of coke types found in SAPO-34 after methanol and propene conversion

    DEFF Research Database (Denmark)

    Wragg, David S.; Grønvold, Arne; Voronov, Alexey

    2013-01-01

    oligomerisation (PO) reactions. The coke caused by MTO leads to two distinct sets of HRPD peaks which can be indexed by two SAPO-34 unit cells with different lattice parameters and coke contents. We believe that these unit cells represent different zones of the catalyst filled with different coke types. PO coking...... does not lead to splitting of the diffraction peaks. Raman spectra show differences between the coke types produced by MTO and PO with the same overall trend of increasingly polyaromatic coke with increasing coke mass. The intensity of the monocyclic and polyaromatic peaks in the MTO Raman spectra...... correspond to the phase fractions of the two cell types used in the Rietveld refinement, suggesting a link between the two phases and the two coke types. The PO Raman spectra have a stronger polyaromatic band at low coke, suggesting that polyaromatics form faster. In situ powder XRD studies suggest...

  4. Identification of reaction compounds in micrometric layers from gothic paintings using combined SR-XRD and SR-FTIR.

    Science.gov (United States)

    Salvadó, Nati; Butí, Salvador; Nicholson, James; Emerich, Hermann; Labrador, Ana; Pradell, Trinitat

    2009-07-15

    Synchrotron radiation X-ray diffraction (micro-SR-XRD) and Fourier transform infrared spectroscopy (micro-SR-FTIR) are used in the non-destructive identification of reaction and aging compounds from micrometric ancient painting layers. The combination of the micrometer size and non-destructive nature of the techniques together with the high resolution and brilliance of the synchrotron radiation has proved to be a procedure most advantageous for the study of reaction, aging and degradation processes. Copper, lead and calcium carboxylates and oxalates are determined in the chromatic, preparation and alteration layers from 15th century egg tempera and oil paintings. Their nature and crystallinity have been assessed. Some hypothesis about the mechanisms of development of both carboxylates and oxalates are presented.

  5. Characterization of ash pond ashes from 3rd thermal power plant by SEM/EDX and XRD methods

    Directory of Open Access Journals (Sweden)

    A Minjigmaa

    2014-10-01

    Full Text Available   Coal combustion by products from ash pond of 3rdthermal power plant of Ulaanbaatar city have been collected in 2010 and 2013 years. The ash samples have been characterized by XRD, XRF and SEM-EDX methods in order to evaluate their chemical and mineralogical composition changes with disposed times. The mineralogical composition of ash varies with time though the chemical composition of the ashes were close each other. Possibly, inefficient operating condition of the TPS shows influence on the mineralogical composition.DOI: http://dx.doi.org/10.5564/mjc.v14i0.201Mongolian Journal of Chemistry 14 (40, 2013, p61-65

  6. Micro-XRD Stress And Texture Study Of Inlaid Copper Lines - Influence Of ILD, Liner And Etch Stop Layer

    International Nuclear Information System (INIS)

    Prinz, H.; Zienert, I.; Rinderknecht, J.; Geisler, H.; Zschech, E.; Besser, P.

    2004-01-01

    The influence of ILD, liner and etch stop layer on the room temperature stress state of copper line test structures was examined by micro-XRD. Test structures consisted of large arrays of parallel lines with line widths of 0.18 μm and 1.8 μm. All these parameters have an influence on the room temperature stress state, whereas the variation of the liner and the ILD showed the largest effects. The change from a full low-k stack to a hybrid stack, where SiO2 ILD is use for the 'via layer' only and low-k material for the 'line layer' results in completely different parameter dependencies. The relationship between copper microstructure and the resulting stress in copper lines is discussed

  7. Platinum incorporation in the Na Y zeolite through impregnation method, and characterization by XRD, FTIR and nitrogen adsorption

    International Nuclear Information System (INIS)

    Araujo, A.S.; Sousa, B.V.; Andrade, A.C.C.; Rodrigues, M.G.F.; Rangel, M.C.

    2007-01-01

    Supported metal catalysts are widely used in petroleum refining, chemical and petroleum industries. These catalysts are important in ammonia synthesis, conversion of hydrocarbons with water vapor to synthesis gas, reforming, hydrocracking, ... Platinum has long been used in cracking, hydrogenation and dehydrogenation processes. The aim of this project is the Na Y zeolitic sample preparation through impregnation for incipient humidity, with 0,5% concentration of platinum, aiming its use as a catalyst in the steam reforming reaction. The characterization techniques used were: X Rays Diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR) and Nitrogen Adsorption (BET Method). From the obtained results through the techniques mentioned previously it is possible to evidence that the platinum impregnation process did not change the Na Y zeolite structure. Through the superficial specific area (BET) it was possible to observe that the platinum impregnation process caused a decrease in the specific area due to the reduction to the accessibility to the micropores of the zeolitic structure. (author)

  8. Spectral Resolution for Five-Element, Filtered, X-Ray Detector (XRD) Arrays Using the Methods of Backus and Gilbert

    International Nuclear Information System (INIS)

    FEHL, DAVID LEE; BIGGS, F.; CHANDLER, GORDON A.; STYGAR, WILLIAM A.

    2000-01-01

    The generalized method of Backus and Gilbert (BG) is described and applied to the inverse problem of obtaining spectra from a 5-channel, filtered array of x-ray detectors (XRD's). This diagnostic is routinely fielded on the Z facility at Sandia National Laboratories to study soft x-ray photons ((le)2300 eV), emitted by high density Z-pinch plasmas. The BG method defines spectral resolution limits on the system of response functions that are in good agreement with the unfold method currently in use. The resolution so defined is independent of the source spectrum. For noise-free, simulated data the BG approximating function is also in reasonable agreement with the source spectrum (150 eV black-body) and the unfold. This function may be used as an initial trial function for iterative methods or a regularization model

  9. Growth and XRD analysis of the diluted magnetic semiconductor Zn{sub 1-x}Ni{sub x}O

    Energy Technology Data Exchange (ETDEWEB)

    Syed Ali, K.S. [Department of Science, Estill High School, Post Office Box 754, Estill, South Carolina - 29918 (United States); Saravanan, R. [Department of Physics, The Madura College, Madurai - 625 011 (India); Acikgoez, M. [Bahcesehir University, Faculty of Arts and Sciences, Besiktas - 34349 (Turkey)

    2011-01-15

    Diluted magnetic semiconductor compound Zn{sub 1-x}Ni{sub x} O(x =0.01, 0.02, 0.03, 0.04 and 0.05) was prepared by sol-gel method and characterized using powder XRD for the distribution of electrons and bonding in the unit cell. The electronic structural studies of this material were carried out by maximum entropy method (MEM) for the quantitative and qualitative measurement on the inclusion and the effect induced on bonding by Ni doping. The spatial arrangement of charge and the bonding behavior of this material were analyzed from 3D, 2D and 1D density distributions. The evidence for the addition of Ni in the host lattice of Zn is realized. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  10. The use of combined synchrotron radiation micro FT-IR and XRD for the characterization of Romanesque wall paintings

    International Nuclear Information System (INIS)

    Salvado, N.; Buti, S.; Pantos, E.; Bahrami, F.; Labrador, A.; Pradell, T.

    2008-01-01

    The high analytical sensitivity and high spatial resolution of synchrotron radiation-based techniques, in particular SR-XRD and SR-FT-IR, allows the identification of complex micrometric mixtures of compounds that constitute the different layers of ancient paintings. The reliability of the measurements even with an extremely small amount of sampled material is very high, and this is particularly important when analyzing art works. Furthermore, the micro size (10 x 10μm for FT-IR and 30 to 50 μm squared spot size for XRD) of the beam enables one to obtain detailed compositional profiles from the different chromatic and preparation layers. The sensitivity of the techniques is high enough for the determination of minor and trace compounds, such as reaction and weathering compounds. We report here the identification of pigments in the Romanesque wall paintings found in situ in the church of Saint Eulalia of Unha place in the Aran valley (central Pyrenees). During the first centuries of the second millennium numerous religious buildings were built in Western Europe in the Romanesque style. In particular, a great number of churches were built in the Pyrenees, most of which were decorated with wall paintings. Although only a few of these paintings have survived, they represent one of the most important collections of Romanesque art, both for their quantity and quality. A full identification of the pigments, binder, supports, and reaction and weathering compounds has been obtained. The results obtained, in particular aerinite as a pigment, indicate a clear connection between the paintings found in this Occitanian church and the Catalan Romanesque paintings from the south bound of the Pyrenees. (orig.)

  11. The use of combined synchrotron radiation micro FT-IR and XRD for the characterization of Romanesque wall paintings

    Energy Technology Data Exchange (ETDEWEB)

    Salvado, N.; Buti, S. [Universitat Politecnica de Catalunya, Dpt. d' Enginyeria Quimica, EPSEVG, Vilanova i la Geltru, Barcelona (Spain); Pantos, E.; Bahrami, F. [CCLRC, Daresbury Laboratory, Warrington (United Kingdom); Labrador, A. [LLS, BM16-ESRF, BP 220, Grenoble Cedex (France); Pradell, T. [Universitat Politecnica de Catalunya, Dpt. Fisica i Enginyeria Nuclear, ESAB, Castelldefels, Barcelona (Spain)

    2008-01-15

    The high analytical sensitivity and high spatial resolution of synchrotron radiation-based techniques, in particular SR-XRD and SR-FT-IR, allows the identification of complex micrometric mixtures of compounds that constitute the different layers of ancient paintings. The reliability of the measurements even with an extremely small amount of sampled material is very high, and this is particularly important when analyzing art works. Furthermore, the micro size (10 x 10{mu}m for FT-IR and 30 to 50 {mu}m squared spot size for XRD) of the beam enables one to obtain detailed compositional profiles from the different chromatic and preparation layers. The sensitivity of the techniques is high enough for the determination of minor and trace compounds, such as reaction and weathering compounds. We report here the identification of pigments in the Romanesque wall paintings found in situ in the church of Saint Eulalia of Unha place in the Aran valley (central Pyrenees). During the first centuries of the second millennium numerous religious buildings were built in Western Europe in the Romanesque style. In particular, a great number of churches were built in the Pyrenees, most of which were decorated with wall paintings. Although only a few of these paintings have survived, they represent one of the most important collections of Romanesque art, both for their quantity and quality. A full identification of the pigments, binder, supports, and reaction and weathering compounds has been obtained. The results obtained, in particular aerinite as a pigment, indicate a clear connection between the paintings found in this Occitanian church and the Catalan Romanesque paintings from the south bound of the Pyrenees. (orig.)

  12. Characterisation of 1,3-diammonium propylselenate monohydrate by XRD, FT-IR, FT-Raman, DSC and DFT studies

    Science.gov (United States)

    Thirunarayanan, S.; Arjunan, V.; Marchewka, M. K.; Mohan, S.; Atalay, Yusuf

    2016-03-01

    The crystals of 1,3-diammonium propylselenate monohydrate (DAPS) were prepared and characterised X-ray diffraction (XRD), FT-IR, FT-Raman spectroscopy, and DFT/B3LYP methods. It comprises protonated propyl ammonium moieties (diammonium propyl cations), selenate anions and water molecule which are held together by a number of hydrogen bonds and form infinite chains. The XRD data confirm the transfer of two protons from selenic acid to 1,3-diaminopropane molecule. The DAPS complex is stabilised by the presence of O-H···O and N-H···O hydrogen bonds and the electrostatic interactions as well. The N···O and O···O bond distances are 2.82-2.91 and 2.77 Å, respectively. The FT-IR and FT-Raman spectra of 1,3-diammonium propyl selenate monohydrate are recorded and the complete vibrational assignments have been discussed. The geometry is optimised by B3LYP method using 6-311G, 6-311+G and 6-311+G* basis sets and the energy, structural parameters, vibrational frequencies, IR and Raman intensities are determined. Differential scanning colorimetry (DSC) data were also presented to analyse the possibility of the phase transition. Complete natural bonding orbital (NBO) analysis is carried out to analyse the intramolecular electronic interactions and their stabilisation energies. The electrostatic potential of the complex lies in the range +1.902e × 10-2 to -1.902e × 10-2. The limits of total electron density of the complex is +8.43e × 10-2 to -8.43e × 10-2.

  13. Multivariate analysis of DSC-XRD simultaneous measurement data: a study of multistage crystalline structure changes in a linear poly(ethylene imine) thin film.

    Science.gov (United States)

    Kakuda, Hiroyuki; Okada, Tetsuo; Otsuka, Makoto; Katsumoto, Yukiteru; Hasegawa, Takeshi

    2009-01-01

    A multivariate analytical technique has been applied to the analysis of simultaneous measurement data from differential scanning calorimetry (DSC) and X-ray diffraction (XRD) in order to study thermal changes in crystalline structure of a linear poly(ethylene imine) (LPEI) film. A large number of XRD patterns generated from the simultaneous measurements were subjected to an augmented alternative least-squares (ALS) regression analysis, and the XRD patterns were readily decomposed into chemically independent XRD patterns and their thermal profiles were also obtained at the same time. The decomposed XRD patterns and the profiles were useful in discussing the minute peaks in the DSC. The analytical results revealed the following changes of polymorphisms in detail: An LPEI film prepared by casting an aqueous solution was composed of sesquihydrate and hemihydrate crystals. The sesquihydrate one was lost at an early stage of heating, and the film changed into an amorphous state. Once the sesquihydrate was lost by heating, it was not recovered even when it was cooled back to room temperature. When the sample was heated again, structural changes were found between the hemihydrate and the amorphous components. In this manner, the simultaneous DSC-XRD measurements combined with ALS analysis proved to be powerful for obtaining a better understanding of the thermally induced changes of the crystalline structure in a polymer film.

  14. The importance of XRD analysis in provenance and palaeoenvironmental studies of the Piedras de Afilar Formation, Neoproterozoic of Uruguay

    Science.gov (United States)

    Pamoukaghlian, K.; Poiré, D. G.; Gaucher, C.; Uriz, N.; Cingolani, C.; Frigeiro, P.

    2009-04-01

    The Piedras de Afilar Formation crops out in the southeast part of Uruguay, forming part of the Tandilia Terrane (sensu Bossi et al. 2005). Pamoukaghlian et al. (2006) and Gaucher et al. (2008) have published δ13C, δ18O and U/Pb SHRIMP results, which indicate a Neoproterozoic age for this formation. The palaeoenvironment has been defined as a shallow marine platform based on the presence of interference ripples, hummocky and mega-hummocky cross-stratification. X-ray diffraction (XRD) analyses help to better constrain the palaeoenvironment: the presence of chlorite/smectite found in black shales, suggest a reducing environment, and abundant illite indicates a cold to temperate climate. Provenance studies have been undertaken that utilise a combination of detailed palaeocurrent measurements, petrographic descriptions, XRD analyses, and geochemical isotopic analyses, including U/Pb SHRIMP determinations. Mineral compositional diagrams for sandstones suggest a stable cratonic provenance. Palaeocurrents are mainly from the NNE, indicating a provenance from the cratonic areas of the Tandilia Terrane. The illite crystal index indicates diagenetic to low-metamorphic conditions for the sequence; this is important to confirm that the identified minerals are authigenic. Clay minerals identified by XRD analysis of sandstones from the siliciclastic member are illite (80 - 90%), kaolinite (5 - 10%), and chlorite (5 - 10%). This is consistent with a provenance from the cratonic areas (quartz-feldspar dominated rock types). Isotopic analyses have been undertaken to provide better constraints on the tectonic setting. U/Pb SHRIMP ages for the youngest zircons are 990 Ma (Gaucher et al. 2008), and the basal granite (Granito de la Paz) is 2056 ± 11 Ma (Hartmann et al. 2001), suggesting a provenance from the Archaean basement for the Piedras de Afilar Formation, like its counterparts in the Rio de la Plata Craton. References Bossi, J., Piñeyro, D., Cingolani, C. (2005). El l

  15. Dynamics of Polymorphic Transformations in Palm Oil, Palm Stearin and Palm Kernel Oil Characterized by Coupled Powder XRD-DSC.

    Science.gov (United States)

    Zaliha, Omar; Elina, Hishamuddin; Sivaruby, Kanagaratnam; Norizzah, Abd Rashid; Marangoni, Alejandro G

    2018-06-01

    The in situ polymorphic forms and thermal transitions of refined, bleached and deodorized palm oil (RBDPO), palm stearin (RBDPS) and palm kernel oil (RBDPKO) were investigated using coupled X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Results indicated that the DSC onset crystallisation temperature of RBDPO was at 22.6°C, with a single reflection at 4.2Å started to appear from 23.4 to 17.1°C, and were followed by two prominent exothermic peaks at 20.1°C and 8.5°C respectively. Further cooling to -40°C leads to the further formation of a β'polymorph. Upon heating, a of β'→βtransformation was observed between 32.1 to 40.8°C, before the sample was completely melted at 43.0°C. The crystallization onset temperature of RBDPS was 44.1°C, with the appearance of the α polymorph at the same temperature as the appearance of the first sharp DSC exothermic peak. This quickly changed from α→β´ in the range 25 to 21.7°C, along with the formation of a small β peak at -40°C. Upon heating, a small XRD peak for the β polymorph was observed between 32.2 to 36.0°C, becoming a mixture of (β´+ β) between 44.0 to 52.5°C. Only the β polymorph survived further heating to 59.8°C. For RBDPKO, the crystallization onset temperature was 11.6°C, with the formation of a single sharp exothermic peak at 6.5°C corresponding to the β' polymorphic form until the temperature reached -40°C. No transformation of the polymorphic form was observed during the melting process of RBDPKO, before being completely melted at 33.2°C. This work has demonstrated the detailed dynamics of polymorphic transformations of PKO and PS, two commercially important hardstocks used widely by industry and will contribute to a greater understanding of their crystallization and melting dynamics.

  16. Uranium speciation in 30-year old Freital mine tailings: an EXAFS, {mu}-XRD, and {mu}-XRF study

    Energy Technology Data Exchange (ETDEWEB)

    Scheinost, A.C.; Hennig, C. [Institute of Radiochemistry, FZR, D-01314 Dresden (Germany); Somogyi, A. [Synchrotron Soleil, F-91192 Gif-sur-Yvette (France); Martinez-Criado, G. [ESRF, ID-22, F-38043 Grenoble (France); Knappik, R. [VKTA Rossendorf, D-01314 Dresden (Germany)

    2005-07-01

    Full text of publication follows: Risk assessments of actinide-contaminated soils and sediments require detailed knowledge of actinide speciation and its long-term kinetics. Former Saxonian mine tailings, which have been covered but else left undisturbed, are ideally suited to study changes in uranium speciation over timescales of decades. We investigated the major uranium species in two samples from buried mine tailings using a combination of Synchrotron-based microfocus-techniques ({mu}-XRF, {mu}-XRD with micrometer resolution), bulk EXAFS spectroscopy, and chemical extractions. In sample F1 (5 m depth, oxic, pH 8, U = 440 mg/kg, high Ca, S, Pb, Cu, Zn concentrations), uranium is diffusely distributed among aggregates of layer silicates (muscovite, illite and kaolinite). The chemical extractions and EXAFS results confirm that uranium is sorbed to these minerals, but is not incorporated into their crystal structure. Sorption is also in line with the high pH and low carbonate concentrations in pore water. In sample F3 (12 m depth, oxic, pH 4, U = 430 mg/kg), the combination of {mu}-XRF and {mu}-XRD enabled us to identify several U(IV) and U(VI) containing minerals like coffinite, uraninite, uranyl hydroxide, and vanuralite. Only a minor part of U is sorbed to layer silicates as confirmed by chemical extractions and EXAFS spectroscopy. At smaller depth (F1, 5 m), sulfuric acid from the ore extraction procedure was completely neutralized by the construction waste used as cover material, resulting in precipitation of jarosite and gypsum. Even 30 years after the ore extraction, uranium remains highly soluble. At greater depth (F3, 12 m), the low pH from ore extraction was conserved. The presence of U(IV) minerals suggest either precipitation of secondary (IV) minerals due to microbial redox activity, or incomplete dissolution of primary (IV) minerals due to ore processing inefficiency of these older sediments. The U(IV) minerals were recalcitrant during chemical

  17. Uranium speciation in 30-year old Freital mine tailings: an EXAFS, μ-XRD, and μ-XRF study

    International Nuclear Information System (INIS)

    Scheinost, A.C.; Hennig, C.; Somogyi, A.; Martinez-Criado, G.; Knappik, R.

    2005-01-01

    Full text of publication follows: Risk assessments of actinide-contaminated soils and sediments require detailed knowledge of actinide speciation and its long-term kinetics. Former Saxonian mine tailings, which have been covered but else left undisturbed, are ideally suited to study changes in uranium speciation over timescales of decades. We investigated the major uranium species in two samples from buried mine tailings using a combination of Synchrotron-based microfocus-techniques (μ-XRF, μ-XRD with micrometer resolution), bulk EXAFS spectroscopy, and chemical extractions. In sample F1 (5 m depth, oxic, pH 8, U = 440 mg/kg, high Ca, S, Pb, Cu, Zn concentrations), uranium is diffusely distributed among aggregates of layer silicates (muscovite, illite and kaolinite). The chemical extractions and EXAFS results confirm that uranium is sorbed to these minerals, but is not incorporated into their crystal structure. Sorption is also in line with the high pH and low carbonate concentrations in pore water. In sample F3 (12 m depth, oxic, pH 4, U = 430 mg/kg), the combination of μ-XRF and μ-XRD enabled us to identify several U(IV) and U(VI) containing minerals like coffinite, uraninite, uranyl hydroxide, and vanuralite. Only a minor part of U is sorbed to layer silicates as confirmed by chemical extractions and EXAFS spectroscopy. At smaller depth (F1, 5 m), sulfuric acid from the ore extraction procedure was completely neutralized by the construction waste used as cover material, resulting in precipitation of jarosite and gypsum. Even 30 years after the ore extraction, uranium remains highly soluble. At greater depth (F3, 12 m), the low pH from ore extraction was conserved. The presence of U(IV) minerals suggest either precipitation of secondary (IV) minerals due to microbial redox activity, or incomplete dissolution of primary (IV) minerals due to ore processing inefficiency of these older sediments. The U(IV) minerals were recalcitrant during chemical extractions

  18. Single pulse analysis of intracranial pressure for a hydrocephalus implant.

    Science.gov (United States)

    Elixmann, I M; Hansinger, J; Goffin, C; Antes, S; Radermacher, K; Leonhardt, S

    2012-01-01

    The intracranial pressure (ICP) waveform contains important diagnostic information. Changes in ICP are associated with changes of the pulse waveform. This change has explicitly been observed in 13 infusion tests by analyzing 100 Hz ICP data. An algorithm is proposed which automatically extracts the pulse waves and categorizes them into predefined patterns. A developed algorithm determined 88 %±8 % (mean ±SD) of all classified pulse waves correctly on predefined patterns. This algorithm has low computational cost and is independent of a pressure drift in the sensor by using only the relationship between special waveform characteristics. Hence, it could be implemented on a microcontroller of a future electromechanic hydrocephalus shunt system to control the drainage of cerebrospinal fluid (CSF).

  19. Trichloroethylene (TCE) removal in a single pulse suspension bioreactor

    Czech Academy of Sciences Publication Activity Database

    Volčík, V.; Hoffmann, J.; Růžička, J.; Sergejevova, Magda

    2005-01-01

    Roč. 74, - (2005), s. 293-304 ISSN 0301-4797 R&D Projects: GA MŠk LN00A141 Institutional research plan: CEZ:AV0Z50200510 Keywords : trichlorethylene * phenol * cometabolism Subject RIV: EE - Microbiology, Virology Impact factor: 1.163, year: 2005

  20. Cooling the vertical surface by conditionally single pulses

    Directory of Open Access Journals (Sweden)

    Karpov Pavel

    2017-01-01

    Full Text Available You Sprays with periodic supply of the droplet phase have great opportunities to control the heat exchange processes. Varying pulse duration and frequency of their repetition, we can achieve the optimal conditions of evaporative cooling with minimization of the liquid flow rate. The paper presents experimental data on studying local heat transfer on a large subcooled surface, obtained on the original setup with multinozzle controlled system of impact irrigation by the gas-droplet flow. A contribution to intensification of the spray parameters (flow rate, pulse duration, repetition frequency per a growth of integral heat transfer was studied. Data on instantaneous distribution of the heat flux value helped us to describe the processes occurring on the studied surface. These data could describe the regime of “island” film cooling.

  1. Cooling the vertical surface by conditionally single pulses

    Science.gov (United States)

    Karpov, Pavel; Nazarov, Alexander; Serov, Anatoly; Terekhov, Victor

    2017-10-01

    You Sprays with periodic supply of the droplet phase have great opportunities to control the heat exchange processes. Varying pulse duration and frequency of their repetition, we can achieve the optimal conditions of evaporative cooling with minimization of the liquid flow rate. The paper presents experimental data on studying local heat transfer on a large subcooled surface, obtained on the original setup with multinozzle controlled system of impact irrigation by the gas-droplet flow. A contribution to intensification of the spray parameters (flow rate, pulse duration, repetition frequency) per a growth of integral heat transfer was studied. Data on instantaneous distribution of the heat flux value helped us to describe the processes occurring on the studied surface. These data could describe the regime of "island" film cooling.

  2. The Improvement Effect of Dispersant in Fluorite Flotation: Determination by the Analysis of XRD and FESEM-EDX

    Directory of Open Access Journals (Sweden)

    Y. J. Li

    2015-01-01

    Full Text Available Different dispersants were added in the dispersion process to improve the efficiency of fluorite flotation. The types and dosage of dispersant on the improvement of fluorite flotation were investigated; when the sodium polyacrylate (SPA was used as the dispersant and its addition is 0.5%, the concentrate grade of CaF2 increased from 90% to 98% and the fluorite recovery increased from 81% to 85%. Methods of X-ray powder diffraction (XRD, field emission scanning electron microscopy (FESEM, and Energy dispersive X-ray spectrometer (EDX were used to characterize the sample. According to the analysis of results, the optimal sample consisted of CaF2 and very little CaCO3 in the size range of 0–5 μm. It could be concluded that the mechanism of improvement for the concentrate grade and recovery of CaF2 was attributed to the change of potential energy barrier which caused the separation of particles with different charge. All results indicate that SPA has a great potential to be an efficient and cost-effective dispersant for the improvement of fluorite flotation.

  3. SR-XRD and SR-FTIR study of the alteration of silver foils in medieval paintings.

    Science.gov (United States)

    Salvadó, Nati; Butí, Salvador; Labrador, Ana; Cinque, Gianfelice; Emerich, Hermann; Pradell, Trinitat

    2011-03-01

    Altarpieces and polychrome carved wood from the fifteenth century AD usually exhibit golden and silvery areas by the application of a very thin foil of metal. The metal foils were normally protected from the atmosphere by a varnish or resin which maybe either preserved or absent. Moreover, they were glued to the background surface by adhesive substances (egg yolk, drying oil or animal glue). The high proportion of the glueing substances often renders the development of reaction compounds. With time, silver alters blacken or simply disappear completely. In this paper, we study the alterations to metal foils from a selection of fifteenth century artworks showing different glueing agents, organic coatings and several degrees of conservation of the organic coatings and metal leafs. The submillimetric layered structure and the high variability and low amount of most of the compounds present in the different layers, as well as their differing nature (organic and inorganic) make the use of micron-sensitive high-resolution techniques essential for their study. In particular, the high resolution, high brilliance and small footprint renders synchrotron radiation most adequate for their study. SR-XRD was performed to identify the reaction compounds formed in the different layers; μFTIR was used at to identify the silver protecting organic coatings, the metal foil glueing layers and the corresponding reaction compounds. The results obtained suggest that atmospheric corrosion is the dominant mechanism, and therefore that the degree of corrosion of the metal foils is mainly related to the conservation state of the protecting coatings.

  4. Mössbauer and XRD studies of NiCuZn ferrites by Sol-Gel auto-combustion

    International Nuclear Information System (INIS)

    Lei Chenglong; Lin Qing; Zhang Hui; He Yun; Huang Haifu

    2013-01-01

    The Ni 0.6 Cu 0.2 Zn 0.2 Ce x Fe 2-x O 4 ferrites (0≤x≤0.85) have been prepared by Sol-Gel auto-combustion method and we have investigated the effect of impurity CeO 2 phase to the microstructure and hyperfine magnetic field in spinel ferrite. The results of XRD patterns confirm the average crystallite size of samples decreases with Ce 3+ substitution increasing and the lattice parameters vary as a function of x content. 57 Fe Mössbauer spectra at room temperature for all samples confirm the [Fe 3+ - O 2- -Fe 3+ ] super exchange interaction decrease due to cerium substitution. For low temperature auto-combustion samples it reveals one normal sextet line and one doublet line x≤0.25, which shows well-resolved ferromagnetic order. Lattice defects are determined and Mössbauer spectrums vary from magnetic sextet to relaxation doublet at x≥0.45 due to a mass of CeO 2 phase. In contrast, the Mössbauer spectra for the samples sintered at 800°C/3h detect the secondary phase α -Fe 2 O 3 where the cation distribution occurs and it collapses to paramagnetic doublet (x≥0.85). Ce 3+ substitution has its maximum limit values of super exchange interaction and high sintering temperature will affect this interaction. (author)

  5. Adsorption of Lysine on Na-Montmorillonite and Competition with Ca(2+): A Combined XRD and ATR-FTIR Study.

    Science.gov (United States)

    Yang, Yanli; Wang, Shengrui; Liu, Jingyang; Xu, Yisheng; Zhou, Xiaoyun

    2016-05-17

    Lysine adsorption at clay/aqueous interfaces plays an important role in the mobility, bioavailability, and degradation of amino acids in the environment. Knowledge of these interfacial interactions facilitates our full understanding of the fate and transport of amino acids. Here, X-ray diffraction (XRD) and attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR) measurements were used to explore the dynamic process of lysine adsorption on montmorillonite and the competition with Ca(2+) at the molecular level. Density functional theory (DFT) calculations were employed to determine the peak assignments of dissolved lysine in the solution phase. Three surface complexes, including dicationic, cationic, and zwitterionic structures, were observed to attach to the clay edge sites and penetrate the interlayer space. The increased surface coverage and Ca(2+) competition did not affect the interfacial lysine structures at a certain pH, whereas an elevated lysine concentration contributed to zwitterionic-type coordination at pH 10. Moreover, clay dissolution at pH 4 could be inhibited at a higher surface coverage with 5 and 10 mM lysine, whereas the inhibition effect was inconspicuous or undetected at pH 7 and 10. The presence of Ca(2+) not only could remove a part of the adsorbed lysine but also could facilitate the readsorption of dissolved Si(4+) and Al(3+) and surface protonation. Our results provide new insights into the process of lysine adsorption and its effects on montmorillonite surface sites.

  6. Measurement and characterization of external oil in the fried waxy maize starch granules using ATR-FTIR and XRD.

    Science.gov (United States)

    Chen, Long; Tian, Yaoqi; Sun, Binghua; Cai, Canxin; Ma, Rongrong; Jin, Zhengyu

    2018-03-01

    Concerns regarding increased dietary oil uptake have prompted efforts to investigate the oil absorption and distribution in fried starchy foods. In the present study, attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, together with a chloroform-methanol method, was used to analyze the external and internal oil contents in fried starchy samples. The micromorphology of fried starchy samples was further investigated using scanning electron microscope (SEM), polarized light microscope (PLM) and confocal laser scanning microscopy (CLSM). The results indicated that large amounts of oil were absorbed in or within waxy maize starch, but the majority of oil was located near the surface layer of the starch granules. After defatting, the internal oil was thoroughly removed, while a small amount of external oil remained. As evidenced by the changes of the crystalline characteristics with the help of X-ray diffraction (XRD), the interaction between starch and lipids on the surface was confirmed to form V-type complex compounds during frying at high moisture. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. Investigation of structural resorption behavior of biphasic bioceramics with help of gravimetry, μCT, SEM, and XRD.

    Science.gov (United States)

    de Wild, Michael; Amacher, Fabienne; Bradbury, Christopher R; Molenberg, Aart

    2016-04-01

    Resorbable bone substitute materials are widely used for bone augmentation after tumor resection, parallel to implant placement, or in critical size bone defects. In this study, the structural dissolution of a biphasic calcium phosphate bone substitute material with a hydroxyapatite (HA)/tricalcium phosphate (β-TCP) ratio of 60/40 was investigated by repeatedly placing porous blocks in EDTA solution at 37 °C. At several time points, the blocks were investigated by SEM, µCT, and gravimetry. It was found that always complete 2-3 µm sized grains were removed from the structure and that the β-TCP is dissolved more rapidly. This selective dissolution of the β-TCP grains was confirmed by XRD measurements. The blocks were eroded from the outside toward the center. The structure remained mechanically stable because the central part showed a delayed degradation and because the slower dissolving HA grains preserved the integrity of the structure. © 2015 Wiley Periodicals, Inc.

  8. XRD investigation of the Effect of MgO Additives on ZTA-TiO2 Ceramic Composites

    Science.gov (United States)

    Azhar, Ahmad Zahirani Ahmad; Manshor, Hanisah; Ali, Afifah Mohd

    2018-01-01

    Alumina (Al2O3) based ceramics possess good mechanical properties and suitable for the application of cutting inserts. However, this monolithic ceramics suffer from lack of toughness. Hence, there are some modification were made such as the addition of yttria stabilized zirconia (YSZ) to the Al2O3 helps in increasing the toughness of the Al2O3 ceramics. Some additives such as MgO and TiO2 were used to further improve the mechanical properties of ZTA. In this study, high purity raw materials which consist of ZTA-TiO2 were mixed with different amount of MgO (0.0 - 1.0 wt %). The mixture of materials was going through wet mixing, compaction and pressureless sintering at 1600°C for one hour. The samples were characterized for phase analysis, microstructure, shrinkage rate, bulk density, Vickers hardness and fracture toughness. Based on the XRD analysis results, the secondary phase (MgAl2O4) was detected in the sample with 0.5 wt% of MgO onwards which leads to grains refinement, thus improve the density and hardness of ZTA-TiO2-MgO ceramics composites.

  9. Surface preparation for XRD residual stress measurements; Preparacao de superficie para medicao de tensoes residuais em soldagem por DRX

    Energy Technology Data Exchange (ETDEWEB)

    Mishchenko, Andrii; Oliveira, Bruno Jose de; Scotti, Americo, E-mail: asmwelder@gmail.com, E-mail: brunojoliveira7@gmail.com, E-mail: ascotti@mecanica.ufu.br [Universidade Federal de Uberlandia (UFU), MG (Brazil)

    2016-10-15

    A characteristic feature of the X Ray Diffraction (XRD) method for stress determination is that measurements occur at a thin surface layer. Steel sheets come with surfaces modified by lamination, cleaning (sandblasting, grinding) and even corrosion, which induce residual stresses or roughness inherent to the material. Therefore, surface preparation prior to the residual stress measurement is essential, although no standard procedure seems to be available. A general recommendation is to remove a thin layer so that only residual stresses related to the welding process will be measured. In this study, the use of portable electrolytic equipment was evaluated for mechanized surface material removal. Chemical compositions of electrolytic solutions and the influence of current on the removed material, removal time and temperature during the process were studied. As a result, a suitable chemical solution for electro etching of low carbon steel was developed and a set of “soft” parameters that allowed the removal of about 300 um in a reasonable time was found. Higher currents reduce the removal time, yet increasing the consumption of the solution and plate temperature (which could adversely alter the microstructure or generate thermal stresses). Furthermore, the influence of these parameters on the operability of the process was demonstrated. (author)

  10. Synthesis of Co/MCM-41catalysts and characterization by XRD, EDX, DTA/TG, SEM and TEM

    International Nuclear Information System (INIS)

    Sousa, B.V.; Rodrigues, M.G.F.

    2009-01-01

    Full text: In this work, molecular sieve MCM-41 was prepared as well as the Co/MCM-41 catalyst, via humid impregnation with concentration of 5 wt.% and 10 wt.% Co/MCM- 41. The attainment of the mesoporous molecular sieve, Si-MCM-41, was confirmed by the x-ray diffractogram. It was verified that after the calcination all the bromine (Br) was removed indicating that the calcination process removed all surfactant in the mesoporous structure. XRD and EDX analyses indicated that cobalt was found in the form of Co3O2 in the Co/MCM-41 catalysts. The diffraction standards showed that the impregnation and calcination processes caused changes in the structure only for catalyst with 10 wt.% Co/MCM-41. The DTA/TG curves showed that cobalt nitrate was totally decomposed on the MCM-41. From the images of SEM, it was possible to observe that the Co/MCM-41 catalysts were composed by clusters of small crystals. The images obtained from TEM showed clearly the presence of metal cobalt particles in a well dispersed form for catalyst with 5 wt.% Co/MCM41, except for the catalyst with 10 wt.% Co/MCM41. (author)

  11. Study on the Reactivity of Amino Acid Chemosensor, NPFNP, with Ethanol: Structural Elucidation through Single Crystal XRD and DFT Calculations

    Directory of Open Access Journals (Sweden)

    Beena Varghese

    2017-01-01

    Full Text Available A novel ethoxy derivative of an amino acid chemosensor, 3-naphthyl-1-phenyl-5-(2ʹ-fluoro-5ʹ-nitrophenyl-2-pyrazoline (NPFNP, has been synthesized and characterized by different spectroscopic methods.  A single crystal of the ethoxy derivative, 3-naphthyl-1-phenyl-5-(2ʹ-ethoxy-5ʹ-nitrophenyl-2-pyrazoline NPENP, has been obtained and characterized.  The structure holds interest as it carries biologically active pyrazoline as a central ring attaching to electron donating and withdrawing substituents. The major motivation for this work was to gain detailed insight into the structural parameters of this compound for investigating the influence of crystal packing and geometrical dimensions on optical properties. Time-dependent DFT calculations have been employed for comparing the XRD data with theoretical parameters. The results show that the DFT method at B3LYP/6-31G level can well reproduce the structure of the title compound.

  12. Shades of green in 15th century paintings: combined microanalysis of the materials using synchrotron radiation XRD, FTIR and XRF

    International Nuclear Information System (INIS)

    Salvado, Nati; Buti, Salvador; Cotte, Marine; Cinque, Gianfelice; Pradell, Trinitat

    2013-01-01

    A representative selection of green paintings from fifteenth century Catalonia and the Crown of Aragon are analyzed by a combination of synchrotron radiation microanalytical techniques including FTIR, XRD, and XRF. The green pigments themselves are found to be a mixture of copper acetates/basic copper acetates and basic copper chlorides. Nevertheless, a broader range of green shades were obtained by mixing the green pigment with yellow, white, and blue pigments and applied forming a sequence of micrometric layers. Besides the nature of the pigments themselves, degradation and reaction products, such as carboxylates, formates and oxalates were also identified. Some of the copper based compounds, such as the basic copper chloride, may be either part of the original pigment or a weathering product. The high resolution, high brilliance, and small footprint of synchrotron radiation proved to be essential for the analysis of those submillimetric paint layers made of a large variety of compounds heterogeneous in nature and distribution and present in extremely low concentrations. (orig.)

  13. In-situ XRD study of alloyed Cu2ZnSnSe4-CuInSe2 thin films for solar cells

    International Nuclear Information System (INIS)

    Hartnauer, Stefan; Wägele, Leonard A.; Jarzembowski, Enrico; Scheer, Roland

    2015-01-01

    We investigate the growth of Cu 2 ZnSnSe 4 -CuInSe 2 (CZTISe) thin films using a 2-stage (Cu-rich/Cu-free) co-evaporation process under simultaneous application of in-situ angle dispersive X-ray diffraction (XRD). In-situ XRD allows monitoring the phase formation during preparation. A variation of the content of indium in CZTISe leads to a change in the lattice constant. Single phase CZTISe is formed in a wide range, while at high In contents a phase separation is detected. Because of different thermal expansion coefficients, the X-ray diffraction peaks of ZnSe and CZTISe can be distinguished at elevated substrate temperatures. The formation of ZnSe appears to be inhibited even for low indium content. In-situ XRD shows no detectable sign for the formation of ZnSe. First solar cells of CZTISe have been prepared and show comparable performance to CZTSe. - Highlights: • In-situ XRD study of two-stage co-evaporated Cu 2 ZnSnSe 4 -CuInSe 2 alloyed thin films. • No detection of ZnSe with in-situ XRD due to Indium incorporation • Comparable efficiency of alloyed solar cells

  14. The comparison of the structures of some cationic forms of clinoptilolite obtained from Manisa-Gordes in Turkey using their XRD spectrums

    International Nuclear Information System (INIS)

    Izci, E.; Orhun, O.

    2000-01-01

    In this study, at room temperature, XRD spectrums of Na, Ca, Li, Pb and natural forms of clinoptilolite, which is a natural zeolite obtained from Manisa-Gordes in Turkey, were taken and compared with each other according to their structures. Firstly, clinoptilolite samples, whose, diameters are smaller than 63 μm, were purified by HCl. Thus, impurities through the channels of clinoptilolite samples, were removed from their structures. Then, the samples washed several times by deionised water and filtered. So, HCl was removed from structures of these samples. Na, Ca, Li, Pb ionic forms of clinoptilolite were prepared by using batch method. XRD apparatus from Rigaku-Rint 2000 series. Comparing of XRD spectrums of these ionic and natural forms of clinoptilolite and finding the variations of their spectrums, what changes in their structures could be, were investigated. (authors)

  15. Characterizing the Phyllosilicate Component of the Sheepbed Mudstone in Gale Crater, Mars Using Laboratory XRD and EGA

    Science.gov (United States)

    Rampe, E. B.; Morris, R. V.; Ming, D. W.; Archer, P. D.; Bish, D. L.; Chipera, S. J.; Vaniman, D. T.; Blake, D. F.; Bristow, T. F.; Sutter, B.; hide

    2014-01-01

    The Curiosity rover investigated the mineralogy of the Sheepbed mudstone member of the Yellowknife Bay formation in Gale crater. Data from the Chemistry and Mineralogy (CheMin) X-ray diffractometer (XRD) helped identify phyllosilicates in the two drilled samples, John Klein and Cumberland. These patterns showed peaks at low angles, consistent with (001) peaks in 2:1 swelling phyllosilicates [1]. Evolved gas analyses (EGA) by the Sample Analysis at Mars (SAM) instrument of these samples confirmed the presence of phyllosilicates through the release of H2O at high temperatures, consistent with dehydroxylation of octahedral OH in phyllosilicates [2]. CheMin data for the phyllosilicates at John Klein and Cumberland show that they are structurally similar in that their (02l) peaks are near 22.5 deg 2theta, suggesting both samples contain trioctahedral 2:1 phyllosilicates [1]. However, the positions of the (001) peaks differ: the phyllosilicate at John Klein has its (001) peak at 10 Angstroms, whereas the phyllosilicate at Cumberland has an (001) peak at 14 Angstroms. Such differences in (001) dspacings can be ascribed to the type of cation in the interlayer site [3]. For example, large monovalent cations (e.g., K(+)) have low hydration energies and readily lose their H2O of hydration, whereas small divalent cations (e.g., Mg(2+)) have high energies of hydration and retain H2O in the phyllosilicate interlayers [3,4]. The goal of this study is to determine whether differences in the interlayer cation composition can explain the CheMin data from John Klein and Cumberland and to use this knowledge to better understand phyllosilicate formation mechanisms.

  16. Synthesis, dynamic NMR characterization and XRD studies of novel N,N'-substituted piperazines for bioorthogonal labeling.

    Science.gov (United States)

    Mamat, Constantin; Pretze, Marc; Gott, Matthew; Köckerling, Martin

    2016-01-01

    Novel, functionalized piperazine derivatives were successfully synthesized and fully characterized by 1 H/ 13 C/ 19 F NMR, MS, elemental analysis and lipophilicity. All piperazine compounds occur as conformers resulting from the partial amide double bond. Furthermore, a second conformational shape was observed for all nitro derivatives due to the limited change of the piperazine chair conformation. Therefore, two coalescence points were determined and their resulting activation energy barriers were calculated using 1 H NMR. To support this result, single crystals of 1-(4-nitrobenzoyl)piperazine ( 3a , monoclinic, space group C 2/ c , a = 24.587(2), b = 7.0726(6), c = 14.171(1) Å, β = 119.257(8)°, V = 2149.9(4) Å 3 , Z = 4, D obs = 1.454 g/cm 3 ) and the alkyne derivative 4-(but-3-yn-1-yl)-1-(4-fluorobenzoyl)piperazine ( 4b , monoclinic, space group P 2 1 / n , a = 10.5982(2), b = 8.4705(1), c = 14.8929(3) Å, β = 97.430(1)°, V = 1325.74(4) Å 3 , Z = 4, D obs = 1.304 g/cm 3 ) were obtained from a saturated ethyl acetate solution. The rotational conformation of these compounds was also verified by XRD. As proof of concept for future labeling purposes, both nitropiperazines were reacted with [ 18 F]F - . To test the applicability of these compounds as possible 18 F-building blocks, two biomolecules were modified and chosen for conjugation either using the Huisgen-click reaction or the traceless Staudinger ligation.

  17. Transformation of meta-stable calcium silicate hydrates to tobermorite: reaction kinetics and molecular structure from XRD and NMR spectroscopy

    Science.gov (United States)

    2009-01-01

    Understanding the integrity of well-bore systems that are lined with Portland-based cements is critical to the successful storage of sequestered CO2 in gas and oil reservoirs. As a first step, we investigate reaction rates and mechanistic pathways for cement mineral growth in the absence of CO2 by coupling water chemistry with XRD and NMR spectroscopic data. We find that semi-crystalline calcium (alumino-)silicate hydrate (Al-CSH) forms as a precursor solid to the cement mineral tobermorite. Rate constants for tobermorite growth were found to be k = 0.6 (± 0.1) × 10-5 s-1 for a solution:solid of 10:1 and 1.6 (± 0.8) × 10-4 s-1 for a solution:solid of 5:1 (batch mode; T = 150°C). This data indicates that reaction rates for tobermorite growth are faster when the solution volume is reduced by half, suggesting that rates are dependent on solution saturation and that the Gibbs free energy is the reaction driver. However, calculated solution saturation indexes for Al-CSH and tobermorite differ by less than one log unit, which is within the measured uncertainty. Based on this data, we consider both heterogeneous nucleation as the thermodynamic driver and internal restructuring as possible mechanistic pathways for growth. We also use NMR spectroscopy to characterize the site symmetry and bonding environment of Al and Si in a reacted tobermorite sample. We find two [4]Al coordination structures at δiso = 59.9 ppm and 66.3 ppm with quadrupolar product parameters (PQ) of 0.21 MHz and 0.10 MHz (± 0.08) from 27Al 3Q-MAS NMR and speculate on the Al occupancy of framework sites by probing the protonation environment of Al metal centers using 27Al{1H}CP-MAS NMR. PMID:19144195

  18. Bone matrix calcification during embryonic and postembryonic rat calvarial development assessed by SEM-EDX spectroscopy, XRD, and FTIR spectroscopy.

    Science.gov (United States)

    Henmi, Akiko; Okata, Hiroshi; Anada, Takahisa; Yoshinari, Mariko; Mikami, Yasuto; Suzuki, Osamu; Sasano, Yasuyuki

    2016-01-01

    Bone mineral is constituted of biological hydroxyapatite crystals. In developing bone, the mineral crystal matures and the Ca/P ratio increases. However, how an increase in the Ca/P ratio is involved in maturation of the crystal is not known. The relationships among organic components and mineral changes are also unclear. The study was designed to investigate the process of calcification during rat calvarial bone development. Calcification was evaluated by analyzing the atomic distribution and concentration of Ca, P, and C with scanning electron microscopy (SEM)-energy-dispersive X-ray (EDX) spectroscopy and changes in the crystal structure with X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Histological analysis showed that rat calvarial bone formation started around embryonic day 16. The areas of Ca and P expanded, matching the region of the developing bone matrix, whereas the area of C became localized around bone. X-ray diffraction and FTIR analysis showed that the amorphous-like structure of the minerals at embryonic day 16 gradually transformed into poorly crystalline hydroxyapatite, whereas the proportion of mineral to protein increased until postnatal week 6. FTIR analysis also showed that crystallization of hydroxyapatite started around embryonic day 20, by which time SEM-EDX spectroscopy showed that the Ca/P ratio had increased and the C/Ca and C/P ratios had decreased significantly. The study suggests that the Ca/P molar ratio increases and the proportion of organic components such as proteins of the bone matrix decreases during the early stage of calcification, whereas crystal maturation continues throughout embryonic and postembryonic bone development.

  19. Investigations into the Surface Strain/Stress State in a Single-Crystal Superalloy via XRD Characterization

    Directory of Open Access Journals (Sweden)

    Haodong Duan

    2018-05-01

    Full Text Available The present study was aimed at determining the surface strain/stress state in an Ni-based single-crystal (SC superalloy that was subjected to two different cooling rates from solid solution temperature through using the X-ray diffraction (XRD method. The normal stresses σ 11 s and σ 22 s were determined, then the Von Mises stresses ( σ V M s were derived from them. Field emission gun scanning electron microscope (FEG-SEM and transmission electron microscope (TEM micrographs were taken to illustrate the strain/stress state change. The precipitation of the secondary γ′ phases in the γ phase and the formation of the dislocation in the interphase upon a slower cooling rate caused the γ phase lattice distortion to increase, so a larger σ V M s of the γ phase was realized in comparison to the faster cooling sample. For both of the two cooling modes, we found that the σ V M s of the γ′ phase increased due to the growth of the γ′ phase during the aging process. Also, the aging process led to pronouncedly anisotropic lattice mismatches in the {331} and {004} planes. In addition, the surface strain/stress states of a cylinder sample and a tetragonal sample were also studied using a faster cooling rate, and σ 11 s and σ 22 s were analyzed to explain the influence of the shape factor on the stress anisotropy in the [001] and [ 1 1 ¯ 0 ] orientations. The strain in the [001] orientation of the γ phase is more sensitive to the shape change.

  20. Following the Formation of Active Co(III) Sites in Cobalt Substituted Aluminophosphates Catalysts by In-Situ Combined UV-VIS/XAFS/XRD Technique

    International Nuclear Information System (INIS)

    Sankar, Gopinathan; Fiddy, Steven; Harvey, Ian; Hayama, Shusaku; Bushnell-Wye, Graham; Beale, Andrew M.

    2007-01-01

    Cobalt substituted aluminophosphates, CoAlPO-34 (Chabazite structure) and DAF-8 (Phillipsite structure) were investigated by in situ combined XRD/EXAFS/UV-VIS technique. In-situ combined XRD, Co K-edge EXAFS and UV-Vis measurements carried out during the calcination process reveal that CoAlPO-34 containing 10 wt percent cobalt is stable and the cobalt ions are converted from Co(II) in the as synthesised form to Co(III); DAF-8 containing about 25 percent cobalt is not stable and does not show change in oxidation state

  1. Location of rare-earth dopants on LiCAF and LiSAF laser hosts via XRD, EXAFS and computer modeling technique

    International Nuclear Information System (INIS)

    Valerio, Mario Ernesto Giroldo; Amaral, Jomar Batista de; Baldochi, Sonia Licia Vera; Mazzocchi, L.; Sasaki, Jose Marcos; Jackson, Robert A.

    2004-01-01

    Full text: Cr-doped LiCaAlF 6 (LiCAF) and LiSrAlF 6 (LiSAF) were used as laser operating in the near infrared region. Ce-doped LiCAF and LiSAF have been reported as leading candidates for tunable all-solid-state lasers in the UV region. Spectroscopic properties of LiCaAlF 6 : Nd suggest that this crystal can be used as selective optical filter and refractive element for 157 nm photolithography. The question of whether the RE dopant will prefer the Li + , the M 2+ site or the Al 3+ site is not yet known. Nevertheless most of the optical properties of these hosts including their laser action depend on the local symmetry, charge compensation mechanism and possible deformation of the lattice. In the present work, Powder X-ray Diffraction (XRD), X-ray Absorption Spectroscopy (XAS), Spectro fluorimetry, combined with computer modeling, were used to study the local structure around the dopant and determine the site occupied by them and also the distance and nature of the co-ordinating atoms. The compounds were prepared from commercially available CaF2 and SrF2 powders of high purity; LiF previously purified by the zone melting method, and AlF3 and RE dopants obtained from the hydro fluorination of commercial Al 2 O 3 . The synthesis of 2 mol % RE doped LiCAF and LiSAF samples were performed in a platinum reactor. The compositions were 2 mol % LiF and AlF3 enriched to compensate for their high vaporization. Powder XRD measurements were performed at room temperature in a Rigaku DMAX diffractometer in step scan mode using Cu K radiation. The Rietveld method (DBWS-9807a software) was employed in the analysis of the patterns. It was found that in the doped samples the concentration of the LiCAF or LiSAF phases are 84-95% and a small amount of AlF 3 and α - Li 3 AlF 6 were formed. The XAS experiments were performed on and above the L III absorption edge of the Er, Ho and Nd ions in fluorescence and transmission mode at room temperature in the XAS station at the LNLS, Campinas

  2. Corrosion of non-irradiated UAl{sub x}-Al fuel in the presence of clay pore solution. A quantitative XRD secondary phase analysis applying the DDM method

    Energy Technology Data Exchange (ETDEWEB)

    Neumann, Andreas [Halle-Wittenberg Univ. (Germany). Dept. of Mineralogy and Geochemistry; RWTH Aachen Univ. (Germany). Inst. of Crystallography; Klinkenberg, Martina; Curtius, Hildegard [Forschungszentrum Juelich GmbH (Germany). Inst. of Energy and Climate Research, IEK-6 Nuclear Waste Management

    2017-04-01

    Corrosion experiments with non-irradiated metallic UAl{sub x}-Al research reactor fuel elements were carried out in autoclaves to identify and quantify the corrosion products. Such compounds, considering the long-term safety assessment of final repositories, can interact with the released inventory and this constitutes a sink for radionuclide migration in formation waters. Therefore, the metallic fuel sample was subjected to clay pore solution to investigate its process of disintegration by analyzing the resulting products and the remnants, i.e. the secondary phases. Due to the fast corrosion rate a full sample disintegration was observed within the experimental period of 1 year at 90 C. The obtained solids were subdivided into different grain size fractions and prepared for analysis. The elemental analysis of the suspension showed that, uranium and aluminum are concentrated in the solids, whereas iron was mainly dissolved. Non-ambient X-ray diffraction (XRD) combined with the derivative difference minimization (DDM) method was applied for the qualitative and quantitative phase analysis (QPA) of the secondary phases. Gypsum and hemihydrate (bassanite), residues of non-corroded nuclear fuel, hematite, and goethite were identified. The quantitative phase analysis showed that goethite is the major crystalline phase. The amorphous content exceeded 80 wt% and hosted the uranium. All other compounds were present to a minor content. The obtained results by XRD were well supported by complementary scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) analysis.

  3. Design and development of the helicity injection system in Versatile Experiment Spherical Torus

    International Nuclear Information System (INIS)

    Park, JongYoon; An, Younghwa; Jung, Bongki; Lee, Jeongwon; Lee, HyunYoung; Chung, Kyoung-Jae; Na, Yong-Su; Hwang, Y.S.

    2015-01-01

    Graphical abstract: - Highlights: • A high current electron gun with single pulse power for both arc and extraction is developed. • The optimal gun operation is confirmed by impedance matching between the PFN and plasma. • The gun injected currents of 0.95 kA with the voltage of ∼410 V for 5 ms with a 1.2 kV PFN. • The helicity injection system using the gun has been developed and tested successfully in VEST. • Toroidal currents of up to 3.8 kA confirm possible relaxation into tokamak-like plasma. - Abstract: A helicity injection system for the Versatile Experiment Spherical Torus (VEST) has been successfully developed and commissioned. A high current electron gun utilizing hollow cathode and washer stacks has been designed and constructed with a single pulse power system that can provide voltages for both arc discharge and extraction sequentially. Tests for electron gun operation with the single pulse power system have been conducted under various toroidal and poloidal field strengths. The estimated plasma impedance, depending on the injection magnetic field structure, can be utilized for the optimal gun operation by impedance matching between the pulse power system and plasma. With the charging voltage of 1.2 kV, injection current of 0.95 kA has been obtained with the injection voltage of 410 V for about 5 ms. Initial helicity injection experiments have been conducted under various toroidal and poloidal field strengths and a toroidal plasma current of up to 3.8 kA is observed with the current multiplication larger than the geometric stacking ratio, confirming the possibility of relaxation into tokamak-like plasma with closed flux formation.

  4. Design and development of the helicity injection system in Versatile Experiment Spherical Torus

    Energy Technology Data Exchange (ETDEWEB)

    Park, JongYoon; An, Younghwa; Jung, Bongki; Lee, Jeongwon; Lee, HyunYoung; Chung, Kyoung-Jae; Na, Yong-Su; Hwang, Y.S., E-mail: yhwang@snu.ac.kr

    2015-10-15

    Graphical abstract: - Highlights: • A high current electron gun with single pulse power for both arc and extraction is developed. • The optimal gun operation is confirmed by impedance matching between the PFN and plasma. • The gun injected currents of 0.95 kA with the voltage of ∼410 V for 5 ms with a 1.2 kV PFN. • The helicity injection system using the gun has been developed and tested successfully in VEST. • Toroidal currents of up to 3.8 kA confirm possible relaxation into tokamak-like plasma. - Abstract: A helicity injection system for the Versatile Experiment Spherical Torus (VEST) has been successfully developed and commissioned. A high current electron gun utilizing hollow cathode and washer stacks has been designed and constructed with a single pulse power system that can provide voltages for both arc discharge and extraction sequentially. Tests for electron gun operation with the single pulse power system have been conducted under various toroidal and poloidal field strengths. The estimated plasma impedance, depending on the injection magnetic field structure, can be utilized for the optimal gun operation by impedance matching between the pulse power system and plasma. With the charging voltage of 1.2 kV, injection current of 0.95 kA has been obtained with the injection voltage of 410 V for about 5 ms. Initial helicity injection experiments have been conducted under various toroidal and poloidal field strengths and a toroidal plasma current of up to 3.8 kA is observed with the current multiplication larger than the geometric stacking ratio, confirming the possibility of relaxation into tokamak-like plasma with closed flux formation.

  5. Combining µXANES and µXRD mapping to analyse the heterogeneity in calcium carbonate granules excreted by the earthworm Lumbricus terrestris

    International Nuclear Information System (INIS)

    Brinza, Loredana; Schofield, Paul F.; Hodson, Mark E.; Weller, Sophie; Ignatyev, Konstantin; Geraki, Kalotina; Quinn, Paul D.; Mosselmans, J. Frederick W.

    2014-01-01

    A new experimental set-up enabling microfocus fluorescence XANES mapping and microfocus XRD mapping on the same sample at beamline I18 at Diamond Light Source is described. To demonstrate this set-up the heterogeneous mineralogy in calcium carbonate granules excreted by the earthworm Lumbricus terrestris has been analysed. Data analysis methods have been developed which enable µXRD and µXANES two-dimensional maps to be compared. The use of fluorescence full spectral micro-X-ray absorption near-edge structure (µXANES) mapping is becoming more widespread in the hard energy regime. This experimental method using the Ca K-edge combined with micro-X-ray diffraction (µXRD) mapping of the same sample has been enabled on beamline I18 at Diamond Light Source. This combined approach has been used to probe both long- and short-range order in calcium carbonate granules produced by the earthworm Lumbricus terrestris. In granules produced by earthworms cultured in a control artificial soil, calcite and vaterite are observed in the granules. However, granules produced by earthworms cultivated in the same artificial soil amended with 500 p.p.m. Mg also contain an aragonite. The two techniques, µXRD and µXANES, probe different sample volumes but there is good agreement in the phase maps produced

  6. Combined XRD and XANES studies of a Re-promoted Co/γ-Al2O3 catalyst at Fischer–Tropsch synthesis conditions

    DEFF Research Database (Denmark)

    Rønning, Magnus; Tsakoumis, Nikolaos E.; Voronov, Alexey

    2010-01-01

    A cobalt based Fischer–Tropsch catalyst was studied during the initial stages of the reaction at industrially relevant conditions. The catalyst consists of 20wt% cobalt supported on γ-Al2O3 and promoted by 1wt% of rhenium. X-ray diffraction (XRD) in combination with X-ray absorption near edge...

  7. Use of an Ultrasonic/Sonic Driller/Corer to Obtain Sample Powder for CHEMIN, a Combined XRD/XRF Instrument

    Science.gov (United States)

    Chipera, S. J.; Bish, D. L.; Vaniman, D. T.; Sherrit, S.; Bar-Cohen, Y.; Sarrazin, P.; Blake, D. F.

    2003-01-01

    A miniature CHEMIN XRD/XRF (X-Ray Diffraction/X-Ray Fluourescence) instrument is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed in order to enable XRD analysis on an extraterrestrial body is how best to obtain a representative sample powder for analysis. For XRD powder diffraction analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a 2-dimensional detector as used in the CHEMIN instrument will produce good results with poorly prepared powders, the quality of the data will improve if the sample is fine-grained and randomly oriented. An Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL is an effective mechanism of sampling rock to produce cores and powdered cuttings. It requires low axial load (XRD/XRF spectrometer such as CHEMIN, powders obtained from the JPL ultrasonic drill were analyzed and the results were compared to carefully prepared powders obtained using a laboratory bench scale Retsch mill.

  8. Sol-gel route of synthesis of nanoparticles of MgFe2O4 and XRD, FTIR and VSM study

    International Nuclear Information System (INIS)

    Pradeep, A.; Priyadharsini, P.; Chandrasekaran, G.

    2008-01-01

    Nanoparticles of MgFe 2 O 4 are synthesized using sol-gel autocombustion method. Structural studies are carried out using X-ray diffraction (XRD). The XRD pattern of MgFe 2 O 4 provides information about single-phase formation of spinel structure with cubic symmetry. The grain size and lattice constant are obtained using XRD data. The cation distribution is also proposed theoretically. The change in site preference of cations in nano-MgFe 2 O 4 is compared with its bulk counterpart. The structural morphology of the nanoparticles is studied using Scanning Electron Microscopy (SEM). Formation of spinel structure is conformed using Fourier transform infrared spectroscopy (FTIR), which also lends support for the cation distribution proposed using XRD data. The effect of nanoregime on parameters such as bond length, vibration frequency and force constant are discussed with the help of FTIR data. The M-H loop of MgFe 2 O 4 has been traced using the Vibrating Sample Magnetometer (VSM) and magnetic parameters such as saturation magnetization (M S ), coercivity (H C ) and retentivity (M R ) are obtained from VSM data

  9. Identification of a deleterious phase in photocatalyst based on Cd1 - xZnxS/Zn(OH)2 by simulated XRD patterns.

    Science.gov (United States)

    Cherepanova, Svetlana; Markovskaya, Dina; Kozlova, Ekaterina

    2017-06-01

    The X-ray diffraction (XRD) pattern of a deleterious phase in the photocatalyst based on Cd 1 - x Zn x S/Zn(OH) 2 contains two relatively intense asymmetric peaks with d-spacings of 2.72 and 1.56 Å. Very small diffraction peaks with interplanar distances of (d) ≃ 8.01, 5.40, 4.09, 3.15, 2.49 and 1.35 Å are characteristic of this phase but not always observed. To identify this phase, the XRD patterns for sheet-like hydroxide β-Zn(OH) 2 and sheet-like hydrozincite Zn 5 (CO 3 ) 2 (OH) 6 as well as for turbostratic hydrozincite were simulated. It is shown that the XRD pattern calculated on the basis of the last model gives the best correspondence with experimental data. Distances between layers in the turbostratically disordered hydrozincite fluctuate around d ≃ 8.01 Å. This average layer-to-layer distance is significantly higher than the interlayer distance 6.77 Å in the ordered Zn 5 (CO 3 ) 2 (OH) 6 probably due to a deficiency of CO 3 2- anions, excess OH - and the presence of water molecules in the interlayers. It is shown by variable-temperature XRD and thermogravimetric analysis (TGA) that the nanocrystalline turbostratic nonstoichiometric hydrozincite-like phase is quite thermostable. It decomposes into ZnO in air above 473 K.

  10. Cooperative use of VCD and XRD for the determination of tetrahydrobenzoisoquinolines absolute configuration: a reliable proof of memory of chirality and retention of configuration in enediyne rearrangements.

    Science.gov (United States)

    Mondal, Shovan; Naubron, Jean-Valère; Campolo, Damien; Giorgi, Michel; Bertrand, Michéle P; Nechab, Malek

    2013-12-01

    The absolute configurations (AC) of azaheterocylic compounds resulting from the cascade rearrangement of enediynes involving only light atoms were unambiguously assigned by the joint use of vibrational circular dichroism (VCD) and copper radiation single crystal X-ray diffraction (XRD). These AC determinations proved that the rearrangements of enediynes proceeded with memory of chirality and retention of configuration. © 2013 Wiley Periodicals, Inc.

  11. XRD, DRS, and SEM stundies of the effects of metal dopants (Pt and Au) on the structural and optical properties of TiO2

    CSIR Research Space (South Africa)

    Moloantoa, JR

    2011-07-01

    Full Text Available Au and Pt doped TiO2 nanocrystlas were prepared using the sol gel method. Diffuse Reflectance Spectroscopy (DRS) was used to study the characteristics of these precious metals and X-ray diffraction (XRD) with calculated lattice parameters was used...

  12. Combining µXANES and µXRD mapping to analyse the heterogeneity in calcium carbonate granules excreted by the earthworm Lumbricus terrestris

    Energy Technology Data Exchange (ETDEWEB)

    Brinza, Loredana [Diamond Light Source, Harwell Campus, Didcot, Oxon OX11 0DE (United Kingdom); Schofield, Paul F. [Natural History Museum, Cromwell Road, London SW7 5BD (United Kingdom); Hodson, Mark E. [University of York, York YO10 5DD (United Kingdom); Weller, Sophie [University of Oxford, South Parks Road, Oxford OX1 3QR (United Kingdom); Ignatyev, Konstantin; Geraki, Kalotina; Quinn, Paul D.; Mosselmans, J. Frederick W., E-mail: fred.mosselmans@diamond.ac.uk [Diamond Light Source, Harwell Campus, Didcot, Oxon OX11 0DE (United Kingdom)

    2014-01-01

    A new experimental set-up enabling microfocus fluorescence XANES mapping and microfocus XRD mapping on the same sample at beamline I18 at Diamond Light Source is described. To demonstrate this set-up the heterogeneous mineralogy in calcium carbonate granules excreted by the earthworm Lumbricus terrestris has been analysed. Data analysis methods have been developed which enable µXRD and µXANES two-dimensional maps to be compared. The use of fluorescence full spectral micro-X-ray absorption near-edge structure (µXANES) mapping is becoming more widespread in the hard energy regime. This experimental method using the Ca K-edge combined with micro-X-ray diffraction (µXRD) mapping of the same sample has been enabled on beamline I18 at Diamond Light Source. This combined approach has been used to probe both long- and short-range order in calcium carbonate granules produced by the earthworm Lumbricus terrestris. In granules produced by earthworms cultured in a control artificial soil, calcite and vaterite are observed in the granules. However, granules produced by earthworms cultivated in the same artificial soil amended with 500 p.p.m. Mg also contain an aragonite. The two techniques, µXRD and µXANES, probe different sample volumes but there is good agreement in the phase maps produced.

  13. Characterization of ceramics from the archaeological site of San Miguel Ixtapan, Mexico State, Mexico, using NAA, SEM, XRD and PIXE techniques

    International Nuclear Information System (INIS)

    Tenorio, D.; Monroy-Guzman, F.; Longoria, L.C.; Almazan-Torres, M.G.; Universidad Autonoma del Estado de Mexico, Toluca; Rodriguez-Garcia, N.L.

    2005-01-01

    Ceramic samples found in San Miguel Ixtapan, Mexico State, Mexico, were analyzed by means of NAA, PIXE, SEM and XRD. Statistical treatments such as bivariate cluster and principal-components analysis were applied to the data set. The origins of these ceramic samples were classified as local, regional and foreign. (author)

  14. In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6

    Czech Academy of Sciences Publication Activity Database

    Morris, S. A.; Bignami, G. P. M.; Tian, Y.; Navarro, M.; Firth, D. S.; Čejka, Jiří; Wheatley, P. S.; Dawson, D. M.; Slawinski, W. A.; Wragg, D. S.; Morris, R. E.; Ashbrook, S. E.

    2017-01-01

    Roč. 9, č. 10 (2017), s. 1012-1018 ISSN 1755-4330 R&D Projects: GA ČR GBP106/12/G015 Institutional support: RVO:61388955 Keywords : NMR * XRD * ADOR process Subject RIV: CF - Physical ; Theoretical Chemistry OBOR OECD: Physical chemistry Impact factor: 25.870, year: 2016

  15. XRD measurement of mean crystallite thickness of illite and illite/smectite: Reappraisal of the Kubler index and the Scherrer equation

    Science.gov (United States)

    Drits, Victor A.; Środoń, Jan; Eberl, D.D.

    1997-01-01

    The standard form of the Scherrer equation, which has been used to calculate the mean thickness of the coherent scattering domain (CSD) of illite crystals from X-ray diffraction (XRD) full width data at half maximum (FWHM) intensity, employs a constant, Ksh, of 0.89. Use of this constant is unjustified, even if swelling has no effect on peak broadening, because this constant is valid only if all CSDs have a single thickness. For different thickness distributions, the Scherrer “constant” has very different values.Analysis of fundamental particle thickness data (transmission electron microscopy, TEM) for samples of authigenic illite and illite/smectite from diagenetically altered pyroclastics and filamentous illites from sandstones reveals a unique family of lognormal thickness distributions for these clays. Experimental relations between the distributions' lognormal parameters and mean thicknesses are established. These relations then are used to calculate the mean thickness of CSDs for illitic samples from XRD FWHM, or from integral XRD peak widths (integrated intensity/maximum intensity).For mixed-layer illite/smectite, the measured thickness of the CSD corresponds to the mean thickness of the mixed-layer crystal. Using this measurement, the mean thickness of the fundamental particles that compose the mixed-layer crystals can be calculated after XRD determination of percent smectitic interlayers. The effect of mixed layering (swelling) on XRD peak width for these samples is eliminated by using the 003 reflection for glycolated samples, and the 001, 002 or 003 reflection for dehydrated, K-saturated samples. If this technique is applied to the 001 reflection of air-dried samples (Kubler index measurement), mean CSD thicknesses are underestimated due to the mixed-layering effect.The technique was calibrated using NEW MOD©-simulated XRD profiles of illite, and then tested on well-characterized illite and illite/smectite samples. The XRD measurements are in good

  16. XRD measurement of mean thickness, thickness distribution and strain for illite and illite-smectite crystallites by the Bertaut-Warren-Averbach technique

    Science.gov (United States)

    Drits, Victor A.; Eberl, Dennis D.; Środoń, Jan

    1998-01-01

    A modified version of the Bertaut-Warren-Averbach (BWA) technique (Bertaut 1949, 1950; Warren and Averbach 1950) has been developed to measure coherent scattering domain (CSD) sizes and strains in minerals by analysis of X-ray diffraction (XRD) data. This method is used to measure CSD thickness distributions for calculated and experimental XRD patterns of illites and illite-smectites (I-S). The method almost exactly recovers CSD thickness distributions for calculated illite XRD patterns. Natural I-S samples contain swelling layers that lead to nonperiodic structures in the c* direction and to XRD peaks that are broadened and made asymmetric by mixed layering. Therefore, these peaks cannot be analyzed by the BWA method. These difficulties are overcome by K-saturation and heating prior to X-ray analysis in order to form 10-Å periodic structures. BWA analysis yields the thickness distribution of mixed-layer crystals (coherently diffracting stacks of fundamental illite particles). For most I-S samples, CSD thickness distributions can be approximated by lognormal functions. Mixed-layer crystal mean thickness and expandability then can be used to calculate fundamental illite particle mean thickness. Analyses of the dehydrated, K-saturated samples indicate that basal XRD reflections are broadened by symmetrical strain that may be related to local variations in smectite interlayers caused by dehydration, and that the standard deviation of the strain increases regularly with expandability. The 001 and 002 reflections are affected only slightly by this strain and therefore are suited for CSD thickness analysis. Mean mixed-layer crystal thicknesses for dehydrated I-S measured by the BWA method are very close to those measured by an integral peak width method.

  17. Nanostructured synthetic hydroxyapatite and dental enamel heated and irradiated by ER,CR:YSGG: characterized by FTIR and XRD

    International Nuclear Information System (INIS)

    Rabelo Neto, Jose da Silva

    2009-01-01

    The study evaluate the physical changes and/or chemical that occurs in synthetic hydroxyapatite (HAP) and in enamel under action of thermal heating in oven or laser irradiation of Er,Cr:YSGG that may cause changes in its structure to make them more resistant to demineralization aiming the formation of dental caries. The synthetic HAP was produced by reaction of solutions of Ca(NO 3 ) and (NH 4 ) 2 HPO 4 with controlled temperature and pH. The enamel powder was collected from the bovine teeth. Samples of powder enamel and synthetic HAP were subjected to thermal heating in oven at temperatures of 200 deg C, 400 deg C, 600 deg C, 800 deg C and 1000 deg C. For the laser irradiation of materials, were made with 5,79 J/cm 2 of irradiation, 7,65 J/cm 2 , 10,55 J/cm 2 and 13,84 J/cm 2 for synthetic HAP and 7,53 J/cm 2 , 10,95 J/cm 2 , and 13,74 J/cm 2 for the enamel. The samples were evaluated by X-ray diffraction (XRD) for analysis of crystallographic phases and analysis by the Rietveld method, to determine their respective proportions in the material, as well as results of changes of the lattice unit cell parameters (axis-a, axis-c and volume), crystallites sizes and the occupation rate of sites of Ca and P atoms. The samples were analyzed by Fourier transform infrared spectroscopy (FTIR), which should compositional changes due to treatment related to carbonate, phosphate, adsorbed water and hydroxyl radicals content. The infrared was used to measure the surface temperature generated by the laser beam in the solid samples of enamel. Besides the major hydroxyapatite crystallographic phases, there was formations of octa calcium phosphate (OCP) and phase β of tricalcium phosphate (β-TCP ) in enamel heated at 800 deg C. There was reduction of the axis-a, volume and size of crystallites to the temperatures between 400 degree C and 600 deg C and also on laser irradiated samples. Above the temperature of 600 degree C it is observed the effect in the lattice parameters. The Ca

  18. Combining µXANES and µXRD mapping to analyse the heterogeneity in calcium carbonate granules excreted by the earthworm Lumbricus terrestris.

    Science.gov (United States)

    Brinza, Loredana; Schofield, Paul F; Hodson, Mark E; Weller, Sophie; Ignatyev, Konstantin; Geraki, Kalotina; Quinn, Paul D; Mosselmans, J Frederick W

    2014-01-01

    The use of fluorescence full spectral micro-X-ray absorption near-edge structure (µXANES) mapping is becoming more widespread in the hard energy regime. This experimental method using the Ca K-edge combined with micro-X-ray diffraction (µXRD) mapping of the same sample has been enabled on beamline I18 at Diamond Light Source. This combined approach has been used to probe both long- and short-range order in calcium carbonate granules produced by the earthworm Lumbricus terrestris. In granules produced by earthworms cultured in a control artificial soil, calcite and vaterite are observed in the granules. However, granules produced by earthworms cultivated in the same artificial soil amended with 500 p.p.m. Mg also contain an aragonite. The two techniques, µXRD and µXANES, probe different sample volumes but there is good agreement in the phase maps produced.

  19. Multiscale structural characterizations of mixed U(iv)-An(iii) oxalates (An(iii) = Pu or Am) combining XAS and XRD measurements.

    Science.gov (United States)

    Arab-Chapelet, B; Martin, P M; Costenoble, S; Delahaye, T; Scheinost, A C; Grandjean, S; Abraham, F

    2016-04-28

    Mixed actinide(III,IV) oxalates of the general formula M2.2UAn(C2O4)5·nH2O (An = Pu or Am and M = H3O(+) and N2H5(+)) have been quantitatively precipitated by oxalic precipitation in nitric acid medium (yield >99%). Thorough multiscale structural characterization using XRD and XAS measurements confirmed the existence of mixed actinide oxalate solid solutions. The XANES analysis confirmed that the oxidation states of the metallic cations, tetravalent for uranium and trivalent for plutonium and americium, are maintained during the precipitation step. EXAFS measurements show that the local environments around U(+IV), Pu(+III) and Am(+III) are comparable, and the actinides are surrounded by ten oxygen atoms from five bidentate oxalate anions. The mean metal-oxygen distances obtained by XAS measurements are in agreement with those calculated from XRD lattice parameters.

  20. Thermal dehydration of cobalt and zinc formate dihydrates by controlled-rate thermogravimetry (CRTG) and simultaneous X-ray diffractometry-differential scanning calorimetry (XRD-DSC)

    International Nuclear Information System (INIS)

    Arii, T.; Kishi, A.

    1999-01-01

    The thermal dehydration study of the similar hydrated salts, cobalt and zinc formate dihydrates, have been carried out successfully by means of X-ray diffractometry-differential scanning calorimetry (XRD-DSC) and controlled-rate thermogravimetry (CRTG). X-ray diffraction analysis recorded simultaneously indicates that the resulting anhydrous product, Zn(HCO 2 ) 2 , was crystalline, while Co(HCO 2 ) 2 was amorphous.The XRD-DSC data are proven to be invaluable in verifying the interpretation of overlapping processes in thermal events. In addition, these differences in the resulting anhydrous products can be explained from kinetic analysis results based on the CRTG data. The kinetic mechanism governing the dehydration of zinc formate dihydrate is a nucleation and growth process, while in the case of cobalt formate dihydrate a phase boundary controlled reaction is the governing mechanism. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  1. Leonardo da Vinci's drapery studies: characterization of lead white pigments by μ-XRD and 2D scanning XRF

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez, Victor; Calligaro, Thomas [Centre de Recherche et de Restauration des Musees de France, C2RMF, Paris (France); PSL Research University, Chimie ParisTech-CNRS, Institut de Recherche de Chimie Paris, UMR8247, Paris (France); Pichon, Laurent; Mottin, Bruno [Centre de Recherche et de Restauration des Musees de France, C2RMF, Paris (France); Wallez, Gilles [PSL Research University, Chimie ParisTech-CNRS, Institut de Recherche de Chimie Paris, UMR8247, Paris (France); Sorbonne University, UPMC Univ., Paris 06 (France)

    2015-11-15

    This work focuses on the composition and microstructure of the lead white pigment employed in a set of paintworks, using a combination of μ-XRD and 2D scanning XRF, directly applied on five drapery studies attributed to Leonardo da Vinci (1452-1519) and conserved in the Departement des Arts Graphiques, Musee du Louvre and in the Musee des Beaux-Arts de Rennes. Trace elements present in the composition as well as in the lead white highlights were imaged by 2D scanning XRF. Mineral phases were determined in a fully noninvasive way using a special μ-XRD diffractometer. Phase proportions were estimated by Rietveld refinement. The analytical results obtained will contribute to differentiate lead white qualities and to highlight the artist's technique. (orig.)

  2. Leonardo da Vinci's drapery studies: characterization of lead white pigments by μ-XRD and 2D scanning XRF

    International Nuclear Information System (INIS)

    Gonzalez, Victor; Calligaro, Thomas; Pichon, Laurent; Mottin, Bruno; Wallez, Gilles

    2015-01-01

    This work focuses on the composition and microstructure of the lead white pigment employed in a set of paintworks, using a combination of μ-XRD and 2D scanning XRF, directly applied on five drapery studies attributed to Leonardo da Vinci (1452-1519) and conserved in the Departement des Arts Graphiques, Musee du Louvre and in the Musee des Beaux-Arts de Rennes. Trace elements present in the composition as well as in the lead white highlights were imaged by 2D scanning XRF. Mineral phases were determined in a fully noninvasive way using a special μ-XRD diffractometer. Phase proportions were estimated by Rietveld refinement. The analytical results obtained will contribute to differentiate lead white qualities and to highlight the artist's technique. (orig.)

  3. Quantitative assessment of alkali-reactive aggregate mineral content through XRD using polished sections as a supplementary tool to RILEM AAR-1 (petrographic method)

    International Nuclear Information System (INIS)

    Castro, Nélia; Sorensen, Bjørn E.; Broekmans, Maarten A.T.M.

    2012-01-01

    The mineral content of 5 aggregate samples from 4 different countries, including reactive and non-reactive aggregate types, was assessed quantitatively by X-ray diffraction (XRD) using polished sections. Additionally, electron probe microanalyzer (EPMA) mapping and cathodoluminescence (CL) were used to characterize the opal-CT identified in one of the aggregate samples. Critical review of results from polished sections against traditionally powdered specimen has demonstrated that for fine-grained rocks without preferred orientation the assessment of mineral content by XRD using polished sections may represent an advantage over traditional powder specimens. Comparison of data on mineral content and silica speciation with expansion data from PARTNER project confirmed that the presence of opal-CT plays an important role in the reactivity of one of the studied aggregates. Used as a complementary tool to RILEM AAR-1, the methodology suggested in this paper has the potential to improve the strength of the petrographic method.

  4. XRF, μ-XRD and μ-spectroscopic techniques for revealing the composition and structure of paint layers on polychrome sculptures after multiple restorations.

    Science.gov (United States)

    Franquelo, M L; Duran, A; Castaing, J; Arquillo, D; Perez-Rodriguez, J L

    2012-01-30

    This paper presents the novel application of recently developed analytical techniques to the study of paint layers on sculptures that have been restored/repainted several times across centuries. Analyses were performed using portable XRF, μ-XRD and μ-Raman instruments. Other techniques, such as optical microscopy, SEM-EDX and μ-FTIR, were also used. Pigments and other materials including vermilion, minium, red lac, ivory black, lead white, barium white, zinc white (zincite), titanium white (rutile and anatase), lithopone, gold and brass were detected. Pigments from both ancient and modern times were found due to the different restorations/repaintings carried out. μ-Raman was very useful to characterise some pigments that were difficult to determine by μ-XRD. In some cases, pigments identification was only possible by combining results from the different analytical techniques used in this work. This work is the first article devoted to the study of sculpture cross-section samples using laboratory-made μ-XRD systems. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. SR-XRD in situ monitoring of copper-IUD corrosion in simulated uterine fluid using a portable spectroelectrochemical cell.

    Science.gov (United States)

    Grayburn, Rosie A; Dowsett, Mark G; Sabbe, Pieter-Jan; Wermeille, Didier; Anjos, Jorge Alves; Flexer, Victoria; De Keersmaecker, Michel; Wildermeersch, Dirk; Adriaens, Annemie

    2016-08-01

    The objective of this work is to study the initial corrosion of copper in the presence of gold when placed in simulated uterine fluid in order to better understand the evolution of active components of copper-IUDs. In order to carry out this study, a portable cell was designed to partially simulate the uterine environment and provide a way of tracking the chemical changes occurring in the samples in situ within a controlled environment over a long period of time using synchrotron spectroelectrochemistry. The dynamically forming crystalline corrosion products are determined in situ for a range of copper-gold surface ratios over the course of a 10-day experiment in the cell. It is concluded that the insoluble deposits forming over this time are not the origin of the anticonception mechanism. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Metal dioxides as analogue of SiO2 under strong compression studied by synchrotron XRD and simulations

    Science.gov (United States)

    Liu, H.; Liu, L. L.

    2017-12-01

    The phase transition sequence of SiO2 inducing by high pressure was theoretically predicted as coordination number (CN=6) structures (rutile, pyrite), CN=8 (Pnma) and CN=9 (P-62m) structures, but only the phases up to pyrite structure in SiO2 were observed experimentally up to now. The CN8 phase and CN9 phases of SiO2 were predicted to be stable at least 650 GPa, which is challenging to achieve in the static DAC experiment at present. In other metal dioxide systems, such as TiO2, the ambient rutile and anatase phases first transform to pyrite (CN6), then to the baddeleyite (CN7) phase, to a Pnma (CN8) phase and P-62m(CN9) phase. In this report, under strong compression at room temperature, several metal dioxides were studied experimentally and theoretically, to verify whether this theoretical predicted trend is common transition path under strong compression. This work was supported by Natural Science Foundation of China (11374075), Heilongjiang Province Science Fund for Distinguished Young Scholars (JC201005), Longjiang Scholar, the Fundamental Research Funds for the Central Universities (HIT. BRET1.2010002, HIT. IBRSEM.A.201403).

  7. An internally consistent pressure calibration of geobarometers applicable to the Earth’s upper mantle using in situ XRD

    Energy Technology Data Exchange (ETDEWEB)

    Beyer, Christopher; Rosenthal, Anja; Myhill, Robert; Crichton, Wilson A.; Yu, Tony; Wang, Yanbin; Frost, Daniel J.

    2018-02-01

    We have performed an experimental cross calibration of a suite of mineral equilibria within mantle rock bulk compositions that are commonly used in geobarometry to determine the equilibration depths of upper mantle assemblages. Multiple barometers were compared simultaneously in experimental runs, where the pressure was determined using in-situ measurements of the unit cell volumes of MgO, NaCl, Re and h-BN between 3.6 and 10.4 GPa, and 1250 and 1500 °C. The experiments were performed in a large volume press (LVPs) in combination with synchrotron X-ray diffraction. Noble metal capsules drilled with multiple sample chambers were loaded with a range of bulk compositions representative of peridotite, eclogite and pyroxenite lithologies. By this approach, we simultaneously calibrated the geobarometers applicable to different mantle lithologies under identical and well determined pressure and temperature conditions. We identified discrepancies between the calculated and experimental pressures for which we propose simple linear or constant correction factors to some of the previously published barometric equations. As a result, we establish internally-consistent cross-calibrations for a number of garnet-orthopyroxene, garnet-clinopyroxene, Ca-Tschermaks-in-clinopyroxene and majorite geobarometers.

  8. Use of tourmaline as a potential petrogenetic indicator in the determination of host magma: CRS, XRD and PED-XRF methods.

    Science.gov (United States)

    Gullu, Bahattin; Kadioglu, Yusuf Kagan

    2017-08-05

    Tourmaline defines a group of complex borosilicate forms as accessory mineral in igneous and metamorphic rocks and they act an important role in the interpretation of the chemical composition changes of the composition of the host fluid of the magma. The variety of tourmaline can be identified by using optical microscopy, X-Ray Diffraction (XRD) and by determining its chemical composition through Polarized Energy Dispersive X-Ray Fluorescence (PED-XRF) methods. However, microscopic investigations and XRD analyses are not quite adequate for detailed determination of tourmaline sub-groups. In addition, the use of chemical composition of tourmaline as a strict indicator of geochemical processes might be a misleading method. In this study, variable tourmaline crystals were collected from three different pegmatitic occurrences in Behrekdag, Yozgat and Karakaya granitic bodies of Central Anatolia to identify their chemical properties through Confocal Raman Spectroscopy (CRS), PED-XRF and XRD analyses. The confocal Raman spectrometry of collected tourmalines from the Behrekdag, Yozgat and Karakaya granites are in the compositions of schorl, schorl and elbaite respectively. The dominant compositional groups of these tourmalines are in the form of schorl. Raman shift values of tourmalines revealed four bands centered at almost 1050, 750, 400 and 300cm -1 . The first group of the band arises from SiO stretching, the second from BO stretching and the other two belong to bending modes of OBO and BOAl with symmetrical deformation of SiOSi. The strongest spectra near 360cm -1 should belong to the bonding of AlO. As a result, the confocal Raman studies are more sensitive for identification of tourmaline subgroup compositions and have a quite important in the explaining source of the magma. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Use of tourmaline as a potential petrogenetic indicator in the determination of host magma: CRS, XRD and PED-XRF methods

    Science.gov (United States)

    Gullu, Bahattin; Kadioglu, Yusuf Kagan

    2017-08-01

    Tourmaline defines a group of complex borosilicate forms as accessory mineral in igneous and metamorphic rocks and they act an important role in the interpretation of the chemical composition changes of the composition of the host fluid of the magma. The variety of tourmaline can be identified by using optical microscopy, X-Ray Diffraction (XRD) and by determining its chemical composition through Polarized Energy Dispersive X-Ray Fluorescence (PED-XRF) methods. However, microscopic investigations and XRD analyses are not quite adequate for detailed determination of tourmaline sub-groups. In addition, the use of chemical composition of tourmaline as a strict indicator of geochemical processes might be a misleading method. In this study, variable tourmaline crystals were collected from three different pegmatitic occurrences in Behrekdag, Yozgat and Karakaya granitic bodies of Central Anatolia to identify their chemical properties through Confocal Raman Spectroscopy (CRS), PED-XRF and XRD analyses. The confocal Raman spectrometry of collected tourmalines from the Behrekdag, Yozgat and Karakaya granites are in the compositions of schorl, schorl and elbaite respectively. The dominant compositional groups of these tourmalines are in the form of schorl. Raman shift values of tourmalines revealed four bands centered at almost 1050, 750, 400 and 300 cm- 1. The first group of the band arises from SiO stretching, the second from Bsbnd O stretching and the other two belong to bending modes of Osbnd Bsbnd O and Bsbnd Osbnd Al with symmetrical deformation of Sisbnd Osbnd Si. The strongest spectra near 360 cm- 1 should belong to the bonding of Alsbnd O. As a result, the confocal Raman studies are more sensitive for identification of tourmaline subgroup compositions and have a quite important in the explaining source of the magma.

  10. XRD and spectral dataset of the UV-A stable nanotubes of 3,5-bis(trifluoromethyl)benzylamine derivative of tyrosine.

    Science.gov (United States)

    Govindhan, R; Karthikeyan, B

    2017-10-01

    The data presented in this article are related to the research entitled of UV-A stable nanotubes. The nanotubes have been prepared from 3,5-bis(trifluoromethyl)benzylamine derivative of tyrosine (BTTP). XRD data reveals the size of the nanotubes. As-synthesized nanotubes (BTTPNTs) are characterized by UV-vis optical absorption studies [1] and photo physical degradation kinetics. The resulted dataset is made available to enable critical or extended analyzes of the BTTPNTs as an excellent light resistive materials.

  11. Effect of interparticle interactions on size determination of zirconia and silica based systems – A comparison of SAXS, DLS, BET, XRD and TEM

    Science.gov (United States)

    Pabisch, Silvia; Feichtenschlager, Bernhard; Kickelbick, Guido; Peterlik, Herwig

    2012-01-01

    The aim of this work is a systematic comparison of size characterisation methods for two completely different model systems of oxide nanoparticles, i.e. amorphous spherical silica and anisotropic facet-shaped crystalline zirconia. Size and/or size distribution were determined in a wide range from 5 to 70 nm using small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), nitrogen sorption (BET), X-ray diffraction (XRD) and transmission electron microscopy (TEM). A nearly perfect coincidence was observed only for SAXS and TEM for both types of particles. For zirconia nanoparticles considerable differences between different measurement methods were observed. PMID:22347721

  12. Isotopes for fundamental research 83mKr for KATRIN and 101Rh and 109Cd for XRD studies on planets

    International Nuclear Information System (INIS)

    Rasulbaev, Makhsud

    2011-01-01

    The feasibility of production of 83 Rb from liquid, natural Br at the Bonn Cyclotron was shown. Production of 83 Rb/ 83m Kr generators for KATRIN Collaboration was optimized. 83m Kr release from RbBr residue after the evaporation of the excess Br was studied. A possibility of 83 Rb implantation with 38 % efficiency was shown in the example of non-radioactive 85 Rb implantation. Production optimization of X-ray sources, 101 Rh and 109 Cd, for implementation in XRD analysis set-up at Technical University of Dresden was experimentally investigated at the Bonn Cyclotron. (orig.)

  13. Isotopes for fundamental research {sup 83m}Kr for KATRIN and {sup 101}Rh and {sup 109}Cd for XRD studies on planets

    Energy Technology Data Exchange (ETDEWEB)

    Rasulbaev, Makhsud

    2011-12-16

    The feasibility of production of {sup 83}Rb from liquid, natural Br at the Bonn Cyclotron was shown. Production of {sup 83}Rb/{sup 83m}Kr generators for KATRIN Collaboration was optimized. {sup 83m}Kr release from RbBr residue after the evaporation of the excess Br was studied. A possibility of {sup 83}Rb implantation with 38 % efficiency was shown in the example of non-radioactive {sup 85}Rb implantation. Production optimization of X-ray sources, {sup 101}Rh and {sup 109}Cd, for implementation in XRD analysis set-up at Technical University of Dresden was experimentally investigated at the Bonn Cyclotron. (orig.)

  14. Structural, electronic and optical properties of monoclinic Na{sub 2}Ti{sub 3}O{sub 7} from density functional theory calculations: A comparison with XRD and optical absorption measurements

    Energy Technology Data Exchange (ETDEWEB)

    Araújo-Filho, Adailton A. [Departamento de Física, Universidade Federal do Ceará, Caixa Postal 6030, 60455-760 Fortaleza, CE (Brazil); Silva, Fábio L.R.; Righi, Ariete [Departamento de Física, Universidade Federal de Minas Gerais, Belo Horizonte, MG 31270-901 (Brazil); Silva, Mauricélio B. da; Silva, Bruno P. [Departamento de Física, Universidade Federal do Ceará, Caixa Postal 6030, 60455-760 Fortaleza, CE (Brazil); Caetano, Ewerton W.S., E-mail: ewcaetano@gmail.com [Instituto Federal de Educação, Ciência e Tecnologia do Ceará, 60040-531 Fortaleza, CE (Brazil); Freire, Valder N. [Departamento de Física, Universidade Federal do Ceará, Caixa Postal 6030, 60455-760 Fortaleza, CE (Brazil)

    2017-06-15

    Powder samples of bulk monoclinic sodium trititanate Na{sub 2}Ti{sub 3}O{sub 7} were prepared carefully by solid state reaction, and its monoclinic P2{sub 1}/m crystal structure and morphology were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM), respectively. Moreover, the sodium trititanate main energy band gap was estimated as E{sub g}=3.51±0.01 eV employing UV–Vis spectroscopy, which is smaller than the measured 3.70 eV energy gap published previously by other authors. Aiming to achieve a better understanding of the experimental data, density functional theory (DFT) computations were performed within the local density and generalized gradient approximations (LDA and GGA, respectively) taking into account dispersion effects through the scheme of Tkatchenko and Scheffler (GGA+TS). Optimal lattice parameters, with deviations relative to measurements Δa=−0.06 Å, Δb=0.02 Å, and Δc=−0.09 Å, were obtained at the GGA level, which was then used to simulate the sodium trititanate electronic and optical properties. Indirect band transitions have led to a theoretical gap energy value of about 3.25 eV. Our results, however, differ from pioneer DFT results with respect to the specific Brillouin zone vectors for which the indirect transition with smallest energy value occurs. Effective masses for electrons and holes were also estimated along a set of directions in reciprocal space. Lastly, our calculations revealed a relatively large degree of optical isotropy for the Na{sub 2}Ti{sub 3}O{sub 7} optical absorption and complex dielectric function. - Graphical abstract: Monoclinic sodium trititanate Na2Ti3O7 was characterized by experiment and dispersion-corrected DFT calculations. An indirect gap of 3.5 eV is predicted, with heavy electrons and anisotropic holes ruling its conductivity. - Highlights: • Monoclinic Na2Ti3O7 was characterized by experiment (XRD, SEM, UV–Vis spectroscopy). • DFT GGA+TS optimized geometry and

  15. Effect of microwave treatment on structure of binders based on sodium carboxymethyl starch: FT-IR, FT-Raman and XRD investigations

    Science.gov (United States)

    Kaczmarska, Karolina; Grabowska, Beata; Spychaj, Tadeusz; Zdanowicz, Magdalena; Sitarz, Maciej; Bobrowski, Artur; Cukrowicz, Sylwia

    2018-06-01

    The paper deals with the influence of the microwave treatment on sodium carboxymethyl starch (CMS-Na) applied as a binder for moulding sands. The Fourier transformation infrared spectrometry (FT-IR), Raman spectroscopy (FT-Raman) and XRD analysis data of native potato starch and three different carboxymethyl starches (CMS-Na) with various degree of substitution (DS) before and after exposition to microwave radiation have been compared. FT-IR studies showed that polar groups present in CMS-Na structure take part in the formation of new hydrogen bonds network after water evaporation. However, these changes depend on DS value of the modified starch. The FT-Raman study confirmed that due to the impact on the samples by microwave, the changes of intensity in the characteristic bands associated with the crystalline regions in the sample were noticed. The X-ray diffraction data for microwave treated CMS-Na samples have been compared with the diffractograms of initial materials and analysis of XRD patterns confirmed that microwave-treated samples exhibit completely amorphous structure. Analysis of structural changes allows to state that the binding of sand grains in moulding sand with CMS-Na polymeric binder consists in the formation of hydrogen bonds networks (physical cross-linking).

  16. Synthesis, structural and vibrational investigation on 2-phenyl-N-(pyrazin-2-yl)acetamide combining XRD diffraction, FT-IR and NMR spectroscopies with DFT calculations.

    Science.gov (United States)

    Lukose, Jilu; Yohannan Panicker, C; Nayak, Prakash S; Narayana, B; Sarojini, B K; Van Alsenoy, C; Al-Saadi, Abdulaziz A

    2015-01-25

    The optimized molecular structure, vibrational frequencies, corresponding vibrational assignments of 2-phenyl-N-(pyrazin-2-yl)acetamide have been investigated experimentally and theoretically using Gaussian09 software package. The title compound was optimized by using the HF/6-31G(6D,7F) and B3LYP/6-31G(6D,7F) calculations. The geometrical parameters are in agreement with the XRD data. The stability of the molecule arising from hyper-conjugative interaction and charge delocalization has been analyzed using NBO analysis. Gauge-including atomic orbital (1)H-NMR chemical shifts calculations were carried out and compared with experimental data. The HOMO and LUMO analysis is used to determine the charge transfer within the molecule. Molecular electrostatic potential was performed by the DFT method. First hyperpolarizability is calculated in order to find its role in non linear optics. From the XRD data, in the crystal, molecules are held together by strong C-H⋯O and N-H⋯O intermolecular interactions. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. In-situ investigation of stress conditions during expansion of bare metal stents and PLLA-coated stents using the XRD sin(2)ψ-technique.

    Science.gov (United States)

    Kowalski, Wolfgang; Dammer, Markus; Bakczewitz, Frank; Schmitz, Klaus-Peter; Grabow, Niels; Kessler, Olaf

    2015-09-01

    Drug eluting stents (DES) consist of platform, coating and drug. The platform often is a balloon-expandable bare metal stent made of the CoCr alloy L-605 or stainless steel 316 L. The function of the coating, typically a permanent polymer, is to hold and release the drug, which should improve therapeutic outcome. Before implantation, DES are compressed (crimped) to allow implantation in the human body. During implantation, DES are expanded by balloon inflation. Crimping, as well as expansion, causes high stresses and high strains locally in the DES struts, as well as in the polymer coating. These stresses and strains are important design criteria of DES. Usually, they are calculated numerically by finite element analysis (FEA), but experimental results for validation are hardly available. In this work, the X-ray diffraction (XRD) sin(2)ψ-technique is applied to in-situ determination of stress conditions of bare metal L-605 stents, and Poly-(L-lactide) (PLLA) coated stents. This provides a realistic characterization of the near-surface stress state and a validation option of the numerical FEA. XRD-results from terminal stent struts of the bare metal stent show an increasing compressive load stress in tangential direction with increasing stent expansion. These findings correlate with numerical FEA results. The PLLA-coating also bears increasing compressive load stress during expansion. Copyright © 2015 Elsevier Ltd. All rights reserved.

  18. Mineralogical In-situ Investigation of Acid-Sulfate Samples from the Rio Tinto River, Spain, with a Portable XRD/XRF Instrument

    Science.gov (United States)

    Sarrazin, P.; Ming, D. W.; Morris, R. V.; Fernandez-Remolar, D.; Amils, R.; Arvidson, R. E.; Blake, D.; Bish, D. L.

    2007-01-01

    A field campaign was organized in September 2006 by Centro de Astobiologica (Spain) and Washington University (St Louis, USA) for the geological study of the Rio Tinto river bed sediments using a suite of in-situ instruments comprising an ASD reflectance spectrometer, an emission spectrometer, panoramic and close-up color imaging cameras, a life detection system and NASA's CheMin 4 XRD/XRF prototype. The primary objectives of the field campaign were to study the geology of the site and test the potential of the instrument suite in an astrobiological investigation context for future Mars surface robotic missions. The results of the overall campaign will be presented elsewhere. This paper focuses on the results of the XRD/XRF instrument deployment. The specific objectives of the CheMin 4 prototype in Rio Tinto were to 1) characterize the mineralogy of efflorescent salts in their native environments; 2) analyze the mineralogy of salts and oxides from the modern environment to terraces formed earlier as part of the Rio Tinto evaporative system; and 3) map the transition from hematite-dominated terraces to the mixed goethite/salt-bearing terraces where biosignatures are best preserved.

  19. In situ characterization of uranium and americium oxide solid solution formation for CRMP process: first combination of in situ XRD and XANES measurements.

    Science.gov (United States)

    Caisso, Marie; Picart, Sébastien; Belin, Renaud C; Lebreton, Florent; Martin, Philippe M; Dardenne, Kathy; Rothe, Jörg; Neuville, Daniel R; Delahaye, Thibaud; Ayral, André

    2015-04-14

    Transmutation of americium in heterogeneous mode through the use of U1-xAmxO2±δ ceramic pellets, also known as Americium Bearing Blankets (AmBB), has become a major research axis. Nevertheless, in order to consider future large-scale deployment, the processes involved in AmBB fabrication have to minimize fine particle dissemination, due to the presence of americium, which considerably increases the risk of contamination. New synthesis routes avoiding the use of pulverulent precursors are thus currently under development, such as the Calcined Resin Microsphere Pelletization (CRMP) process. It is based on the use of weak-acid resin (WAR) microspheres as precursors, loaded with actinide cations. After two specific calcinations under controlled atmospheres, resin microspheres are converted into oxide microspheres composed of a monophasic U1-xAmxO2±δ phase. Understanding the different mechanisms during thermal conversion, that lead to the release of organic matter and the formation of a solid solution, appear essential. By combining in situ techniques such as XRD and XAS, it has become possible to identify the key temperatures for oxide formation, and the corresponding oxidation states taken by uranium and americium during mineralization. This paper thus presents the first results on the mineralization of (U,Am) loaded resin microspheres into a solid solution, through in situ XAS analysis correlated with HT-XRD.

  20. Effect of microwave treatment on structure of binders based on sodium carboxymethyl starch: FT-IR, FT-Raman and XRD investigations.

    Science.gov (United States)

    Kaczmarska, Karolina; Grabowska, Beata; Spychaj, Tadeusz; Zdanowicz, Magdalena; Sitarz, Maciej; Bobrowski, Artur; Cukrowicz, Sylwia

    2018-06-15

    The paper deals with the influence of the microwave treatment on sodium carboxymethyl starch (CMS-Na) applied as a binder for moulding sands. The Fourier transformation infrared spectrometry (FT-IR), Raman spectroscopy (FT-Raman) and XRD analysis data of native potato starch and three different carboxymethyl starches (CMS-Na) with various degree of substitution (DS) before and after exposition to microwave radiation have been compared. FT-IR studies showed that polar groups present in CMS-Na structure take part in the formation of new hydrogen bonds network after water evaporation. However, these changes depend on DS value of the modified starch. The FT-Raman study confirmed that due to the impact on the samples by microwave, the changes of intensity in the characteristic bands associated with the crystalline regions in the sample were noticed. The X-ray diffraction data for microwave treated CMS-Na samples have been compared with the diffractograms of initial materials and analysis of XRD patterns confirmed that microwave-treated samples exhibit completely amorphous structure. Analysis of structural changes allows to state that the binding of sand grains in moulding sand with CMS-Na polymeric binder consists in the formation of hydrogen bonds networks (physical cross-linking). Copyright © 2018 Elsevier B.V. All rights reserved.

  1. XRD and HREM studies from the decomposition of icosahedral AlCuFe single-phase by high-energy ball milling

    International Nuclear Information System (INIS)

    Patino-Carachure, C.; Tellez-Vazquez, O.; Rosas, G.

    2011-01-01

    Highlights: → Point defects induced during milling leading to an order-disorder quasicrystal transition. → Nanoquasicrystalline regions of 12 nm are obtained. → Highly ordered i-phase with high symmetry transforms to a crystalline phase of intermetallic character and lower symmetry. - Abstract: In this investigation the Al 64 Cu 24 Fe 12 alloy was melted in an induction furnace and solidified under normal casting conditions. In order to obtain the icosahedral phase (i-phase) in a single-phase region, the as-cast sample was subject to a heat treatment at 700 deg. C under argon atmosphere. Subsequently, the i-phase was milled for different times in order to evaluate phase stability under heavy deformation. X-ray diffraction (XRD) and high-resolution electron microscopy (HREM) analysis were conducted to the structural characterization of ball-milled powders. XRD results indicated a reduction in quasicrystal size during mechanical ball milling to about 30 h. HREM analysis revealed the presence of aperiodic nano-domains, for example, with apparent fivefold symmetry axis. Therefore, the i-phase remains stable over the first 30 h of ball-milling time. However, among 30-50 h of mechanical milling the i-phase transforms progressively into β-cubic phase.

  2. XRD and HREM studies from the decomposition of icosahedral AlCuFe single-phase by high-energy ball milling

    Energy Technology Data Exchange (ETDEWEB)

    Patino-Carachure, C.; Tellez-Vazquez, O. [Instituto de Investigaciones Metalurgicas, UMSNH, Edificio U, Ciudad Universitaria, Morelia, Michoacan 58000 (Mexico); Rosas, G., E-mail: grtrejo@umich.mx [Instituto de Investigaciones Metalurgicas, UMSNH, Edificio U, Ciudad Universitaria, Morelia, Michoacan 58000 (Mexico)

    2011-10-13

    Highlights: > Point defects induced during milling leading to an order-disorder quasicrystal transition. > Nanoquasicrystalline regions of 12 nm are obtained. > Highly ordered i-phase with high symmetry transforms to a crystalline phase of intermetallic character and lower symmetry. - Abstract: In this investigation the Al{sub 64}Cu{sub 24}Fe{sub 12} alloy was melted in an induction furnace and solidified under normal casting conditions. In order to obtain the icosahedral phase (i-phase) in a single-phase region, the as-cast sample was subject to a heat treatment at 700 deg. C under argon atmosphere. Subsequently, the i-phase was milled for different times in order to evaluate phase stability under heavy deformation. X-ray diffraction (XRD) and high-resolution electron microscopy (HREM) analysis were conducted to the structural characterization of ball-milled powders. XRD results indicated a reduction in quasicrystal size during mechanical ball milling to about 30 h. HREM analysis revealed the presence of aperiodic nano-domains, for example, with apparent fivefold symmetry axis. Therefore, the i-phase remains stable over the first 30 h of ball-milling time. However, among 30-50 h of mechanical milling the i-phase transforms progressively into {beta}-cubic phase.

  3. Development of Fe-Ni/YSZ-GDC electro-catalysts for application as SOFC anodes. XRD and TPR characterization, and evaluation in ethanol steam reforming reaction

    Energy Technology Data Exchange (ETDEWEB)

    Paz Fiuza, Raigenis da; Silva, Marcos Aurelio da; Boaventura, Jaime Soares [UFBA, Salvador, Bahia (Brazil). Energy and Materials Science Group

    2010-07-01

    Electro-catalysts based on Fe-Ni alloys were prepared using physical mixture and modified Pechini methods; they were supported on a composite of Yttria Stabilized Zirconia (YSZ) and Gadolinia Doped Ceria (GDC). The composites had compositions of 35% metal load and 65% support (70% wt. YSZ and 30% wt. GDC mixture) (cermets). The samples were characterized by Temperature-Programmed Reduction (TPR) and X-Ray Diffraction (XRD) and evaluated in ethanol steam reforming at 650 C for six hours and in the temperature range 300 - 900 C. The XRD results showed that the bimetallic sample calcined at 800 C formed a mixed oxide (NiFe{sub 2}O{sub 4}) in spinel structure; after reducing the sample in hydrogen, Ni-Fe alloys were formed. The presence of Ni decreased the final reduction temperature of the NiFe{sub 2}O{sub 4} species. The addition of Fe to Ni anchored to YSZ-GDC increased the hydrogen production and inhibits the carbon deposition. The bimetallic 30Fe5Ni samples reached an ethanol conversion of about 95%, and a hydrogen yield up to 48% at 750 C. In general, the ethanol conversion and hydrogen production were independent of the metal content in the electro-catalyst. However, the substitution of Ni for Fe significantly reduced the carbon deposition on the electro-catalyst: 74, 31 and 9 wt. % in the 35Ni, 20Fe15Ni, and 30Fe5Ni samples, respectively. (orig.)

  4. Co-ordination properties of diglycol-amide (DGA) to trivalent curium and lanthanides studied by XAS, XRD and XPS methods

    International Nuclear Information System (INIS)

    Yaita, T.; Hirata, M.; Narita, H.; Tachimori, S.; Yamamoto, H.; Edelstein, N.M.; Bucher, J.J.; Shuh, D.K.; Rao, L.

    2001-01-01

    Co-ordination properties of diglycol-amide (DGA) to trivalent curium and to the trivalent lanthanides were studied by the EXAFS, the XRD and the XPS methods. The structural determinations by both the crystal XRD and the solution EXAFS methods showed that the DGA co-ordinated to the trivalent lanthanide ion in a tridentate fashion: co-ordination of three oxygen atoms of each ligand to the metal ion. The bond distances of Er-O (carbonyl) and Er-O (ether) in the Er-DGA complex were 2.35 Angstrom, and 2.46 Angstrom, respectively, while the atom distances of Cm-O (carbonyl) and Cm-O (ether) in the Cm-DGA complex were 2.42 Angstrom and 3.94 Angstrom, respectively from the EXAFS data for the Cm-DGA complex. Accordingly, the DGA would behave only as a semi-tridentate in the co-ordination to trivalent curium in solution. We determined the valence band structures of the Er-DGA complex by the XPS in order to clarify the bond properties of the complex, and assigned the XPS spectrum by using the DV-DS molecular orbital calculation method. (authors)

  5. Mössbauer, XRD and TEM Study on the Intercalation and the Release of Drugs in/from Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    E. Kuzmann

    2015-12-01

    Full Text Available Layered double hydroxides (LDHs are one of the very important nano-carriers for drug delivery, due to their many advantageous features, such as the ease and low-cost of preparation, low cytotoxicity, good biocompatibility, protection for the intercalated drugs, and the capacity to facilitate the uptake of the loaded drug in the cells. In our previous studies, Mössbauer spectroscopy was applied to monitor structural changes occurring during the incorporation of Fe(III in MgFe- and CaFe-LDHs, and the intercalation of various organic compounds in anionic form. Recently, we have successfully elaborated a protocol for the intercalation and release of indol-2-carboxylate and L-cysteinate in CaFe-LDH. The corresponding structural changes in the LDH samples were studied by XRD, HR-TEM and 57Fe Mössbauer spectroscopy. The Mössbauer spectra reflected small but significant changes upon both the intercalation and the release of drugs. The changes in the basal distances could be followed by XRD measurements, and HR-TEM images made these changes visible.

  6. Ce-doped nanoparticles of TiO2: Rutile-to-brookite phase transition and evolution of Ce local-structure studied with XRD and XANES

    International Nuclear Information System (INIS)

    Kityakarn, Sutasinee; Worayingyong, Attera; Suramitr, Anwaraporn; Smith, M.F.

    2013-01-01

    The crystal and electronic structural changes undergone by TiO 2 nanoparticles when Ce is introduced were studied using X-ray diffraction (XRD) and X-ray absorption near-edge spectroscopy (XANES). A small amount of Ce (less than 1% molar concentration) resulted in i/a significant reduction of the average size of the TiO 2 nanoparticles and ii/a phase transition in which brookite replaced rutile as the minority phase component (anatase was the majority phase component at all Ce concentrations studied up to 10% molar concentration). The Ce L3 edge XANES revealed changes in the local environment of Ce impurities. As Ce concentration was increased the fraction of Ce that have formal valence of +3 decreased and, for the remaining Ce with valence +4, the 4f orbitals became less-strongly hybridized with the p-orbitals of oxygen neighbors. The results have implications for photocatalytic and gas sensing properties of Ce-doped TiO 2 . - Highlights: ► Ce-doping: TiO 2 nanoparticles shrink and minority phase changes rutile-> brookite. ► XANES reveals phase change for arbitrarily small particles (while XRD fails). ► As Ce added: fraction of Ce +3 dopants falls, hybridization of Ce +4 with O weakens

  7. Raman-Mössbauer-XRD studies of selected samples from "Los Azulejos" outcrop: A possible analogue for assessing the alteration processes on Mars

    Science.gov (United States)

    Lalla, E. A.; Sanz-Arranz, A.; Lopez-Reyes, G.; Sansano, A.; Medina, J.; Schmanke, D.; Klingelhoefer, G.; Rodríguez-Losada, J. A.; Martínez-Frías, J.; Rull, F.

    2016-06-01

    The outcrop of "Los Azulejos" is visible at the interior of the Cañadas Caldera in Tenerife Island (Spain). It exhibits a great variety of alteration processes that could be considered as terrestrial analogue for several geological processes on Mars. This outcrop is particularly interesting due to the content of clays, zeolite, iron oxides, and sulfates corresponding to a hydrothermal alteration catalogued as "Azulejos" type alteration. A detailed analysis by portable and laboratory Raman systems as well as other different techniques such as X-ray diffraction (XRD) and Mössbauer spectroscopy has been carried out (using twin-instruments from Martian lander missions: Mössbauer spectrometer MIMOS-II from the NASA-MER mission of 2001 and the XRD diffractometer from the NASA-MSL Curiosity mission of 2012). The mineral identification presents the following mineral species: magnetite, goethite, hematite, anatase, rutile, quartz, gregoryite, sulfate (thenardite and hexahydrite), diopside, feldspar, analcime, kaolinite and muscovite. Moreover, the in-situ Raman and Micro-Raman measurements have been performed in order to compare the capabilities of the portable system specially focused for the next ESA Exo-Mars mission. The mineral detection confirms the sub-aerial alteration on the surface and the hydrothermal processes by the volcanic fluid circulations in the fresh part. Therefore, the secondary more abundant mineralization acts as the color agent of the rocks. Thus, the zeolite-illite group is the responsible for the bluish coloration, as well as the feldspars and carbonates for the whitish and the iron oxide for the redish parts. The XRD system was capable to detect a minor proportion of pyroxene, which is not visible by Raman and Mössbauer spectroscopy due to the "Azulejos" alteration of the parent material on the outcrop. On the other hand, Mössbauer spectroscopy was capable of detecting different types of iron-oxides (Fe3+/2+-oxide phases). These analyses

  8. Atmospheric corrosion in subtropical areas: XRD and electrochemical study of zinc atmospheric corrosion products in the province of Santa Cruz de Tenerife (Canary Islands, Spain)

    Energy Technology Data Exchange (ETDEWEB)

    Morales, J. [Departamento de Quimica Fisica, Universidad de La Laguna, 38071 La Laguna, Tenerife (Spain)]. E-mail: jmorales@ull.es; Diaz, F. [Departamento de Quimica Fisica, Universidad de La Laguna, 38071 La Laguna, Tenerife (Spain); Hernandez-Borges, J. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de La Laguna, 38071 La Laguna, Tenerife (Spain); Gonzalez, S. [Departamento de Quimica Fisica, Universidad de La Laguna, 38071 La Laguna, Tenerife (Spain)

    2006-02-15

    In the present paper, zinc sheets have been exposed for 4 years to the action of different atmospheres in 35 test sites located in the province of Santa Cruz de Tenerife, Canary Islands, Spain. Corrosion products formed on the surface of the samples have been identified by means of X-ray diffraction (XRD) for the first and second year of exposure. Zincite, hydrozincite, simonkolleite, zinc chlorohydroxysulphate, zinc oxysulphate and zinc hydroxysulphate have been identified in the test sheets. Preliminary results of an electrochemical study of the breakdown potential of zinc samples are also presented in order to test the protective effect of the film formed on the surface of the samples. It was found that the protective effect of this film increases linearly with exposure time.

  9. Application of low current intensity electrolytic treatment for the chlorides extraction in underwater archaeological objects of iron. Observation of the mineralogical phases evolution through XRD-Rietveld

    International Nuclear Information System (INIS)

    Bethencourt, M.; Gil, M. L. A.; Fernandez-Lorenzo, C.; Santos, A.

    2004-01-01

    With the purpose of optimising a suitable methodology for the conservation of an archaeological object of iron, a low current intensities electrolytic treatment has been applied, to a piece of cast iron, proving to be effective in the extraction of chloride ions from the structure of akaganeite, principal corrosion product of iron in the marine medium. The monitoring of the electrolytic treatment has been proven by applying the Rietveld method to the patterns XRD of samples extracted from the corroded surface before and after the treatment. This method has permitted the unequivocal determination of the akaganeite and its chemical composition. This identification has been corroborated by means of SEM and EDS. After the electrolytic treatment, akaganeite was not present in the sample. (Author) 9 refs

  10. A Study on the quantification of hydration and the strength development mechanism of cementitious materials including amorphous phases by using XRD/Rietveld method

    International Nuclear Information System (INIS)

    Yamada, Kazuo; Hoshino, Seiichi; Hirao, Hiroshi; Yamashita, Hiroki

    2008-01-01

    X-ray diffraction (XRD)/Rietveld method was applied to measure the phase composition of cement. The quantative analysis concerning the progress of hydration was accomplished in an error of about the maximum 2-3% in spite of including amorphous materials such as blast furnace slag, fly ash, silica fume and C-S-H. The influence of the compressive strength on the lime stone fine powder mixture material was studied from the hydration analysis by Rietveld method. The two stages were observed in the strength development mechanism of cement; the hydration promotion of C 3 S in the early stage and the filling of cavities by carbonate hydrate for the longer term. It is useful to use various mixture materials for the formation of the resource recycling society and the durability improvement of concrete. (author)

  11. Influence of the stirring time on the exfoliation of the Cloisite 30 B clay in PVC composite: structural characterization by XRD

    International Nuclear Information System (INIS)

    Cabral, Andreia M.V.; Rodrigues, Meiry G.F.

    2009-01-01

    This study aims to evaluate the influence of the stirring time on the exfoliation efficiency of the montmorillonite clay in PVC composites, prepared by the polymerization 'in situ' process. The work was performed in 2 steps. In first stage: tests of expansion with Cloisite 30B clay in MVC, which was used to assess the degree of expansion in MVC of each of them at different stirring times: 2, 4 and 6 h. After stirring, each system was kept in observation for 3 days to evaluate the changes in the decanted volume of the clay in the reactor. Second stage: the Influence of the stirring time for the clay exfoliation. Cloisite 30B clay was used to compare the influence of the stirring time for exfoliation and characterized by X-ray diffraction (XRD). (author)

  12. Development of an Innovative XRD-DRIFTS Prototype Allowing Operando Characterizations during Fischer-Tropsch Synthesis over Cobalt-Based Catalysts under Representative Conditions

    Directory of Open Access Journals (Sweden)

    Scalbert Julien

    2015-03-01

    Full Text Available An original system combining both X-Ray Diffraction and diffuse reflectance infrared Fourier transform spectroscopy was developed with the aim to characterize Fischer-Tropsch catalysts in relevant reaction conditions. The catalytic properties of a model PtCo/silica catalyst tested with this prototype have shown to be in the same range of those obtained in similar conditions with classical fixed-bed reactors. No bulk cobalt oxidation nor sintering were observed on operando XRD patterns. The formation of linear carbonyls and adsorbed hydrocarbons species at the surface of the catalyst was observed on operando DRIFT spectra. The surface of the catalyst was also suspected to be covered with carbon species inducing unfavorable changes in selectivity.

  13. Nano Cu interaction with single amino acid tyrosine derived self-assemblies; study through XRD, AFM, confocal Raman microscopy, SERS and DFT methods

    Science.gov (United States)

    Govindhan, Raman; Karthikeyan, Balakrishnan

    2017-12-01

    3,5-Bis(trifluoromethyl)benzylamine derivatives of single amino acid tyrosine produced self-assembled nanotubes (BTTNTs) as simple Phe-Phe. It has been observed that tyrosine derivative gives exclusively micro and nano tubes irrespective of the concentration of the precursor monomer. However, the introduced xenobiotic trifluoromethyl group (TFM) present in key backbone positionsof the self assembly gives the specific therapeutic function has been highlighted. Herein this work study of such self assembled nanotubes were studied through experimental and theoretical methods. The interaction of nanocopper cluster with the nanotubes (Cu@BTTNTs) were extensively studied by various methods like XRD, AFM, confocal Raman microscopy, SERS and theoretical methods like Mulliken's atomic charge analysis. SERS reveals that the interactions of Cu cluster with NH2, OH, NH and phenyl ring π-electrons system of BTTNTs. DFT studies gave the total dipole moment values of Cu@BTTNTs and explained the nature of interaction.

  14. Stability of mineral fibres in contact with human cell cultures. An in situ μXANES, μXRD and XRF iron mapping study.

    Science.gov (United States)

    Pollastri, Simone; Gualtieri, Alessandro F; Vigliaturo, Ruggero; Ignatyev, Konstantin; Strafella, Elisabetta; Pugnaloni, Armanda; Croce, Alessandro

    2016-12-01

    Relevant mineral fibres of social and economic importance (chrysotile UICC, crocidolite UICC and a fibrous erionite from Jersey, Nevada, USA) were put in contact with cultured diploid human non-tumorigenic bronchial epithelial (Beas2B) and pleural transformed mesothelial (MeT5A) cells to test their cytotoxicity. Slides of each sample at different contact times up to 96 h were studied in situ using synchrotron XRF, μ-XRD and μ-XAS (I18 beamline, Diamond Light Source, UK) and TEM investigations. XRF maps of samples treated for 96 h evidenced that iron is still present within the chrysotile and crocidolite fibres and retained at the surface of the erionite fibres, indicating its null to minor mobilization in contact with cell media; this picture was confirmed by the results of XANES pre-edge analyses. μ-XRD and TEM data indicate greater morphological and crystallinity modifications occurring in chrysotile, whereas crocidolite and erionite show to be resistant in the biological environment. The contact of chrysotile with the cell cultures seems to lead to earlier amorphization, interpreted as the first dissolution step of these fibres. The formation of such silica-rich fibre skeleton may prompt the production of HO in synergy with surface iron species and could indicate that chrysotile may be much more reactive and cytotoxic in vitro in the (very) short term whereas the activity of crocidolite and erionite would be much more sluggish but persistent in the long term. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. High resolution HH-XRF scanning and XRD modelling as a tool in sedimentological analysis - A case study from the Enreca-3 core, Bach Long Vi Island, Vietnam

    Science.gov (United States)

    Rizzi, Malgorzata; Hemmingsen Schovsbo, Niels; Korte, Christoph; Bryld Wessel Fyhn, Michael

    2017-04-01

    To improve the understanding and interpretation of the depositional environment of a late Oligocene lacustrine organic rich oil-prone source rock succession, 2464 hand held (HH)-XRF measurements were made systematically on the 500 m long, continuous core from the fully cored Enreca-3 well. This core, drilled on the remote Bach Long Vi Island, northern Gulf of Tonkin, offshore Vietnam, represents a deep lake succession alternating between lacustrine pelagic dominated sediments interrupted by hyperpycnal turbidites, high density turbidites and debris flows [1, 2]. From a combined HH-XRF-XRD data set, multivariate data analysis and regression models are used to type the rock and to predict the XRD mineral composition based on HH-XRF composition. The rock types and the modelled mineral composition highlight the geochemical variations of the sediment and allows for direct comparison with sedimentological processes and facies changes. The modeling also depicts the cyclic alteration of rock types that are present on many different scales ranging from centimeters to hundreds of meters [1, 2]. The sedimentological and geochemical variations observed throughout the cored section reflects fluctuating paleoclimate, tectonism and hinterland condition controlling the depositional setting, which may provide a deeper understanding of the deposition of this and similar Paleogene syn-rift succession in the South China Sea region. It allows furthermore the development of a more generalized depositional model relevant for other deep-lacustrine syn-rift basins. [1] Petersen et al. (2014) Journal of Petroleum Geology, 37: 373-389. [2] Hovikoski et al. (2016) Journal of Sedimentary Research, 86(8): 982-1007.

  16. [X-ray diffraction (XRD) and near infrared spectrum (NIR) analysis of the soil overlying the Bairendaba deposit of the Inner Mongolia Grassland].

    Science.gov (United States)

    Luo, Song-ying; Cao, Jian-jin; Wu, Zheng-quan

    2014-08-01

    The soil samples uniformly overlying the Bairendaba deposit of the Inner Mongolia grassland were collected, and ana- lyzed with X-ray diffraction (XRD) and near infrared spectrum (NIR), for exploring the origins of the soil from the, grassland mining area and the relationship with the underground rock. The results show that the samp]s consist of quartz, graphite, carbonate, hornblende, mica, chlorite, montmorillonite, illite, berlinite, diaspore, azurite, hen tite, etc. These indicate that the soil samples were not only from the weathering products of the surface rock, but also from the underground rock mass and the alteration of the wall rock. The azurite and the hematite contained in the soil, mainly coming from the oxidation zone of the orebodies, can be used as the prospecting marks. The alteration mineral assemblage is mainly chlorite-illite-montmorillonite and it experienced the alteration process of potassic alteration-->silicification-->carbonatization-->silk greisenization-->clayization. Also, the wall rock alteration and the physical weathering processes can be accurately restored by analyzing the combination of the alteration minerals, which can provide important reference information for the deep ore prospecting and the ore deposit genesis study, improving the rate of the prospecting. The XRD and NIR with the characteristics of the economy and quickness can be used for the identification of mineral composition of soil, and in the study of mineral and mineral deposits. Especially, NIR has its unique superiority, that is, its sample request is low, and it can analyze a batch of samples quickly. With the development of INR, it will be more and more widely applied in geological field, and can play an important role in the ore exploration.

  17. Development of Fe-Ni/YSZ-GDC electrocatalysts for application as SOFC anodes: XRD and TPR characterization and evaluation in the ethanol steam reforming reaction

    Energy Technology Data Exchange (ETDEWEB)

    da Paz Fiuza, Raigenis; Aurelio da Silva, Marcos; Boaventura, Jaime Soares [Energy and Materials Science Group - GECIM, Institute of Chemistry, Physical Chemistry Department, Universidade Federal da Bahia, 41170290 Salvador, Bahia (Brazil)

    2010-10-15

    Electrocatalysts based on Fe-Ni alloys were prepared by means of modified Pechini and physical mixture methods and using on a composite of Yttria Stabilized Zirconia (YSZ) and Gadolinia-Doped Ceria (GDC) as support. The former method was based on the formation a polymeric precursor that was subsequently calcined; the later method was based on the mixture of NiO and the support. The resulting composites had 35 wt.% metal load and 65 wt.% support (70 wt.% YSZ and 30 wt.% GDC mixture) (cermets). The samples were then characterized by Temperature-Programmed Reduction (TPR) and X-Ray Diffraction (XRD) and evaluated in the ethanol steam reforming at 650 C for 6 h in the temperature range of 300-900 C. The XRD results showed that the bimetallic sample calcined at 800 C formed a mixed oxide (NiFe{sub 2}O{sub 4}) with a spinel structure, which, after reduction in hydrogen, formed Ni-Fe alloys. The presence of Ni was observed to decrease the final reduction temperature of the NiFe{sub 2}O{sub 4} species. The addition of iron to the nickel anchored to YSZ-GDC increased the hydrogen production and inhibited carbon deposition. The resulting bimetallic 30Fe5Ni sample reached an ethanol conversion of about 95% and a hydrogen yield up to 48% at 750 C. In general, ethanol conversion and hydrogen production were independent of the metal content in the electrocatalyst. However, the substitution of nickel for iron significantly reduced carbon deposition on the electrocatalyst: 74, 31, and 9 wt.% in the 35Ni, 20Fe15Ni, and 30Fe5Ni samples, respectively. (author)

  18. Characterization of wet precipitation by X-ray diffraction (XRD) and scanning electron microscopy (SEM) in the metropolitan area of Porto Alegre, Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Montanari Migliavacca, Daniela [Instituto de Biociencias, Programa de Pos-Graduacao em Ecologia, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91509-900 Porto Alegre, RS (Brazil); Fundacao Estadual de Protecao Ambiental Henrique Luis Roessler, RS. Rua Carlos Chagas 55/802, 90030-020 Porto Alegre, RS (Brazil); Calesso Teixeira, Elba, E-mail: gerpro.pesquisa@fepam.rs.gov.br [Fundacao Estadual de Protecao Ambiental Henrique Luis Roessler, RS. Rua Carlos Chagas 55/802, 90030-020 Porto Alegre, RS (Brazil); Gervasoni, Fernanda; Vieira Conceicao, Rommulo [Instituto de Geociencias, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91509-900 Porto Alegre, RS (Brazil); Raya Rodriguez, Maria Teresa [Instituto de Biociencias, Programa de Pos-Graduacao em Ecologia, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91509-900 Porto Alegre, RS (Brazil)

    2009-11-15

    The purpose of this study is to assess the composition of wet precipitation in three sites of the metropolitan area of Porto Alegre. Besides the variables usually considered, such as pH, conductivity, major ions (Cl{sup -}, NO{sub 3}{sup -}, F{sup -}, SO{sub 4}{sup 2-}, Na{sup +}, K{sup +}, Mg{sup 2+}, NH{sub 4}{sup +} and Ca{sup 2+}) and metallic elements (Cd, Co, Cr, Cu, Fe, Mn and Ni), the suspended matter was examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM), with energy dispersive system (EDS), for better identification of possible anthropogenic material in this wet precipitation. Results showed an alkaline pH in the samples analyzed and higher concentrations for Na{sup +}, Cl{sup -} and SO{sub 4}{sup 2-}. The acidification and neutralization potential between anions (SO{sub 4}{sup 2-} + NO{sub 3}{sup -}) and cations (Ca{sup 2+} + Mg{sup 2+} + K{sup +} + NH{sub 4}{sup +}) showed a good correlation (0.922). The metallic elements with highest values were Zn, Fe and Mn. Results of XRD identified the presence of some minerals such as quartz, feldspar, mica, clay, carbonates and sulfates. In samples analyzed with SEM, we detected pyroxene, biotite, amphibole and oxides. Cluster analysis (CA) was applied to the data matrix to identify potential pollution sources of metals (natural or anthropogenic) and the association with minerals found in the analysis of SEM.

  19. Mossbauer and XRD characterization of the phase transformations in a Fe-Mn-Al-C-Mo-Si-Cu as cast alloy during tribology test

    Science.gov (United States)

    Ramos, J.; Piamba, J. F.; Sánchez, H.; Alcazar, G. A. Pérez

    2015-06-01

    In present study Fe-29.0Mn-6Al-0.9C-1.8Mo-1.6Si-0.4Cu (%w) alloy was obtained after melted in an induction furnace, and then molded as an ingot. From the as cast ingot it were cut samples for the different characterization measurements. The microstructure of the as-cast sample is of dendritic type and its XRD pattern was refined with the lines of the austenite, with a big volumetric fraction, and the lines of the martensite, with small volumetric fraction. The Mössbauer spectrum of the sample was fitted with a broad singlet which corresponds to disordered austenite. After the tribology test, its XRD pattern was refined with the lines of two austenite phases, one similar to the previous one and other with bigger lattice parameter. The total volumetric fraction of the austenite is smaller than that obtained for sample without wear. It was added the lines of the martensite phase with bigger volumetric fraction than that of the previous sample. The Mössbauer spectrum of the weared sample was fitted with two paramagnetic sites which correspond to the two Fe austenite phases and a hyperfine magnetic field distribution which is associated to the disordered original martensite and the new one which appears in the surface as a consequence of the wear process. These results show that during wear process the original austenite phase is transformed in martensite and in a new austenite phase. The increases of the martensitic phase improves mechanical properties and wear behavior.

  20. Mossbauer and XRD characterization of the phase transformations in a Fe-Mn-Al-C-Mo-Si-Cu as cast alloy during tribology test

    Energy Technology Data Exchange (ETDEWEB)

    Ramos, J. [Universidad Autónoma de Occidente (Colombia); Piamba, J. F. [Universidad del Valle, Departamento Física (Colombia); Sánchez, H. [Universidad del Valle, Escuela de Materiales (Colombia); Alcazar, G. A. Pérez, E-mail: gpgeperez@gmail.com [Universidad del Valle, Departamento Física (Colombia)

    2015-06-15

    In present study Fe-29.0Mn-6Al–0.9C-1.8Mo-1.6Si-0.4Cu (%w) alloy was obtained after melted in an induction furnace, and then molded as an ingot. From the as cast ingot it were cut samples for the different characterization measurements. The microstructure of the as-cast sample is of dendritic type and its XRD pattern was refined with the lines of the austenite, with a big volumetric fraction, and the lines of the martensite, with small volumetric fraction. The Mössbauer spectrum of the sample was fitted with a broad singlet which corresponds to disordered austenite. After the tribology test, its XRD pattern was refined with the lines of two austenite phases, one similar to the previous one and other with bigger lattice parameter. The total volumetric fraction of the austenite is smaller than that obtained for sample without wear. It was added the lines of the martensite phase with bigger volumetric fraction than that of the previous sample. The Mössbauer spectrum of the weared sample was fitted with two paramagnetic sites which correspond to the two Fe austenite phases and a hyperfine magnetic field distribution which is associated to the disordered original martensite and the new one which appears in the surface as a consequence of the wear process. These results show that during wear process the original austenite phase is transformed in martensite and in a new austenite phase. The increases of the martensitic phase improves mechanical properties and wear behavior.

  1. XRD applied to the determination of pigments and composition of lithic materials and ceramics from archaeological pre-hispanic sites of the Rio de la Plata

    International Nuclear Information System (INIS)

    Beovide, Laura; Pardo, Helena; Faccio, Ricardo; Mombru, Alvaro; Piston, Mariela

    2011-01-01

    Full text: The earliest records of human occupation on the lower basin of Santa Lucia River are dated ca. 4800 14 C years BP, in the area of one of the major tributaries of the Rio de la Plata on the Uruguayan coast. These societies were basically hunters and gatherers until ca. 3000 14 C years BP when they incorporated the horticulture. In this multidisciplinary work, two cases of application of XRD analysis of archaeological materials are presented to provide new perspectives in solving various problems related to the technological organization of these societies. In the first case, ceramics and pigments from an archaeological context prior to the hispanic-indian contact were analyzed. The X-ray powder diffraction patterns were obtained using a RIGAKU, Ultima IV with CBO monochromator, CuK α radiation was at 40 kV and 20 mA tube power at 0.02 deg/seg, operating in the range from 2θ=5.00 to 60.00 deg. According the comparison between the experimental recorded X-ray diffraction pattern to those stored in a X-ray powder diffraction database reveals that the piece of pottery is mainly constitute of quartz (SiO 2 ) and hematite (Fe 2 O 3 ) while the mineral sample is probably composed mainly of quartz (SiO 2 ) and goethite (FeO 3 .H 2 O). The results allow a first approximation to know the inorganic pigments that were part of the decoration of the pottery and pigments used in the archaeological context. In the second case an amphibolite instrument from ca. 2700 14 C years BP related to a shell midden was analyzed and compared with amphibolites located 15 km of the archaeological site to assess if they were the raw materials for these instruments. Compositional XRD mineralogical analysis shows that the both samples seem to have similar mineral composition, which is mainly quartz (SiO 2 ) and a mixed sodium magnesium and calcium silicate (NaCa 2 (Mg 4 Ti)Si 6 Al 2 O 23 (OH) 2 ). This suggests that most likely the source of supply for the amphibolites instruments come

  2. XRD applied to the determination of pigments and composition of lithic materials and ceramics from archaeological pre-hispanic sites of the Rio de la Plata

    Energy Technology Data Exchange (ETDEWEB)

    Beovide, Laura [Department of Archeology, National Museum of Anthropology, Montevideo, (Uruguay); Pardo, Helena; Faccio, Ricardo; Mombru, Alvaro [Centro NanoMat, Polo Tecnologico de Pando, Facultad de Quimica, Universidad de la Republica, Pando, Canelones (Uruguay); Crystallography, Solid State and Materials Laboratory (Cryssmat-Lab), DETEMA, Facultad de Quimica, Universidad de la Republica, Gral, Montevideo (Uruguay); Piston, Mariela, E-mail: mpiston@fq.edu.u [Analytical Chemistry, Estrella Campos Department, Facultad de Quimica, Universidad de la Republica, Montevideo (Uruguay)

    2011-07-01

    Full text: The earliest records of human occupation on the lower basin of Santa Lucia River are dated ca. 4800 {sup 14}C years BP, in the area of one of the major tributaries of the Rio de la Plata on the Uruguayan coast. These societies were basically hunters and gatherers until ca. 3000 {sup 14}C years BP when they incorporated the horticulture. In this multidisciplinary work, two cases of application of XRD analysis of archaeological materials are presented to provide new perspectives in solving various problems related to the technological organization of these societies. In the first case, ceramics and pigments from an archaeological context prior to the hispanic-indian contact were analyzed. The X-ray powder diffraction patterns were obtained using a RIGAKU, Ultima IV with CBO monochromator, CuK{sub {alpha}} radiation was at 40 kV and 20 mA tube power at 0.02 deg/seg, operating in the range from 2{theta}=5.00 to 60.00 deg. According the comparison between the experimental recorded X-ray diffraction pattern to those stored in a X-ray powder diffraction database reveals that the piece of pottery is mainly constitute of quartz (SiO{sub 2}) and hematite (Fe{sub 2}O{sub 3}) while the mineral sample is probably composed mainly of quartz (SiO{sub 2}) and goethite (FeO{sub 3}.H{sub 2}O). The results allow a first approximation to know the inorganic pigments that were part of the decoration of the pottery and pigments used in the archaeological context. In the second case an amphibolite instrument from ca. 2700 {sup 14}C years BP related to a shell midden was analyzed and compared with amphibolites located 15 km of the archaeological site to assess if they were the raw materials for these instruments. Compositional XRD mineralogical analysis shows that the both samples seem to have similar mineral composition, which is mainly quartz (SiO{sub 2}) and a mixed sodium magnesium and calcium silicate (NaCa{sub 2}(Mg{sub 4}Ti)Si{sub 6}Al{sub 2}O{sub 23}(OH){sub 2}). This

  3. Structural changes and thermal stability of charged LiNixMnyCozO₂ cathode materials studied by combined in situ time-resolved XRD and mass spectroscopy.

    Science.gov (United States)

    Bak, Seong-Min; Hu, Enyuan; Zhou, Yongning; Yu, Xiqian; Senanayake, Sanjaya D; Cho, Sung-Jin; Kim, Kwang-Bum; Chung, Kyung Yoon; Yang, Xiao-Qing; Nam, Kyung-Wan

    2014-12-24

    Thermal stability of charged LiNixMnyCozO2 (NMC, with x + y + z = 1, x:y:z = 4:3:3 (NMC433), 5:3:2 (NMC532), 6:2:2 (NMC622), and 8:1:1 (NMC811)) cathode materials is systematically studied using combined in situ time-resolved X-ray diffraction and mass spectroscopy (TR-XRD/MS) techniques upon heating up to 600 °C. The TR-XRD/MS results indicate that the content of Ni, Co, and Mn significantly affects both the structural changes and the oxygen release features during heating: the more Ni and less Co and Mn, the lower the onset temperature of the phase transition (i.e., thermal decomposition) and the larger amount of oxygen release. Interestingly, the NMC532 seems to be the optimized composition to maintain a reasonably good thermal stability, comparable to the low-nickel-content materials (e.g., NMC333 and NMC433), while having a high capacity close to the high-nickel-content materials (e.g., NMC811 and NMC622). The origin of the thermal decomposition of NMC cathode materials was elucidated by the changes in the oxidation states of each transition metal (TM) cations (i.e., Ni, Co, and Mn) and their site preferences during thermal decomposition. It is revealed that Mn ions mainly occupy the 3a octahedral sites of a layered structure (R3̅m) but Co ions prefer to migrate to the 8a tetrahedral sites of a spinel structure (Fd3̅m) during the thermal decomposition. Such element-dependent cation migration plays a very important role in the thermal stability of NMC cathode materials. The reasonably good thermal stability and high capacity characteristics of the NMC532 composition is originated from the well-balanced ratio of nickel content to manganese and cobalt contents. This systematic study provides insight into the rational design of NMC-based cathode materials with a desired balance between thermal stability and high energy density.

  4. Vacancy ordered γ-Fe{sub 2}O{sub 3} nanoparticles functionalized with nanohydroxyapatite: XRD, FTIR, TEM, XPS and Mössbauer studies

    Energy Technology Data Exchange (ETDEWEB)

    Ramos Guivar, Juan A., E-mail: juan.ramos5@unmsm.edu.pe [Faculty of Physical Sciences, National University of San Marcos, P. O. Box 14- 0149, Lima 14 (Peru); Sanches, Edgar A., E-mail: sanches.ufam@gmail.com [Federal University of Amazonas, Department of Physics, Manaus/AM (Brazil); Bruns, Florian, E-mail: f.bruns@tu-braunschweig.de [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Sadrollahi, Elaheh, E-mail: elahe.sadrollahi@gmail.com [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Morales, M.A., E-mail: marco.moralestorres@gmail.com [Department of Theoretical and Experimental Physics, UFRN, Natal, RN 59078- 970 (Brazil); López, Elvis O., E-mail: lopmezel@gmail.com [Brazilian Center for Research in Physics (CBPF), Rio de Janeiro, RJ 22290-180 (Brazil); Litterst, F. Jochen, E-mail: litterst@cbpf.br [Institut für Physik der Kondensierten Materie, Technische Universität Braunschweig, 38110 Braunschweig (Germany); Brazilian Center for Research in Physics (CBPF), Rio de Janeiro, RJ 22290-180 (Brazil)

    2016-12-15

    Graphical abstract: Possible bonding configuration in the γ-Fe{sub 2}O{sub 3} nanoparticles functionalized with nanoHAp. - Highlights: • Coprecipitation in alkaline medium for the synthesis of vacancy ordered γ-Fe{sub 2}O{sub 3}@HAp nanocomposite. • Samples were characterized by XRD, FTIR, XPS, TEM, VSM and Mössbauer spectroscopy. • The functionalization is explained with the binding of two oxygens of chemisorbed H{sub 2}O molecules at the common interface of HAp/C{sub 6}H{sub 8}O{sub 7}/γ-Fe{sub 2}O{sub 3}. - Abstract: Vacancy ordered maghemite (γ-Fe{sub 2}O{sub 3}) nanoparticles functionalized with nanohydroxyapatite (HAp – Ca{sub 10}(PO{sub 4}) {sub 6}(OH){sub 2}) have been successfully synthesized using an inexpensive co-precipitation chemical route. Evidence for the presence of vacancy order in maghemite was shown by the superstructure lines observed in X-ray diffraction. The adsorption of carboxyl groups of citric acid (C{sub 6}H{sub 8}O{sub 7}) onto γ-Fe{sub 2}O{sub 3} nanoparticles was investigated by FTIR, XPS and Mössbauer spectroscopy. From XPS surface analysis, two binding energies related to oxygen were attributed to bindings between C{sub 6}H{sub 8}O{sub 7}/γ- Fe{sub 2}O{sub 3} and C{sub 6}H{sub 8}O{sub 7}/HAp from an interfacial reaction promoted by strongly adsorbed H{sub 2}O molecules at the surface of these nanomaterials. Le Bail refinement of the XRD patterns showed the formation of well-crystallized pure tetragonal maghemite before and after functionalization with nanoHAp. The temperature dependence of hyperfine parameters of pure and functionalized γ-Fe{sub 2}O{sub 3} nanoparticles was investigated via Mössbauer spectroscopy. TEM revealed the formation of quasi-spherical γ- Fe{sub 2}O{sub 3} nanoparticles with an average diameter of ca. 12 nm and 16 nm before and after functionalization with nanoHAp in agreement with Le Bail refinement. Magnetometry measurements showed a saturation magnetization of 12 emu/g and a blocking

  5. Identification and characterization of historical pigments with x-ray diffraction analysis (XRD), x-ray fluorescence analysis (XRA) and Fourier transformed infrared spectroscopy (FTIR)

    International Nuclear Information System (INIS)

    Hochleitner, B.

    2002-11-01

    This thesis presents a systematic characterization of historical inorganic pigments with respect to their crystallographic structure, main components, and trade elements, utilizing three complementary methods. The results are compiled in a computer-database containing the experimentally obtained information. The specimens examined in this study originate from a collection of 19th and 20th century pigments, dyes and binders with a wide variety of colors and materials at the Institute of Natural Sciences and Technologies in Art of the Academy of Fine Arts in Vienna. Approximately 400 different inorganic pigments were analysed for this first study of its kind by combining the experimental techniques explained in the next paragraph. For analyzing the inorganic pigments three different methods were applied: x-ray diffraction (XRD), x-ray fluorescence (XRF) and fourier-transformed infrared spectroscopy (FTIR) proved to be suitable techniques to identify and characterize the composition of the materials. The experimental work was focused on x-ray diffraction to detect the main components and to perform phase analysis for the identification of the crystallographic structure. To facilitate the analysis of the diffractograms and investigate differences in the elemental composition, XRF-measurements were carried out and complemented by FTIR-spectroscopy. The latter technique supports the identification of organic components of the samples and both ease phase analysis. In some cases, the obtained results show remarkable differences in composition for pigments having the same trade name. These differences consist either with respect to the identified elements or added components, such as pure white pigments. However, in most cases the chemical structure of the phase determining the color of the relevant pigment group was similar. Knowledge of the composition of the originally used pigments is of great importance for the restoration and conservation of art objects. In order to

  6. S tudies on the phase transitions and properties of tungsten (VI oxide nanoparticles by X - Ray diffraction (XRD and thermal analysis

    Directory of Open Access Journals (Sweden)

    S.F. Abdullah

    2017-11-01

    Full Text Available Tungsten (VI oxide, WO3nanoparticles were synthesized by colloidal gas aphrons(CGAs technique.The resultant WO3nanoparticleswere characterized by thermogravimetric-differential thermal analysis (TG-DTA and X-Ray diffraction (XRD measurements in order to determine the phase transitions, the crystallinity and the size of theWO3nanoparticles. As a comparison, transmission electron microscope (TEM was used to investigate the size of the WO3nanoparticles. The result from XRD and DTA show that the formation of polymorphsWO3nanoparticles have the following sequence: orthorhombic (b-WO3®monoclinic (g-WO3 ®triclinic (d-WO3 ®monoclinic (e-WO3 with respect to the calcination temperature of 400, 500, 600 and 700°C. No diffraction peaks were found in the X-Ray diffraction measurements for the sample heat treated at 300°C (as-prepared, suggesting that an amorphous structure was obtained at this temperature whereas the crystallinity had been obtained by the other samples of theWO3nanoparticles at the calcination temperatures of 400, 500, 600 and 700°C. It is also found that the X-Ray diffraction measurements produced an average diameter of (30 ±5, (50 ±5, (150 ±10 and (200 ±10 nm at calcination temperatures of 400, 500, 600 and 700°C respectively by using Debye-Scherrer formula. The TG curve revealed that the WO3nanoparticles is purely anhydrous since the weight loss is insignificant (0.3 –1.4 % from 30 until 600°C for the WO3nanoparticles calcined at 400°C. Finally, the composition and the purity of the WO3nanoparticleshave been examined by X-Ray photoelectron spectroscopy (XPS. Theresults indicate no significant changes to the composition and the purity of the WO3nanoparticle produced due to the temperature variations

  7. Prompt burst energetics experiments: fresh oxide/sodium series

    International Nuclear Information System (INIS)

    Reil, K.O.; Young, M.F.

    1978-08-01

    A series of in-pile experiments has been performed to provide information on thermal energy to work conversion under prompt burst excursion (PBE) conditions. These consisted of single pin tests using fresh uranium oxide or uranium carbide fuel in a capsule geometry, with either stagnant sodium or helium in the coolant channel. The experiments were irradiated with single or double pulses in the Annular Core Pulse Reactor (ACPR) to provide energy depositions up to 2900 J/g. This report covers the seven single and five double pulse UO 2 sodium-in tests. Experimental data includes pressure and linear motion transducer histories, measured work-energy conversion efficiencies, and post-irradiation examination. Analysis includes derived work-energy conversion efficiencies (up to 0.54%), pin failure modeling, hydrodynamic analysis of pressure pulse propagation in the channel, and piston stopping effects. Initial pressure events in the single pulse experiments appear to be dominated by fuel vapor pressure. Definite fuel-coolant interactions were observed in several experiments, including some that were coincident with stopping of the linear motion transducer piston, suggesting a possible triggering effect by the deceleration pressure

  8. CEMS and XRD studies on changing shape of iron nano-particles by irradiation of Au ions of Fe-implanted Al2O3 granular layer

    International Nuclear Information System (INIS)

    Kato, T.; Wakabayashi, H.; Hashimoto, M.; Toriyama, T.; Taniguchi, S.; Hayashi, N.; Sakamoto, I.

    2007-01-01

    In order to observe an inverse Ostwald ripening of Fe nano-particles in Fe-implanted Al 2 O 3 granular layers, 3 MeV Au ions were irradiated to Fe nano-particles in these layers with doses of 0.5x and 1.5x10 16 ions/cm 2 . It was found by Conversion Electron Mossbauer Spectroscopy (CEMS) that the inverse Ostwald ripening occurred by fractions of percentages and the magnetic anisotropy of Fe nano-particles was induced to the direction of Au ion beam, i.e. perpendicular to the granular plane. The average crystallite diameters of Fe nano-particles for Au ions unirradiated and irradiated samples were measured using Scherrer's formula from FWHM of Fe (110) X-ray Diffraction (XRD) patterns obtained by 2θ and 2θ/θ methods. It was confirmed that the average crystallite diameters of Fe nano-particles in Fe-implanted Al 2 O 3 granular layers were extended by Au ions irradiation. (author)

  9. Determinants for Tight and Selective Binding of a Medicinal Dicarbene Gold(I) Complex to a Telomeric DNA G-Quadruplex: a Joint ESI MS and XRD Investigation.

    Science.gov (United States)

    Bazzicalupi, Carla; Ferraroni, Marta; Papi, Francesco; Massai, Lara; Bertrand, Benoît; Messori, Luigi; Gratteri, Paola; Casini, Angela

    2016-03-18

    The dicarbene gold(I) complex [Au(9-methylcaffein-8-ylidene)2 ]BF4 is an exceptional organometallic compound of profound interest as a prospective anticancer agent. This gold(I) complex was previously reported to be highly cytotoxic toward various cancer cell lines in vitro and behaves as a selective G-quadruplex stabilizer. Interactions of the gold complex with various telomeric DNA models have been analyzed by a combined ESI MS and X-ray diffraction (XRD) approach. ESI MS measurements confirmed formation of stable adducts between the intact gold(I) complex and Tel 23 DNA sequence. The crystal structure of the adduct formed between [Au(9-methylcaffein-8-ylidene)2 ](+) and Tel 23 DNA G-quadruplex was solved. Tel 23 maintains a characteristic propeller conformation while binding three gold(I) dicarbene moieties at two distinct sites. Stacking interactions appear to drive noncovalent binding of the gold(I) complex. The structural basis for tight gold(I) complex/G-quadruplex recognition and its selectivity are described. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Interactions between 2,4-bis-pteridine-1,5-benzodiazepine and group 12 dihalides: synthesis, spectral and XRD structural studies and theoretical calculations.

    Science.gov (United States)

    Illán-Cabeza, Nuria A; Jiménez-Pulido, Sonia B; Hueso-Ureña, Francisco; Peña-Ruiz, Tomás; Quirós-Olozábal, Miguel; Moreno-Carretero, Miguel N

    2016-11-28

    2,4-Bis(1,3,7-trimethyl-pteridine-2,4(1H,3H)-dione-6-yl)-2,3-dihydro-2-methyl-1H-1,5-benzodiazepine (DLMBZD) has been prepared and its molecular and crystal structures have been determined from spectral and XRD data. The benzodiazepine ligand was reacted with zinc(ii), cadmium(ii) and mercury(ii) chloride, bromide and iodide to give complexes with general formula [M(DLMBZD)X 2 ]. The complexes have been synthesized and characterized by IR, NMR and elemental analysis. The structure of seven complexes has been obtained by single crystal X-ray diffraction. In all the cases, the metal is (2 + 2 + 1)-five-coordinated by two halide ligands, two nitrogen atoms from pyrazine and diazepine rings and a carbonyl oxygen from a pteridine ring. The coordinated-metal environment is a square-based pyramid, with increasing trigonality from Hg(ii) to Zn(ii) complexes. To coordinate the metals, the ligand folds itself, establishing four intramolecular σ-π interactions with the pyrimidine and pyrazine rings. A topological analysis of the electron density using the Quantum Theory of Atoms in Molecules and the complexes stability has been performed.

  11. Limestone calcination under calcium-looping conditions for CO2 capture and thermochemical energy storage in the presence of H2O: an in situ XRD analysis.

    Science.gov (United States)

    Valverde, Jose Manuel; Medina, Santiago

    2017-03-15

    This work reports an in situ XRD analysis of whether the calcination/carbonation behavior of natural limestone (CaCO 3 ) is affected by the addition of H 2 O to the calciner at a very low concentration under relevant Calcium-Looping (CaL) conditions for CO 2 capture in coal fired power plants (CFPP) and Thermochemical Energy Storage (TCES) in Concentrated Solar Power plants (CSP). Previous studies have demonstrated that the presence of steam in the calciner at a high concentration yields a significant increase in the reaction rate. However, a further undesired consequence is the serious deterioration of the CaO mechanical strength, which would lead to particle attrition and mass loss in any CaL process based on the use of circulating fluidized beds. The results presented in this manuscript on the time evolution of the wt% and crystallite size of the phases involved in the calcination/carbonation reactions indicate that the calcination rate is still notably increased by the presence of H 2 O at very low concentrations whereas the reactivity toward carbonation and crystal structure of the formed CaO are not essentially affected, which suggests that the CaO mechanical strength is not impaired. Thus, the benefit of using steam for calcination in the CaL process could be still retained while at the same time particle attrition would not be promoted.

  12. Synthesis, molecular structure, FT-IR and XRD investigations of 2-(4-chlorophenyl)-2-oxoethyl 2-chlorobenzoate: a comparative DFT study.

    Science.gov (United States)

    Chidan Kumar, C S; Fun, Hoong Kun; Tursun, Mahir; Ooi, Chin Wei; Chandraju, Siddegowda; Quah, Ching Kheng; Parlak, Cemal

    2014-04-24

    2-(4-Chlorophenyl)-2-oxoethyl 2-chlorobenzoate has been synthesized, its structural and vibrational properties have been reported using FT-IR and single-crystal X-ray diffraction (XRD) studies. The conformational analysis, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of the synthesized compound (C15H10Cl2O3) have been examined by means of Becke-3-Lee-Yang-Parr (B3LYP) density functional theory (DFT) method together with 6-31++G(d,p) basis set. Furthermore, reliable conformational investigation and vibrational assignments have been made by the potential energy surface (PES) and potential energy distribution (PED) analyses, respectively. Calculations are performed with two possible conformations. The title compound crystallizes in orthorhombic space group Pbca with the unit cell dimensions a=12.312(5) Å, b=8.103(3) Å, c=27.565(11) Å, V=2750.0(19) Å(3). B3LYP method provides satisfactory evidence for the prediction of vibrational wavenumbers and structural parameters. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Synthesis of core-shell heterostructured Cu/Cu2O nanowires monitored by in situ XRD as efficient visible-light photocatalysts

    KAUST Repository

    Chen, Wei

    2013-01-01

    Core-shell heterostructured Cu/Cu2O nanowires with a high aspect ratio were synthesized from Cu foam using a novel oxidation/reduction process. In situ XRD was used as an efficient tool to acquire phase transformation details during the temperature-programmed oxidation of Cu foam and the subsequent reduction process. Based on knowledge of the crucial phase transformation, optimal synthesis conditions for producing high-quality CuO and core-shell Cu/Cu2O nanowires were determined. In favor of efficient charge separation induced by the special core-shell heterostructure and the advanced three-dimensional spatial configuration, Cu/Cu2O nanowires exhibited superior visible-light activity in the degradation of methylene blue. The present study illustrates a novel strategy for fabricating efficiently core-shell heterostructured nanowires and provides the potential for developing their applications in electronic devices, for environmental remediation and in solar energy utilization fields. This journal is © The Royal Society of Chemistry.

  14. XRD and SEM/EDS characterization of coconut fibers in raw and treated forms used in the treatment of strontium in aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Fonseca, Heverton C.O.; Garcia, Rafael H.L.; Ferreira, Robson J.; Silva, Flavia R.O.; Potiens Junior, Ademar J.; Sakata, Solange K., E-mail: sksakata@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2015-07-01

    {sup 90}Sr, a radioactive isotope of strontium, is one of the fission products and quite often present in the radioactive waste produced by nuclear power plants. Recently, the removal efficiency of strontium by treated coconut fibers was evaluated and reached up to 95% in an aqueous solution. This work presents the characterization of raw and treated coconut fibers with different concentrations of hydrogen peroxide in basic medium using X-ray diffraction (XRD) and scanning electron microscopy/energy dispersive spectroscopy (SEM / EDS). The analysis of X-ray diffraction shows a crystallinity of 37.6% for raw coconut fiber and crystallinity of 45.4% and 50.6% for coconut fibers 1 and 2, respectively. These results showed that the different degrees of degradation of organic matter can affect the crystallinity of the treated. This study of morphology and crystallinity of theses biosorbent materials with strontium will help in comprehension of the effects of alkaline hydrogen peroxide treatment and it will demonstrate the potential of strontium uptake by coconut fibers. (author)

  15. XRD and SEM/EDS characterization of coconut fibers in raw and treated forms used in the treatment of strontium in aqueous solution

    International Nuclear Information System (INIS)

    Fonseca, Heverton C.O.; Garcia, Rafael H.L.; Ferreira, Robson J.; Silva, Flavia R.O.; Potiens Junior, Ademar J.; Sakata, Solange K.

    2015-01-01

    90 Sr, a radioactive isotope of strontium, is one of the fission products and quite often present in the radioactive waste produced by nuclear power plants. Recently, the removal efficiency of strontium by treated coconut fibers was evaluated and reached up to 95% in an aqueous solution. This work presents the characterization of raw and treated coconut fibers with different concentrations of hydrogen peroxide in basic medium using X-ray diffraction (XRD) and scanning electron microscopy/energy dispersive spectroscopy (SEM / EDS). The analysis of X-ray diffraction shows a crystallinity of 37.6% for raw coconut fiber and crystallinity of 45.4% and 50.6% for coconut fibers 1 and 2, respectively. These results showed that the different degrees of degradation of organic matter can affect the crystallinity of the treated. This study of morphology and crystallinity of theses biosorbent materials with strontium will help in comprehension of the effects of alkaline hydrogen peroxide treatment and it will demonstrate the potential of strontium uptake by coconut fibers. (author)

  16. Analysis of sulphone based organic–inorganic hybrid epoxy nanocomposites for advanced engineering applications—Study of the mechanical, thermomechanical, XRD, EDS and physical properties

    International Nuclear Information System (INIS)

    Shree Meenakshi, K.; Pradeep Jaya Sudhan, E.; Menon, Prathibha G.

    2012-01-01

    Highlights: ► Novel sulphone based tetraglycidyl epoxy nanocomposites were developed for aerospace applications. ► Nano-reinforcements were incorporated and curing was done. ► Excellent results were obtained in the mechanical studies. The nanocomposites developed were flame retardant and hydrophobic. - Abstract: A study was made in the present investigation on sulphone containing tetraglycidyl epoxy nanocomposites to find its suitability for use in high performance applications. The synthesis and characterization of the sulphone tetraglycidyl epoxy resin denoted as ‘B’ was done as reported in our previous study. Nanoclay and POSS-amine nano-reinforcements denoted as N1 and N2 were incorporated into the synthesized epoxy resin. Curing was done with diaminodiphenylmethane (DDM) and bis(3-aminophenyl) phenylphosphine oxide (BAPPO) curing agents denoted as X and Y respectively. In our current research, we continue this research and study the mechanical, thermo-mechanical, X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), viscosity, epoxy equivalent weight (EEW) and gel permeation chromatography (GPC) studies.

  17. Length-Scale-Dependent Phase Transformation of LiFePO4 : An In situ and Operando Study Using Micro-Raman Spectroscopy and XRD.

    Science.gov (United States)

    Siddique, N A; Salehi, Amir; Wei, Zi; Liu, Dong; Sajjad, Syed D; Liu, Fuqiang

    2015-08-03

    The charge and discharge of lithium ion batteries are often accompanied by electrochemically driven phase-transformation processes. In this work, two in situ and operando methods, that is, micro-Raman spectroscopy and X-ray diffraction (XRD), have been combined to study the phase-transformation process in LiFePO4 at two distinct length scales, namely, particle-level scale (∼1 μm) and macroscopic scale (∼several cm). In situ Raman studies revealed a discrete mode of phase transformation at the particle level. Besides, the preferred electrochemical transport network, particularly the carbon content, was found to govern the sequence of phase transformation among particles. In contrast, at the macroscopic level, studies conducted at four different discharge rates showed a continuous but delayed phase transformation. These findings uncovered the intricate phase transformation in LiFePO4 and potentially offer valuable insights into optimizing the length-scale-dependent properties of battery materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Effects of uniformities of deposition of respirable particles on filters on determining their quartz contents by using the direct on-filter X-ray diffraction (DOF XRD) method.

    Science.gov (United States)

    Chen, Ching-Hwa; Tsaia, Perng-Jy; Lai, Chane-Yu; Peng, Ya-Lian; Soo, Jhy-Charm; Chen, Cheng-Yao; Shih, Tung-Sheng

    2010-04-15

    In this study, field samplings were conducted in three workplaces of a foundry plant, including the molding, demolding, and bead blasting, respectively. Three respirable aerosol samplers (including a 25-mm aluminum cyclone, nylon cyclone, and IOSH cyclone) were used side-by-side to collect samples from each selected workplace. For each collected sample, the uniformity of the deposition of respirable dusts on the filter was measured and its free silica content was determined by both the DOF XRD method and NIOSH 7500 XRD method (i.e., the reference method). A same trend in measured uniformities can be found in all selected workplaces: 25-mm aluminum cyclone>nylon cyclone>IOSH cyclone. Even for samples collected by the sampler with the highest uniformity (i.e., 25-mm aluminum cyclone), the use of the DOF XRD method would lead to the measured free silica concentrations 1.15-2.89 times in magnitude higher than that of the reference method. A new filter holder should be developed with the minimum uniformity comparable to that of NIOSH 7500 XRD method (=0.78) in the future. The use of conversion factors for correcting quartz concentrations obtained from the DOF XRD method based on the measured uniformities could be suitable for the foundry industry at this stage. 2009 Elsevier B.V. All rights reserved.

  19. The structure of ZrO2 phases and deviltrification processes in a Ca-Zr-Si-O-based glass ceramic: a combined a-XRD and XAS study

    International Nuclear Information System (INIS)

    Meneghini, C.; Mobilio, S.

    2004-01-01

    The structure of Zr atomic environment in a CaO-ZrO 2 -Si 2 glass ceramic as a function of thermal treatments has been studied, combining X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD) and anomalous XRD (a-XRD) techniques. The analysis of XRD patterns demonstrates that the devitrification process proceeds through the partial segregation of Zr-depleted phases (wollastonite-like) and Zr-rich phases (Zr oxides). The XAS and a-XRD measurements at the Zr K-edge have been exploited in order to obtain a closer insight into the atomic structure around the Zr atoms. In the as-quenched glass the Zr atom is sixfold coordinated to O atoms in an amorphous environment rich in Ca and Si. Thermal treatment firstly (T=1273-1323 K) causes partial segragation of Zr in the form of an oxide with a tetragonal zirconia (t-ZrO 2 ) crystalline structure. Raising the temperature (T=1373 K) causes the formation of ZrO 2 crystallites in the monoclinic crystallographic phase (baddeleyite, m-ZrO 2 ). Analysis of the XAS data shows that a considerable amount of Zr remains in an amorphous calcium silicate phase. (orig.)

  20. Effects of uniformities of deposition of respirable particles on filters on determining their quartz contents by using the direct on-filter X-ray diffraction (DOF XRD) method

    International Nuclear Information System (INIS)

    Chen, Ching-Hwa; Tsaia, Perng-Jy; Lai, Chane-Yu; Peng, Ya-Lian; Soo, Jhy-Charm; Chen, Cheng-Yao; Shih, Tung-Sheng

    2010-01-01

    In this study, field samplings were conducted in three workplaces of a foundry plant, including the molding, demolding, and bead blasting, respectively. Three respirable aerosol samplers (including a 25-mm aluminum cyclone, nylon cyclone, and IOSH cyclone) were used side-by-side to collect samples from each selected workplace. For each collected sample, the uniformity of the deposition of respirable dusts on the filter was measured and its free silica content was determined by both the DOF XRD method and NIOSH 7500 XRD method (i.e., the reference method). A same trend in measured uniformities can be found in all selected workplaces: 25-mm aluminum cyclone > nylon cyclone > IOSH cyclone. Even for samples collected by the sampler with the highest uniformity (i.e., 25-mm aluminum cyclone), the use of the DOF XRD method would lead to the measured free silica concentrations 1.15-2.89 times in magnitude higher than that of the reference method. A new filter holder should be developed with the minimum uniformity comparable to that of NIOSH 7500 XRD method (=0.78) in the future. The use of conversion factors for correcting quartz concentrations obtained from the DOF XRD method based on the measured uniformities could be suitable for the foundry industry at this stage.

  1. Residual stress state in an induction hardened steel bar determined by synchrotron- and neutron diffraction compared to results from lab-XRD

    International Nuclear Information System (INIS)

    Holmberg, Jonas; Steuwer, Axel; Stormvinter, Albin; Kristoffersen, Hans; Haakanen, Merja; Berglund, Johan

    2016-01-01

    Induction hardening is a relatively rapid heat treatment method to increase mechanical properties of steel components. However, results from FE-simulation of the induction hardening process show that a tensile stress peak will build up in the transition zone in order to balance the high compressive stresses close to the surface. This tensile stress peak is located in the transition zone between the hardened zone and the core material. The main objective with this investigation has been to non-destructively validate the residual stress state throughout an induction hardened component. Thereby, allowing to experimentally confirming the existence and magnitude of the tensile stress peak arising from rapid heat treatment. For this purpose a cylindrical steel bar of grade C45 was induction hardened and characterised regarding the microstructure, hardness, hardening depth and residual stresses. This investigation shows that a combined measurement with synchrotron/neutron diffraction is well suited to non-destructively measure the strains through the steel bar of a diameter of 20 mm and thereby making it possible to calculate the residual stress profile. The result verified the high compressive stresses at the surface which rapidly changes to tensile stresses in the transition zone resulting in a large tensile stress peak. Measured stresses by conventional lab-XRD showed however that at depths below 1.5 mm the stresses were lower compared to the synchrotron and neutron data. This is believed to be an effect of stress relaxation from the layer removal. The FE-simulation predicts the depth of the tensile stress peak well but exaggerates the magnitude compared to the measured results by synchrotron/neutron measurements. This is an important knowledge when designing the component and the heat treatment process since this tensile stress peak will have great impact on the mechanical properties of the final component.

  2. Mercury Retention and Accumulation by Plants at the Abandoned New Idria Mine Site - a Preliminary micro-XRF and micro-XRD Study

    Science.gov (United States)

    Siebner, H.; Webb, S. M.; Brown, G. E.

    2008-12-01

    Due to its high toxicity and increasing levels in ecosystems, Hg pollution has become a serious global problem. A lot of research has been conducted with regard to Hg biogeochemical cycles in aquatic systems. Much less is known about terrestrial Hg-cycles in general and in plants specifically. Plants play an important role in these cycles; they are known to be an important sink for both atmospheric and soil Hg, the vegetative cover significantly influences soil erosion and migration of contaminants into aquatic systems. However, the processes involved in the interactions of Hg with plants and plants products are poorly studied. Information concerning the interaction of Hg in plants at the molecular level is sparse. The present study is intended to provide new information on Hg retention, translocation, and accumulation in plants associated with mercury mine wastes in central California. We present here preliminary results of Hg distribution in root and leave samples, taken from different plant species, which have adapted to the hostile environment at the New Idria site. Samples were taken at two locations that differ in water acidity and flooding regime. The distribution of Hg appears to be affected by plant species, growing conditions, and development stage. Micro-XRF images of root sections show that Hg is mainly associated with Fe plaque at the outer surfaces and epidermis, but is distributed differently in roots of the two plants. Micro-XRD showed evidence for mineralogical changes in the plaque through the sections. Mercury in leaves was found to be highly diffuse in its distribution, and is not associated with Fe-rich particles attached to the outer surface of the leaf. This finding implies that Hg is assimilated in the leaf tissue. Further examination of Fe plaque characteristics and associated Hg, as well as Hg speciation in the different organs of these plants, is being conducted in our lab.

  3. Residual stress state in an induction hardened steel bar determined by synchrotron- and neutron diffraction compared to results from lab-XRD

    Energy Technology Data Exchange (ETDEWEB)

    Holmberg, Jonas, E-mail: jonas.holmberg@swerea.se [Swerea IVF AB, Argongatan 30, 431 22 Mölndal (Sweden); University West, 461 86 Trollhättan (Sweden); Steuwer, Axel [Nelson Mandela Metropolitan University, Gardham Avenue, 6031 Port Elizabeth (South Africa); Stormvinter, Albin; Kristoffersen, Hans [Swerea IVF AB, Argongatan 30, 431 22 Mölndal (Sweden); Haakanen, Merja [Stresstech OY, Tikkutehtaantie 1, 40 800 Vaajakoski (Finland); Berglund, Johan [Swerea IVF AB, Argongatan 30, 431 22 Mölndal (Sweden)

    2016-06-14

    Induction hardening is a relatively rapid heat treatment method to increase mechanical properties of steel components. However, results from FE-simulation of the induction hardening process show that a tensile stress peak will build up in the transition zone in order to balance the high compressive stresses close to the surface. This tensile stress peak is located in the transition zone between the hardened zone and the core material. The main objective with this investigation has been to non-destructively validate the residual stress state throughout an induction hardened component. Thereby, allowing to experimentally confirming the existence and magnitude of the tensile stress peak arising from rapid heat treatment. For this purpose a cylindrical steel bar of grade C45 was induction hardened and characterised regarding the microstructure, hardness, hardening depth and residual stresses. This investigation shows that a combined measurement with synchrotron/neutron diffraction is well suited to non-destructively measure the strains through the steel bar of a diameter of 20 mm and thereby making it possible to calculate the residual stress profile. The result verified the high compressive stresses at the surface which rapidly changes to tensile stresses in the transition zone resulting in a large tensile stress peak. Measured stresses by conventional lab-XRD showed however that at depths below 1.5 mm the stresses were lower compared to the synchrotron and neutron data. This is believed to be an effect of stress relaxation from the layer removal. The FE-simulation predicts the depth of the tensile stress peak well but exaggerates the magnitude compared to the measured results by synchrotron/neutron measurements. This is an important knowledge when designing the component and the heat treatment process since this tensile stress peak will have great impact on the mechanical properties of the final component.

  4. Karakteristik mineralisasi epitermal di Daerah Taran, Hulu Kahayan, Kalimantan Tengah berdasarkan studi mikroskopis, X-Ray Diffraction (XRD, dan inklusi fluida

    Directory of Open Access Journals (Sweden)

    Danny Zulkifli Herman

    2014-06-01

    Full Text Available http://dx.doi.org/10.17014/ijog.vol1no3.20064Taran area is occupied predominantly by piroclastic rocks and locally intercalations of lenticular claystones and sandstones. The pyroclastic rocks are intruded by diorite, dacite and andesite, leading alteration and mineralization within the host rocks. Mineralization occurs as a vein type and is associated with a number of pervasive alteration types named respectively: quartz-illite- montmorillonite-kaolinite ± pyrite, quartz-illite ± pyrite, quartz-illite-chlorite ± pyrite and quartz- kaolinite-illite ± pyrite. On the other hand, a propylitic alteration also occurs within the andesite intrusion composed of calcite-epidote-chlorite-sericite-quartz ± pyrite. The mineralization is characterized by several zones of quartz stockwork containing gold and associated ore minerals of chalcopyrite, sphalerite, galena, pyrite and argentite. The quartz veins occurs as fi llings of structural openings in the form of milky quartz and amethyst with textures of sugary, comb, and dogteeth. Evaluation work on results of microscopic (petrography and mineragraphy, X-Ray Diffraction (XRD, and fl uid inclusion studies, and chemical analysis of entirely altered rock/quartz vein samples shows that the alteration and mineralization process were closely related to a change of hydrothermal fl uids, from near neutral into acid conditions at a temperature range of >290o – 100oC. The appearances of quartz variation indicate a relationship with repeated episodes of boiling in an epithermal system, as ground water mixed with hot vapor originated from a remained post-magmatic solution. Corresponding to a salinity of average 1,388 equiv.wt.% NaCl, it indicates that the ore minerals bearing quartz veins were deposited at a depth range of 640 – 1020 m beneath paleosurface.  

  5. Synthesis, XRD single crystal structure analysis, vibrational spectral analysis, molecular dynamics and molecular docking studies of 2-(3-methoxy-4-hydroxyphenyl) benzothiazole

    Science.gov (United States)

    Sarau Devi, A.; Aswathy, V. V.; Sheena Mary, Y.; Yohannan Panicker, C.; Armaković, Stevan; Armaković, Sanja J.; Ravindran, Reena; Van Alsenoy, C.

    2017-11-01

    The vibrational spectra and corresponding vibrational assignments of 2-(3-methoxy-4-hydroxyphenyl)benzothiazole is reported. Single crystal XRD data of the title compound is reported and the orientation of methoxy group is cis to nitrogen atom of the thiazole ring. The phenyl ring breathing modes of the title compound are assigned at 1042 and 731 cm-1 theoretically. The charge transfer within the molecule is studied using frontier molecular orbital analysis. The chemical reactivity descriptors are calculated theoretically. The NMR spectral data predicted theoretically are in good agreement with the experimental data. The strong negative region spread over the phenyl rings, nitrogen atom and oxygen atom of the hydroxyl group in the MEP plot is due to the immense conjugative and hyper conjugative resonance charge delocalization of π-electrons. Molecule sites prone to electrophilic attacks have been determined by analysis of ALIE surfaces, while Fukui functions provided further insight into the local reactivity properties of title molecule. Autoxidation properties have been investigated by calculation of bond dissociation energies (BDEs) of hydrogen abstraction, while BDEs of the rest of the single acyclic bonds were valuable for the further investigation of degradation properties. Calculation of radial distribution functions was performed in order to determine which atoms of the title molecule have pronounced interactions with water molecules. The title compound forms a stable complex with aryl hydrocarbon receptor and can be a lead compound for developing new anti-tumor drug. Antimicrobial properties of the title compound was screened against one bacterial culture Escherchia coli and four fungal cultures viz., Aspergillus niger, Pencillum chrysogenum, Saccharomyces cerevisiae and Rhyzopus stolonifer.

  6. Synthesis and detection the oxidization of Co cores of Co@SiO2 core-shell nanoparticles by in situ XRD and EXAFS.

    Science.gov (United States)

    Zhang, Kunhao; Zhao, Ziyan; Wu, Zhonghua; Zhou, Ying

    2015-01-01

    In this paper, the Co@SiO2 core-shell nanoparticles were prepared by the sol-gel method. The oxidization of Co core nanoparticles was studied by the synchrotron radiation-based techniques including in situ X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS) up to 800°C in air and N2 protection conditions, respectively. It was found that the oxidization of Co cores is undergoing three steps regardless of being in air or in N2 protection condition. In the first step ranging from room temperature to 200°C, the Co cores were dominated by Co(0) state as well as small amount of Co(2+) ions. When temperature was above 300°C, the interface between Co cores and SiO2 shells was gradually oxidized into Co(2+), and the CoO layer was observed. As the temperature increasing to 800°C, the Co cores were oxidized to Co3O4 or Co3O4/CoO. Nevertheless, the oxidization kinetics of Co cores is different for the Co@SiO2 in air and N2 gas conditions. Generally, the O2 in the air could get through the SiO2 shells easily onto the Co core surface and induce the oxidization of the Co cores due to the mesoporous nature of the SiO2 shells. However, in N2 gas condition, the O atoms can only be from the SiO2 shells, so the diffusion effect of O atoms in the interface between Co core and SiO2 shell plays a key role.

  7. Proton transfer and hydrogen bonding in the organic solid state: a combined XRD/XPS/ssNMR study of 17 organic acid-base complexes.

    Science.gov (United States)

    Stevens, Joanna S; Byard, Stephen J; Seaton, Colin C; Sadiq, Ghazala; Davey, Roger J; Schroeder, Sven L M

    2014-01-21

    The properties of nitrogen centres acting either as hydrogen-bond or Brønsted acceptors in solid molecular acid-base complexes have been probed by N 1s X-ray photoelectron spectroscopy (XPS) as well as (15)N solid-state nuclear magnetic resonance (ssNMR) spectroscopy and are interpreted with reference to local crystallographic structure information provided by X-ray diffraction (XRD). We have previously shown that the strong chemical shift of the N 1s binding energy associated with the protonation of nitrogen centres unequivocally distinguishes protonated (salt) from hydrogen-bonded (co-crystal) nitrogen species. This result is further supported by significant ssNMR shifts to low frequency, which occur with proton transfer from the acid to the base component. Generally, only minor chemical shifts occur upon co-crystal formation, unless a strong hydrogen bond is formed. CASTEP density functional theory (DFT) calculations of (15)N ssNMR isotropic chemical shifts correlate well with the experimental data, confirming that computational predictions of H-bond strengths and associated ssNMR chemical shifts allow the identification of salt and co-crystal structures (NMR crystallography). The excellent agreement between the conclusions drawn by XPS and the combined CASTEP/ssNMR investigations opens up a reliable avenue for local structure characterization in molecular systems even in the absence of crystal structure information, for example for non-crystalline or amorphous matter. The range of 17 different systems investigated in this study demonstrates the generic nature of this approach, which will be applicable to many other molecular materials in organic, physical, and materials chemistry.

  8. Structural, electronic and optical properties of monoclinic Na2Ti3O7 from density functional theory calculations: A comparison with XRD and optical absorption measurements

    Science.gov (United States)

    Araújo-Filho, Adailton A.; Silva, Fábio L. R.; Righi, Ariete; da Silva, Mauricélio B.; Silva, Bruno P.; Caetano, Ewerton W. S.; Freire, Valder N.

    2017-06-01

    Powder samples of bulk monoclinic sodium trititanate Na2Ti3O7 were prepared carefully by solid state reaction, and its monoclinic P21/m crystal structure and morphology were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM), respectively. Moreover, the sodium trititanate main energy band gap was estimated as Eg=3.51±0.01 eV employing UV-Vis spectroscopy, which is smaller than the measured 3.70 eV energy gap published previously by other authors. Aiming to achieve a better understanding of the experimental data, density functional theory (DFT) computations were performed within the local density and generalized gradient approximations (LDA and GGA, respectively) taking into account dispersion effects through the scheme of Tkatchenko and Scheffler (GGA+TS). Optimal lattice parameters, with deviations relative to measurements Δa=-0.06 Å, Δb=0.02 Å, and Δc=-0.09 Å, were obtained at the GGA level, which was then used to simulate the sodium trititanate electronic and optical properties. Indirect band transitions have led to a theoretical gap energy value of about 3.25 eV. Our results, however, differ from pioneer DFT results with respect to the specific Brillouin zone vectors for which the indirect transition with smallest energy value occurs. Effective masses for electrons and holes were also estimated along a set of directions in reciprocal space. Lastly, our calculations revealed a relatively large degree of optical isotropy for the Na2Ti3O7 optical absorption and complex dielectric function.

  9. [Comporison Sduty of Microstructure by Metallographicalk on the Polarized Light and Texture by XRD of CC 5083 and CC 5182 Aluminium Alloy after Cold Rolling and Recrystallization].

    Science.gov (United States)

    Chen, Ming-biao; Li, Yong-wei; Tan, Yuan-biao; Ma, Min; Wang, Xue-min; Liu, Wen-chang

    2015-03-01

    At present the study of relation between microstructure, texture and performance of CC 5083 aluminium alloy after cold tolling and recrystallization processes is still finitude. So that the use of the CC 5083 aluminium alloy be influenced. Be cased into electrical furnace, hot up with unlimited speed followed the furnace hot up to different temperature and annealed 2h respectively, and be cased into salt-beth furnace, hot up quickly to different temperature and annealed 30 min respectively for CC 5083 and CC 5182 aluminum alloy after cold roling with 91.5% reduction. The microstructure be watched use metallographic microscope, the texture be inspected by XRD. The start temperature of recrystallization and grain grow up temperature within annealing in the electric furnace of CC 5083 aluminum alloy board is 343 degrees C, and the shap of grain after grow up with long strip (the innovation point ); The start temperature of recrystallization within annealling in the salt bath furnace of CC 5083 is 343 degrees C. The start temperature and end temperature of recrystallization within annealling of CC 5083 and CC 5182 aluminum alloy is 371 degrees C. The grain grow up outstanding of cold rooled CC 5152 aluminum alloy after annealed with 454 degrees C in the electric furnace and salt bath furnace. The start temperature of grain grow up of CC 5083 alluminurn alloy annealed in the electric furnace and salt bath furnace respectively is higher than the start temperature of grain grow up of CC 5182 alluminum alloy annealed in the electric furnace and salt bath furnace respectively. The strat temperature of recrystallization grain grow up is higher than which annealled with other three manner annealing process. The recrystallization temperature of CC 5182 annealed in the salt bath furnace is higher than which annealed in the electric furnace. The recrystallization temperature of the surface layer of CC 5083 and CC 5182 aluminum alloy is higher than the inner layer (the innovation

  10. SEM-EDS and XRD study of a NiCrAlU alloy at temperatures from 800 celsius degree to 1300 celsius degree

    International Nuclear Information System (INIS)

    Al-Badairy, H.; Fox, P.

    2004-01-01

    Full text.The oxidation behaviour of a 74.5wt%Ni, 20wt%Cr, 5wt%Al and 0.5wt%U alloy was examined using Scanning Electron Microscopy with X-ray Energy Dispersive Spectroscopy (SEM-EDS) and X-ray Diffractometry (XRD). The oxidation temperature ranged from 800 to 1300 celsius degree in laboratory air with oxidation times up to 120h. Analysis showed that during short term oxidation (40h) at the lower temperatures there was evidence of the formation of Cr, Ni and Al oxides. With increasing oxidation time, the Cr-rich oxide became predominant with the presence of islands of Ni-rich oxide, but no uranium was detected at the outermost layer of the scale. The scale was of flat topography with spallation occurring after 40h oxidation at 900 celsius degree and increasing with increasing temperature and time. Cross-sectional investigations indicated the presence of an internal oxidation zone comprising an Al-rich oxide beneath the outer Cr-rich scale with significant amounts of uranium. The depth of this zone varied from 1 micron to 60 microns and increased with increasing the oxidation temperature and time. At higher temperatures (above 1000 celsius degree), the internal oxidation zone ceased to grow due to the formation of a complete layer of alumina which protected the metal substrate from further degradation. The constituents of the scales formed reflect the selective oxidation of Cr and Al as a result of the higher reactivity of aluminium and chromium compared to nickel and the greater stability of Al 2 O 3 and Cr 2 O 3 compared to NiO. This study showed that Al-rich oxide was not the predominant protective oxide and the presence of uranium was restricted to the grain boundaries of the metal substrate and to within the internal oxidation zone. It appeared that the Cr-rich scale formed on this alloy does not to convolute. This may be due to the influence of uranium since Cr-rich scales forming on NiCrAl containing no uranium are often convoluted

  11. Formation of CuInSe{sub 2} films from metal sulfide and selenide precursor nanocrystals by gas-phase selenization, an in-situ XRD study

    Energy Technology Data Exchange (ETDEWEB)

    Capon, B., E-mail: boris.capon@ugent.be [Department of Solid State Sciences, Ghent University, Krijgslaan 281-S1, B-9000 Ghent (Belgium); Dierick, R. [Physics and Chemistry of Nanostructures, Ghent University, Krijgslaan 281-S3, B-9000 Ghent (Belgium); Hens, Z. [Physics and Chemistry of Nanostructures, Ghent University, Krijgslaan 281-S3, B-9000 Ghent (Belgium); Center for Nano and Biophotonics, Ghent University, Ghent (Belgium); Detavernier, C. [Department of Solid State Sciences, Ghent University, Krijgslaan 281-S1, B-9000 Ghent (Belgium)

    2016-08-01

    In this work phase pure CuInSe{sub 2} thin flms were obtained by selenization of ternary CuInSe{sub 2} and CuInS{sub 2} nanocrystals and mixtures of binary nanocrystals such as CuS, In{sub 2}S{sub 3}, Cu{sub 2}Se and In{sub 2}Se{sub 3}. The temperature of the selenium source was kept at 400 °C during selenization. Monitoring the process using in-situ x-ray diffraction, the effect of selenization on the phase formation and grain growth in the precursor film was investigated. Whereas CuInSe{sub 2} and CuInS{sub 2} nanocrystals exhibit little grain growth, we found that mixtures of binary nanocrystals can show significant sintering depending on the reaction conditions. For the mixture of CuS and In{sub 2}S{sub 3} nanocrystals, the crystallinity and the morphology of the obtained fims strongly depends on the Cu/In ratio, with a Cu excess strongly promoting grain growth. With mixtures of Cu{sub 2}Se and In{sub 2}Se{sub 3} nanocrystals the selenium partial pressure plays a crucial role. Selenium evaporation from the mixed compounds results in CuInSe{sub 2} films composed of relatively small crystallites. Higher selenium partial pressures however resulted in improved sintering. Incomplete propagation of the selenization reaction through the layer was observed though, only leading to a well sintered CuInSe{sub 2} top layer above a fine grained bottom layer. - Highlights: • Different types of colloidal nanocrystals were used as precursors to obtain CuInSe{sub 2} films by gas-phase selenization. • In-situ XRD was used to study the effect of selenization on the phase formation and grain growth in the precursor films. • For a mixture of binary metal sulfides the crystallinity and the morphology strongly depend on the Cu/In ratio. • Higher selenium partial pressures result in improved sintering for a mixture of binary metal selenides.

  12. Investigation on by-products of bioenergy systems (anaerobic digestion and gasification) as potential crop nutrient using FTIR, XRD, SEM analysis and phyto-toxicity test.

    Science.gov (United States)

    Kataki, Sampriti; Hazarika, Samarendra; Baruah, D C

    2017-07-01

    Success and acceptability of the bio energy conversion technology to a large extent depend upon management of the inevitable by-products generated during the conversion process. By-products can be considered favourable as organic fertilizer as they retain nutrients with varying composition depending upon input biomass. However, characteristics of these heterogeneous resources with respect to feedstock and processing conditions have to be assessed to state on their agricultural and environmental benefits. Therefore, 3 types of anaerobic digestion by-products (digestate) from surplus biomass viz. cow dung, Ipomoea carnea:cow dung (60:40 dry weight basis) and rice straw:green gram stover:cow dung (30:30:40 dry weight basis) and one gasification by-product (biochar) from rice husk are considered to understand the fertilizer prospects. Considering 3 potential application options, digestate from each feedstock option was further processed as separated solid, separated liquid and ash from solid digestates. Thus, a total of 10 by-products were investigated for understanding their prospects as fertilizer using Fourier Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Energy Dispersive X ray Spectroscopy (EDX) and phyto-toxicity test to have a broad insight in terms of their organic, mineral, elemental composition, morphological feature and potential phyto-toxicity. In general, irrespective of origin of feedstock, solid digestate, ash digestate and char showed similarity in terms of composition of functional groups with some degree of variation in relative content as reflected by FTIR analysis. Dominance of organic functional groups in separated solid digestates compared to liquid fraction indicated the former as favourable organic amendments. Quartz was the prevalent mineral phase in all separated solid, ash digestate and rice husk char. Digestates in ash phase represent more concentrated plant nutrient source with

  13. The CheMin XRD on the Mars Science Laboratory Rover Curiosity: Construction, Operation, and Quantitative Mineralogical Results from the Surface of Mars

    Science.gov (United States)

    Blake, David F.

    2015-01-01

    The Mars Science Laboratory mission was launched from Cape Canaveral, Florida on Nov. 26, 2011 and landed in Gale crater, Mars on Aug. 6, 2012. MSL's mission is to identify and characterize ancient "habitable" environments on Mars. MSL's precision landing system placed the Curiosity rover within 2 km of the center of its 20 X 6 km landing ellipse, next to Gale's central mound, a 5,000 meter high pile of laminated sediment which may contain 1 billion years of Mars history. Curiosity carries with it a full suite of analytical instruments, including the CheMin X-ray diffractometer, the first XRD flown in space. CheMin is essentially a transmission X-ray pinhole camera. A fine-focus Co source and collimator transmits a 50µm beam through a powdered sample held between X-ray transparent plastic windows. The sample holder is shaken by a piezoelectric actuator such that the powder flows like a liquid, each grain passing in random orientation through the beam over time. Forward-diffracted and fluoresced X-ray photons from the sample are detected by an X-ray sensitive Charge Coupled Device (CCD) operated in single photon counting mode. When operated in this way, both the x,y position and the energy of each photon are detected. The resulting energy-selected Co Kalpha Debye-Scherrer pattern is used to determine the identities and amounts of minerals present via Rietveld refinement, and a histogram of all X-ray events constitutes an X-ray fluorescence analysis of the sample.The key role that definitive mineralogy plays in understanding the Martian surface is a consequence of the fact that minerals are thermodynamic phases, having known and specific ranges of temperature, pressure and composition within which they are stable. More than simple compositional analysis, definitive mineralogical analysis can provide information about pressure/temperature conditions of formation, past climate, water activity and the like. Definitive mineralogical analyses are necessary to establish

  14. Effect of polishing instruments and polishing regimens on surface topography and phase transformation of monolithic zirconia: An evaluation with XPS and XRD analysis.

    Science.gov (United States)

    Al-Haj Husain, Nadin; Camilleri, Josette; Özcan, Mutlu

    2016-12-01

    Polishing procedures might alter monolithic zirconia (MZ) surface resulting in phase changes that can be deleterious for clinical performance and antagonist tooth wear. This study investigated the topographical features and phase transformation in MZ after polishing with different regimens simulating the clinical workflow. ​ MZ specimens (Katana Zirconia HT, Kuraray-Noritake) (12×12×1.8 mm(3)) were grinded and polished using one of the five systems assessed: BG: Silicone carbide polishers (Brownie, Greenie, Super Greenie); CG: Diamond impregnated ceramic polisher kit (Ceragloss); EV: Synthetically bonded grinder interspersed with diamond (EVE Kit); SL: Urethane coated paper with aluminium oxide grits (Soflex Finishing and Polishing System Kit) and DB: Diamond bur (8 µm). Polished specimens were initially roughened with 220 µm diamond burs (Grinding Bur-GB) (10 s, 160.000160,000 rpm) and considered for baseline measurements. Polishing regimens were performed for 10 s using a slow-speed hand piece under water-cooling except for SL, in a custom made device (750 g; 5000 and 75,000 rpm). Surface roughnesses, phase changes (XRD) were assessed, surface characterization was performed (SEM, EDS). The highest roughness was obtained with the EV system (1.11 µm) compared to those of other systems (0.13-0.4 µm) (pθ and minor peak at 34.94°2θ. While GB, CG, EV, SL and DB exhibited a peak shift to the left, BG demonstrated a right peak shift on the 2θ scale. Monoclinic phase change was not noted in any of the groups. All polishing methods, except BG, exhibited a peak shift towards the lower angles of the 2-theta scale. Since the peak shifts were in the order of fractions of an angle they are attributed to stress formation rather than a phase change in the material. Thus, all polishing systems tested may not be detrimental for the phase transformation of MZ. EV system resulted in the highest roughness and none of the polishing regimens restored the polishability to the

  15. Hodnocení středověké keramiky z Lažan u Chrudimi pomocí analýz XRF, XRD, OM, DSC-TG a RS

    Czech Academy of Sciences Publication Activity Database

    Kloužková, A.; Zemenová, P.; Frolík, Jan; Svobodová, Ljuba

    2014-01-01

    Roč. 39, č. 1 (2014), s. 75-87 ISSN 0231-5823. [Mezinárodní konference archeologie středověku /45./. Kutná Hora, 16.09.2013-19.09.2013] Institutional support: RVO:67985912 Keywords : pottery * Lažany * XRD, XRF, DSC analyses Subject RIV: AC - Archeology, Anthropology, Ethnology

  16. Commissioning and experience in stripping, filtering and measuring the 4.2 MeV/u lead ion beam at CERN Linac 3

    International Nuclear Information System (INIS)

    Lasheras, N. Catalan; Crescenti, M.; Vretenar, M.

    1996-01-01

    The new CERN Heavy Ion Linac (Linac3) accelerates a Pb 27+ beam to 4.2 MeV/u. The beam is then stripped to Pb 53+ by a carbon foil, and, after stripping, a 12 m filter line prepares the beam for the injection into the Proton Synchrotron Booster (PSB). The filter line eliminates the unwanted charge states, checks the beam quality (energy, energy spread, transverse emittance and intensity), and finally transports the beam in the lines leading to the PSB. The paper summarises the transverse beam dynamics of the line, and reports on its commissioning, especially focusing on the experiments that led to the stripper choice, and on the measurements performed with a specially developed single pulse multislit emittance device. The operational experience is also reported. (author)

  17. Studies on the self-catalyzed Knoevenagel condensation, characterization, DPPH radical scavenging activity, cytotoxicity, and molecular properties of 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones using single crystal XRD and DFT techniques

    Science.gov (United States)

    Suresh Kumar, G. S.; Antony Muthu Prabhu, A.; Bhuvanesh, N.

    2014-10-01

    We have studied the self-catalyzed Knoevenagel condensation, spectral characterization, DPPH radical scavenging activity, cytotoxicity, and molecular properties of 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones using single crystal XRD and DFT techniques. In the absence of any catalyst, a series of novel 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones were synthesized using Meldrum’s acid and formylphenoxyaliphatic acid(s) in water. These molecules are arranged in the dimer form through intermolecular H-bonding in the single crystal XRD structure. Compounds have better DPPH radical scavenging activity and cytotoxicity against A431 cancer cell line. The optimized molecular structure, natural bond orbital analysis, electrostatic potential map, HOMO-LUMO energies, molecular properties, and atomic charges of these molecules have been studied by performing DFT/B3LYP/3-21G(*) level of theory in gas phase.

  18. Identification of the silver state in the framework of Ag-containing zeolite by XRD, FTIR, photoluminescence, 109Ag NMR, EPR, DR UV-vis, TEM and XPS investigations.

    Science.gov (United States)

    Popovych, Nataliia; Kyriienko, Pavlo; Soloviev, Sergiy; Baran, Rafal; Millot, Yannick; Dzwigaj, Stanislaw

    2016-10-26

    Silver has been identified in the framework of Ag x SiBEA zeolites (where x = 3-6 Ag wt%) by the combined use of XRD, 109 Ag MAS NMR, FTIR, diffuse reflectance UV-visible, EPR and XPS spectroscopy. The incorporation of Ag ions into the framework of SiBEA zeolite has been evidenced by XRD. The consumption of OH groups as a result of their reaction with the silver precursor has been monitored by FTIR and photoluminescence spectroscopy. The changes in the silver state as a function of Ag content and thermal and hydrogen treatment at 573 K have been identified by 109 Ag MAS NMR, EPR, DR UV-visible, TEM and XPS investigations. The acidity of AgSiBEA has been investigated by FTIR spectroscopy of adsorbed CO and pyridine used as probe molecules.

  19. XRD study of yttria stabilized zirconia irradiated with 7.3 MeV Fe, 10 MeV I, 16 MeV Au, 200 MeV Xe and 2.2 GeV Au ions

    Energy Technology Data Exchange (ETDEWEB)

    Nakano, K.; Yoshizaki, H. [Department of Materials Science, Osaka Prefecture University, Sakai, Osaka 599-8531 (Japan); Saitoh, Y. [Takasaki Advanced Radiation Research Institute, Japan Atomic Energy Agency, Takasaki, Gunma 370-1292 (Japan); Ishikawa, N. [Tokai Research and Development Center, Tokai-mura, Naka-gun, Ibaraki 319-1195 (Japan); Iwase, A., E-mail: iwase@mtr.osakafu-u.ac.jp [Department of Materials Science, Osaka Prefecture University, Sakai, Osaka 599-8531 (Japan)

    2016-03-01

    To simulate energetic neutron irradiation effects, yttria-stabilized zirconia (YSZ) which is one of the major materials for electrical corrosion potential sensors (ECP sensors) was irradiated with heavy ions at energies ranging from 7.3 MeV to 2.2 GeV. Ion irradiation effects on the lattice structure were analyzed using the X-ray diffraction (XRD). The increase in lattice constant was induced by the ion irradiation. It was dominated by the elastic collision process and not by the electronic excitation process. The lattice disordering which was observed as a broadening of XRD peaks was also induced by the irradiation especially for 200 MeV Xe ion irradiation. The present result suggests that the expansion and/or the disordering of YSZ lattice induced by energetic neutrons may affect the durability of a joint interface between a metal housing and YSZ membrane for the usage of ECP sensors in nuclear power reactors.

  20. XRD and solid state 13C-NMR evaluation of the crystallinity enhancement of 13C-labeled bacterial cellulose biosynthesized by Komagataeibacter xylinus under different stimuli: A comparative strategy of analyses.

    Science.gov (United States)

    Meza-Contreras, Juan C; Manriquez-Gonzalez, Ricardo; Gutiérrez-Ortega, José A; Gonzalez-Garcia, Yolanda

    2018-05-22

    The production and crystallinity of 13 C bacterial cellulose (BC) was examined in static culture of Komagataeibacter xylinus with different chemical and physical stimuli: the addition of NaCl or cloramphenicol as well as exposure to a magnetic field or to UV light. Crystalline BC biosynthesized under each stimulus was studied by XRD and solid state 13 C NMR analyses. All treatments produced BC with enhanced crystallinity over 90% (XRD) and 80% (NMR) compared to the control (83 and 76%, respectively) or to Avicel (77 and 62%, respectively). The XRD data indicated that the crystallite size was 80-85 Å. Furthermore, changes on the allomorphs (I α and I β ) ratio tendency of BC samples addressed to the stimuli were estimated using the C4 signal from 13 C NMR data. These results showed a decrease of the allomorph I α (3%) when BC was biosynthesized with UV light and chloramphenicol compared to control (58.79%). In contrast, the BC obtained with NaCl increased up to 60.31% of the I α allomorph ratio. Copyright © 2018 Elsevier Ltd. All rights reserved.

  1. The new insight into the structure-activity relation of Pd/CeO2-ZrO2-Nd2O3 catalysts by Raman, in situ DRIFTS and XRD Rietveld analysis.

    Science.gov (United States)

    Yang, X; Yang, L; Lin, J; Zhou, R

    2016-01-28

    Pd/CeO2-ZrO2-Nd2O3 (CZN) catalysts with different CeO2/ZrO2 molar ratios were synthesized and have been characterized by multiple techniques, e.g. XRD in combination with Rietveld refinement, UV-Raman, XPS and in situ DRIFTS. The XRD pattern of CZN with CeO2/ZrO2 molar ratios ≥1/2 can be indexed satisfactorily to the fluorite structure with a space group Fm3̄m, while the XRD patterns of CZ12 only display diffraction peaks of the tetragonal phase (S.G. P42/nmc). Nd addition can effectively stabilize the cubic structure of the CZN support and increase the enrichment of defect sites on the surface, which may be related to the better catalytic activity of Pd/CZN12 catalysts compared with Pd/CZ12. The presence of moderate ZrO2 can increase the concentration of O* active species, leading to accelerate the formation of nitrate species and thus enhance the catalytic activity of NOx and HC elimination. The Pd-dispersion decreases with the increasing Zr content, leading to the decreased CO catalytic activity, especially for the aged catalysts. The change regularity of the OSC value is almost the same with the in situ dynamic operational window, demonstrating that the in situ dynamic operational window is basically affected by the OSC value.

  2. Microgravity and bone cell mechanosensitivity: FLOW experiment during the DELTA mission

    Science.gov (United States)

    Bacabac, Rommel G.; Van Loon, Jack J. W. A.; de Blieck-Hogervorst, Jolanda M. A.; Semeins, Cor M.; Zandieh-Doulabi, Behrouz; Helder, Marco N.; Smit, Theo H.; Klein-Nulend, Jenneke

    2007-09-01

    The catabolic effects of microgravity on mineral metabolism in bone organ cultures might be explained as resulting from an exceptional form of disuse. It is possible that the mechanosensitivity of bone cells is altered under near weightlessness conditions, which likely contributes to disturbed bone metabolism observed in astronauts. In the experiment "FLOW", we tested whether the production of early signaling molecules that are involved in the mechanical load-induced osteogenic response by bone cells is changed under microgravity conditions. FLOW was one of the Biological experiment entries to the Dutch Soyuz Mission "DELTA" (Dutch Expedition for Life Science, Technology and Atmospheric Research). FLOW was flown by the Soyuz craft, launched on April 19, 2004, on its way to the International Space Station. Primary osteocytes, osteoblasts, and periosteal fibroblasts were incubated in plunger boxes, developed by Centre for Concepts in Mechatronics, using plunger activation events for single pulse fluid shear stress stimulations. Due to unforeseen hardware complications, results from in-flight cultures are considered lost. Ground control experiments showed an accumulative increase of NO in medium for osteocytes (as well as for osteoblasts and periosteal fibroblasts). Data from the online-NO sensor showed that the NO produced in medium by osteocytes increased sharply after pulse shear stress stimulations. COX-2 mRNA expression revealed high levels in osteoblasts compared to the other cell types tested. In conclusion, preparations for the FLOW experiment and preliminary ground results indicate that the FLOW setup is viable for a future flight opportunity.

  3. Metal based pharmacologically active complexes of Cu(II), Ni(II) and Zn(II): synthesis, spectral, XRD, antimicrobial screening, DNA interaction and cleavage investigation.

    Science.gov (United States)

    Raman, Natarajan; Mahalakshmi, Rajkumar; Arun, T; Packianathan, S; Rajkumar, R

    2014-09-05

    The present contribution reports a thorough characterization of newly obtained metallointercalators incorporating Schiff bases, formed by the condensation of N-acetoacetyl-o-toluidine with 1-amino-4-nitrobenzene (L(1))/1-amino-4-chlorobenzene (L(2)) as main ligand and 1,10-phenanthroline as co-ligand respectively. The characterization of newly formed metallointercalators has been done by (1)H NMR, UV-Vis, IR, EPR spectroscopy and molar conductivity studies. X-ray powder diffraction illustrates that they are crystalline nature. Binding interaction of these complexes with calf thymus (CT-DNA) has been investigated by emission, absorption, viscosity, cyclic voltammetry and differential pulse voltammetry. DNA binding experiments results reveal that the synthesized complexes interact with DNA through intercalative mode. The in vitro antibacterial and antifungal assay indicate that these complexes are good antimicrobial agents against various pathogens. The DNA cleavage exhibits that they act as efficient cleaving agents. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Generation of femtosecond electron single pulse using laser photocathode RF gun

    Energy Technology Data Exchange (ETDEWEB)

    Uesaka, M.; Kinoshita, K.; Watanabe, T. [Nuclear Engineering Research Laboratory, University of Tokyo, Tokai, Ibaraki (JP)] [and others

    1998-11-01

    A new laser photocathode RF electron gun was installed in the second linac of the S-band twin linac system of Nuclear Engineering Research Laboratory(NERL) of University of Tokyo in August in 1997. Since then, the behavior of the new gun has been tested and the characteristic parameters have been evaluated. At the exit of the gun, the energy is 4.7 MeV, the charge per bunch 1 nC, the pulse width is 10 ps(FWHM), respectively, for 6 MW RF power supply from a klystron. The electron bunch is accelerated up to 17 MeV. The horizontal normalized emittance is 1 {pi} mm.mrad. Then, the bunch is compressed to be 440 fs(FWHM) with 0.35 nC by the chicane-type magnetic pulse compressor. The gun is planned to be used for femtosecond X-ray generation via the head-on Thomson scattering and laser wakefield acceleration in 1998. (author)

  5. Updating the induction module from single-pulse to double-pulses

    International Nuclear Information System (INIS)

    Huang Ziping; Wang Huacen; Deng Jianjun

    2002-01-01

    A double-pulse Linear Induced Accelerator (LIA) module is reconstructed based on a usual simple-pulse LIA module. By changing the length of one of the cables between the inductive cell and the Blumlein pulse forming line, two induction pulses with 90 ns FWHM and 150 kV pulse voltage are generated by the ferrite cores inductive cell. The interval time of the pulses is adjustable by changing the lengths of the cable

  6. Mechanism of single-pulse ablative generation of laser-induced periodic surface structures

    Czech Academy of Sciences Publication Activity Database

    Shugaev, M.V.; Gnilitskyi, I.; Bulgakova, Nadezhda M.; Zhigilei, L.

    2017-01-01

    Roč. 96, č. 20 (2017), s. 1-9, č. článku 205429. ISSN 2469-9950 R&D Projects: GA MŠk LO1602; GA ČR GA16-12960S; GA MŠk LM2015086 EU Projects: European Commission(XE) 739573 - HiLASE CoE Grant - others:OP VVV - HiLASE-CoE(XE) CZ.02.1.01/0.0/0.0/15_006/0000674 Institutional support: RVO:68378271 Keywords : molecular-dynamics simulations * metals * electron * spallation Subject RIV: BH - Optics, Masers, Lasers OBOR OECD: Optics (including laser optics and quantum optics) Impact factor: 3.836, year: 2016

  7. Transverse emittance measurement of high-current single pulse beams using pepper-pot method

    International Nuclear Information System (INIS)

    Ke Jianlin; Zhou Changgeng; Qiu Rui

    2013-01-01

    A pepper pot-imaging plate system has been developed and used to measure the 4-D transverse emittance of a vacuum arc ion source. Single beam pulses of tens to hundreds milliamperes were extracted from the plasma with 64 kV high voltage. An imaging plate was laid after the pepper pot to visualize the ion beamlets passing though the holes on the pepper pot. An application program was developed to show the phase-space distribution and calculate the ellipse and RMS emittances. The normalized RMS emittances are about 6.41 π·mm·mrad in x-direction and 4.61 π·mm·mrad in y-direction. It is shown that the emittance of the vacuum arc ion source is much larger than that of other types of ion sources, which is mainly attributed to the high current and the convex meniscus of this source. (authors)

  8. A Single Pulse Beam Emittance Measurement for the CERN Heavy Ion Linac

    CERN Document Server

    Crescenti, M

    1995-01-01

    A new device for transverse emittance measurement has been installed in the 4.2 MeV/u filter region of the CERN Heavy Ion Linac (Linac 3). It allows to obtain pulse-to-pulse (every 1.2 sec) visualisation of the Linac 3 beam parameters in order to tune the machine and to match the beam for injection into the first circular accelerator, the PS Booster. The system is based on the "multi-slit" technique similar to the well-known "pepper pot" method. A plate with a series of horizontal or vertical slits is placed in the beam, defining positions in the phase plane. Particles pass through the slits and drift to a scintillator screen where they produce light. The screen is looked at by an externally triggered high resolution CCD camera. For each slit position the light intensity distribution, in the limit of infinitesimal slit aperture, is proportional to the angle distribution of the particles and therefore, provides the angular distribution in the phase plane. The video signal from the camera is digitised and the r...

  9. Transcranial magnetic stimulation: no effect on mood with single pulse during learned helplessness.

    Science.gov (United States)

    Habel, U; Wild, B; Topka, H; Kircher, T; Salloum, J B; Schneider, F

    2001-04-01

    1. Transcranial Magnetic Stimulation (TMS) is suggested to be an effective tool in the treatment of depression. However, the methodology most suitable for clinical application remains unclear. 2. The effect of TMS was tested in a double-blind and placebo-controlled setting on 18 healthy subjects. At the same time an established learned helplessness paradigm was applied to induce dysphoria, which consisted of unsolvable anagrams. 3. Sixty 0.5 Hz stimuli were administered at an intensity of 130% of the subject's motor threshold after the subjects were exposed to the learned helplessness situation. Using a vertically positioned coil, the stimuli were applied to the right or to the left frontal cortex, or on the occipital cortex as a placebo condition. 4. Although dysphoria was successfully induced by unsolvable anagrams, TMS on either of the two frontal locations did not influence mood. This lack of effect may be due to the stimulation characteristics employed here (low TMS intensity, and low frequency). On the other hand, the findings may reflect the neurobiological difference between experimentally induced sad mood and clinical depression.

  10. Single-Pulse Dual-Energy Mammography Using a Binary Screen Coupled to Dual CCD Cameras

    Science.gov (United States)

    1999-08-01

    Fossum, "Active pixel sensors—Are CCD’s Dinosaurs ?," Proc. SPIE 1900, 2-14 (1993). "S. Mendis, S. E. Kemeny, R. Gee, B. Pain, and E. R. Fossum, "Progress...Clin Oncol 13:1470-1477, 1995 12. Wahl RL, Zasadny K, Helvie M, et al: Metabolic monitoring of breast cancer chemohormonotherapy using posi- tron

  11. Single pulse two photon fluorescence lifetime imaging (SP-FLIM) with MHz pixel rate.

    Science.gov (United States)

    Eibl, Matthias; Karpf, Sebastian; Weng, Daniel; Hakert, Hubertus; Pfeiffer, Tom; Kolb, Jan Philip; Huber, Robert

    2017-07-01

    Two-photon-excited fluorescence lifetime imaging microscopy (FLIM) is a chemically specific 3-D sensing modality providing valuable information about the microstructure, composition and function of a sample. However, a more widespread application of this technique is hindered by the need for a sophisticated ultra-short pulse laser source and by speed limitations of current FLIM detection systems. To overcome these limitations, we combined a robust sub-nanosecond fiber laser as the excitation source with high analog bandwidth detection. Due to the long pulse length in our configuration, more fluorescence photons are generated per pulse, which allows us to derive the lifetime with a single excitation pulse only. In this paper, we show high quality FLIM images acquired at a pixel rate of 1 MHz. This approach is a promising candidate for an easy-to-use and benchtop FLIM system to make this technique available to a wider research community.

  12. X-ray topographic investigation of the deformation field around spots irradiated by FLASH single pulses

    Czech Academy of Sciences Publication Activity Database

    Wierzchowski, W.; Wieteska, K.; Balcer, T.; Klinger, D.; Sobierajski, R.; Zymierska, D.; Chalupský, Jaromír; Hájková, Věra; Burian, Tomáš; Gleeson, A.J.; Juha, Libor; Tiedtke, K.; Toleikis, S.; Vyšín, Luděk; Wabnitz, H.; Gaudin, J.

    2011-01-01

    Roč. 80, č. 10 (2011), s. 1036-1040 ISSN 0969-806X R&D Projects: GA AV ČR KAN300100702; GA MŠk LC510; GA ČR(CZ) GAP108/11/1312; GA MŠk(CZ) LC528; GA MŠk LA08024; GA AV ČR IAAX00100903; GA MŠk(CZ) ME10046 Institutional research plan: CEZ:AV0Z10100523 Keywords : silicon * FLASH irradiation * x-ray topography * deformation fields Subject RIV: BH - Optics, Masers, Lasers Impact factor: 1.227, year: 2011

  13. In situ solid-state NMR and XRD studies of the ADOR process and the unusual structure of zeolite IPC-6

    Science.gov (United States)

    Morris, Samuel A.; Bignami, Giulia P. M.; Tian, Yuyang; Navarro, Marta; Firth, Daniel S.; Čejka, Jiří; Wheatley, Paul S.; Dawson, Daniel M.; Slawinski, Wojciech A.; Wragg, David S.; Morris, Russell E.; Ashbrook, Sharon E.

    2017-10-01

    The assembly-disassembly-organization-reassembly (ADOR) mechanism is a recent method for preparing inorganic framework materials and, in particular, zeolites. This flexible approach has enabled the synthesis of isoreticular families of zeolites with unprecedented continuous control over porosity, and the design and preparation of materials that would have been difficult—or even impossible—to obtain using traditional hydrothermal techniques. Applying the ADOR process to a parent zeolite with the UTL framework topology, for example, has led to six previously unknown zeolites (named IPC-n, where n = 2, 4, 6, 7, 9 and 10). To realize the full potential of the ADOR method, however, a further understanding of the complex mechanism at play is needed. Here, we probe the disassembly, organization and reassembly steps of the ADOR process through a combination of in situ solid-state NMR spectroscopy and powder X-ray diffraction experiments. We further use the insight gained to explain the formation of the unusual structure of zeolite IPC-6.

  14. In-Class Quantification of the Mentos and Diet Coke Analogue Experiment: Effects of Wind on Volcanic Isopach Patterns

    Science.gov (United States)

    Quane, S.; Klos, Z.; Jacobsen, R.

    2009-05-01

    The Mentos and Diet Coke experiment, where instantaneous emplacement of Mentos candy in Diet Coke creates a soda/CO2 eruptive plume, is a common educational analogue for a volcanic eruption. In this paper, we quantify the effects of varying directional wind speeds on the eruptive plume as a learning tool in advanced Introductory Geology and Volcanology courses. The Mentos and Diet Coke reaction is a fun, safe and affordable analogue for explosive, single pulse, basaltic eruptions (e.g., Strombolian eruptions). Specifically, the physical and chemical reaction nucleating CO2 bubbles on the pitted surface of Mentos candy is directly analogous to the collapsing foam eruption regime described by Parfitt (2004) where inertia driven fragmentation of the liquid (Namiki and Manga, 2008) leads to basaltic pyroclastic eruptions. Often, in these systems, the pyroclasts are carried downwind, resulting lopsided (downwind side taller) cinder cones. In our experiments, we create a single pulse eruption by simultaneously dropping four Mentos candies into a 16.9 oz. bottle of Diet Coke. The experiments are run under different wind conditions created by three stacked box fans in the off (control experiment) low, medium and high settings. Wind speed is measured using a hand held anemometer. The pyroclast dispersal is recorded by degree of liquid saturation through four layers of newspaper. The liquid is allowed to soak in for thirty seconds post eruption and then the individual layers of newspaper are separated and the saturation envelope is traced with a black marker and digitally photographed. The pyroclast dispersal envelope (or saturation area) is then quantified from the photos by image analysis in Adobe Photoshop. In addition, the experiments are videotaped to quantify ejection velocity using frame by frame analysis in iMovie. The resulting isopach ("deposit thickness") maps indicate a strong tightening of dispersal envelopes with increasing wind speed as seen in natural

  15. Synthesis of nanostructured iron oxides dispersed in carbon materials and in situ XRD study of the changes caused by thermal treatment

    Energy Technology Data Exchange (ETDEWEB)

    Gonçalves, Gustavo R.; Schettino, Miguel A. [Federal University of Espírito Santo, Laboratory of Carbon and Ceramic Materials, Department of Physics (Brazil); Morigaki, Milton K. [Federal University of Espírito Santo, Department of Chemistry (Brazil); Nunes, Evaristo; Cunha, Alfredo G.; Emmerich, Francisco G. [Federal University of Espírito Santo, Laboratory of Carbon and Ceramic Materials, Department of Physics (Brazil); Passamani, Edson C. [Federal University of Espírito Santo, Laboratory of Magnetometry and Mössbauer Spectroscopy, Department of Physics (Brazil); Baggio-Saitovitch, Elisa [Brazilian Center for Physical Research (CBPF) (Brazil); Freitas, Jair C. C., E-mail: jairccfreitas@yahoo.com.br [Federal University of Espírito Santo, Laboratory of Carbon and Ceramic Materials, Department of Physics (Brazil)

    2015-07-15

    Carbon-based magnetic nanocomposites are of large interest for applications in catalysis, magnetic separation, water cleaning, and magnetic resonance imaging, among others. This work describes the synthesis of nanocomposites consisting of iron oxides dispersed into a char (obtained from the carbonization at 700 °C of a lignocellulosic precursor) and the study of the thermal transformations occurring in these materials as a consequence of heat treatments. The materials were prepared by impregnation of the char with iron nitrate in the presence of ammonium hydroxide in aqueous suspension. X-ray diffraction experiments performed using synchrotron radiation and Mössbauer spectroscopy showed that the as-prepared material was composed of amorphous Fe{sup 3+} oxides. Scanning electron microscopy images combined with energy-dispersive X-ray spectrometry indicated a homogeneous dispersion of iron oxides and of silica particles (naturally present in the lignocellulosic precursor) throughout the char. X-ray diffractograms recorded in situ during the heat treatment of the as-prepared material showed the presence of small hematite crystallites (average size ∼22 nm) starting from ca. 300 °C. Further heating caused a progressive growth of the hematite crystallites up to ca. 500 °C, when the conversion to magnetite (Fe{sub 3}O{sub 4}) started to take place. At higher temperatures, wüstite (Fe{sub 1−x}O) was detected as an intermediate phase and austenitic iron (γ-Fe) became the dominant phase at temperatures from 900 °C. A steep weight loss was observed in the TG curve accompanying this last reduction stage; upon cooling, γ-Fe was converted into α-Fe (ferrite), which was the dominant phase at room temperature in this heat-treated sample.

  16. Synthesis of nanostructured iron oxides dispersed in carbon materials and in situ XRD study of the changes caused by thermal treatment

    Science.gov (United States)

    Gonçalves, Gustavo R.; Schettino, Miguel A.; Morigaki, Milton K.; Nunes, Evaristo; Cunha, Alfredo G.; Emmerich, Francisco G.; Passamani, Edson C.; Baggio-Saitovitch, Elisa; Freitas, Jair C. C.

    2015-07-01

    Carbon-based magnetic nanocomposites are of large interest for applications in catalysis, magnetic separation, water cleaning, and magnetic resonance imaging, among others. This work describes the synthesis of nanocomposites consisting of iron oxides dispersed into a char (obtained from the carbonization at 700 °C of a lignocellulosic precursor) and the study of the thermal transformations occurring in these materials as a consequence of heat treatments. The materials were prepared by impregnation of the char with iron nitrate in the presence of ammonium hydroxide in aqueous suspension. X-ray diffraction experiments performed using synchrotron radiation and Mössbauer spectroscopy showed that the as-prepared material was composed of amorphous Fe3+ oxides. Scanning electron microscopy images combined with energy-dispersive X-ray spectrometry indicated a homogeneous dispersion of iron oxides and of silica particles (naturally present in the lignocellulosic precursor) throughout the char. X-ray diffractograms recorded in situ during the heat treatment of the as-prepared material showed the presence of small hematite crystallites (average size 22 nm) starting from ca. 300 °C. Further heating caused a progressive growth of the hematite crystallites up to ca. 500 °C, when the conversion to magnetite (Fe3O4) started to take place. At higher temperatures, wüstite (Fe1-xO) was detected as an intermediate phase and austenitic iron (γ-Fe) became the dominant phase at temperatures from 900 °C. A steep weight loss was observed in the TG curve accompanying this last reduction stage; upon cooling, γ-Fe was converted into α-Fe (ferrite), which was the dominant phase at room temperature in this heat-treated sample.

  17. Real time observation of phase formations by XRD during Ga-rich or In-rich Cu(In, Ga)Se{sub 2} growth by co-evaporation

    Energy Technology Data Exchange (ETDEWEB)

    Pistor, Paul; Zahedi-Azad, Setareh; Hartnauer, Stefan; Waegele, Leonard A.; Jarzembowski, Enrico; Scheer, Roland [Institute of Physics, Martin-Luther-University Halle-Wittenberg, Halle (Saale) (Germany)

    2015-09-15

    Solar cells with Cu(In, Ga)Se{sub 2} absorbers rely on the three-stage co-evaporation process with Cu-poor/Cu-rich/Cu-poor absorber deposition conditions for highest efficiency devices. During the three-stage process, the formation and evolution of different selenide phases with changing compositions throughout the process crucially determine the final absorber quality. In this contribution, we monitor the evolution of crystalline phases in real-time with an X-ray diffraction (XRD) line detector setup implemented into an evaporation setup. Using the common three-stage process, we prepare and compare samples covering the full alloying range from CuInSe{sub 2} to CuGaSe{sub 2}. The in situ XRD allows the detection of the crystalline phases present at all times of the process as well as an advanced analysis of the phase evolution through a closer look at peak shifts and the full width at half maximum. For samples with a Ga/(Ga + In) ratio (GGI) < 0.5, distinct phase transitions associated with the transition to the reported vacancy compounds Cu(In,Ga){sub 5}Se{sub 8} and Cu(In, Ga){sub 3}Se{sub 5} are observed. No such indication was found for samples with a GGI > 0.5. For Ga-rich Cu(In, Ga)Se{sub 2} phases with a GGI of 0.55, the XRD analysis evidenced a Ga-rich phase segregation before the stoichiometric point was reached. The above findings are discussed in view of their implication on wide gap solar cell performances. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  18. XRD and DSC study of the formation and the melting of a new zeolite like borosilicate CsBSi5O12 and (Cs,Rb)BSi5O12 solid solutions

    International Nuclear Information System (INIS)

    Bubnova, R.S.; Ugolkov, V.L.; Krzhizhanovskaya, M.G.; Filatov, S.K.; Paufler, P.

    2007-01-01

    Polycrystalline CsBSi 5 O 12 was prepared from a stoichiometric mixture by solid-state reaction above 1000 C. The solid solutions Cs 1-x Rb x BSi 5 O 12 were obtained at 1000 C during a long heat treatment of polycrystalline Cs 1-x Rb x BSi 2 O 6 boropollucites (x Rb = 0, 0.05, 0.2, 0.4). A new borosilicate compound and its solid solutions were studied using X-ray powder diffraction (XRD), annealing, differential scanning calorimetry (DSC), and thermogravimetry (TG). For Cs,Rb-boropollucites the new phase formation is accompanied by significant mass losses detected by DSC and TG. The following mechanism of phase transformations is assumed: (Cs,Rb)BSi 2 O 6 → (Cs,Rb)BSi 5 O 12 + (Cs,Rb)BO 2 ↑. The zeolite phase forms as a result of the boropollucite decomposition over 1000 C. Zeolite decomposes also on further heating and the SiO 2 reflections are observed in the XRD pattern only. Thus above 1000 C both boropollucite and zeolite phases are unstable presumably due to the ability of the alkali cations to leave the structure. Using XRD the unit cell parameters of CsBSi 5 O 12 have been determined in the orthorhombic crystal system: a = 16.242(4) A, b = 13.360(4) A, c = 4.874(1) A. The compound is isostructural with the zeolite compound CsAlSi 5 O 12 . In the crystal structure of Cs 1-x Rb x BSi 5 O 12 solid solutions the changes of cell parameters are insignificant under the substitution of Cs by Rb atoms that indicates a very limited substitution range. (orig.)

  19. Characterization of electron beam deposited thin films of HfO2 and binary thin films of (HfO2:SiO2) by XRD and EXAFS measurements

    International Nuclear Information System (INIS)

    Das, N.C.; Sahoo, N.K.; Bhattacharyya, D.; Thakur, S.; Kamble, N.M.; Nanda, D.; Hazra, S.; Bal, J.K.; Lee, J.F.; Tai, Y.L.; Hsieh, C.A.

    2009-10-01

    In this report, we have discussed the microstructure and the local structure of composite thin films having varying hafnia and silica compositions and prepared by reactive electron beam evaporation. XRD and EXAFS studies have confirmed that the pure hafnium oxide thin film has crystalline microstructure whereas the films with finite hafnia and silica composition are amorphous. The result of EXAFS analysis has shown that the bond lengths as well as coordination numbers around hafnium atom change with the variation of hafnia and silica compositions in the thin film. Finally, change of bond lengths has been correlated with change of refractive index and band gap of the composite thin films. (author)

  20. Customer experience

    OpenAIRE

    Koperdáková, Zuzana

    2016-01-01

    Bachelor thesis deals with the theme of customer experience and terms related to this topic. The thesis consists of three parts. The first part explains the terms generally, as the experience or customer loyalty. The second part is dedicated to medotology used for Customer Experience Management. In the third part is described application of Customer Experience Management in practice, particularly in the context Touch Point Analyses in GE Money Bank.

  1. Fe K-Edge X-ray absorption near-edge spectroscopy (XANES) and X-ray diffraction (XRD) analyses of LiFePO4 and its base materials

    Science.gov (United States)

    Latif, C.; Negara, V. S. I.; Wongtepa, W.; Thamatkeng, P.; Zainuri, M.; Pratapa, S.

    2018-03-01

    XANES analysis has been performed with the aim of knowing the Fe oxidation state in a synthesized LiFePO4 and its base materials. XANES measurements were performed at SLRI on energy around Fe K-edge. An XRD analysis has also been performed with the aim of knowing the phase composition, lattice parameters and crystallite size of the LiFePO4 as well as the base materials. From the XRD analysis, it was found that the dominating phase in the iron sand sample was Fe3O4 and the only phase found after calcination was LiFePO4. The latter phase exhibited crystallite size of 100 nm and lattice parameters a = 10.169916 Å, b = 5.919674 Å, c = 4.627893 Å. Qualitative analysis of XANES data revealed that the oxidation number of Fe in the sample before calcination was greater than that after calcination and Fe in the natural iron sand, indicated by the E0 values of 7129.2 eV, 7120.6 eV and 7124.4 eV respectively.

  2. Solid-state one-way photoisomerisation of Z,E,Z-1,6-(4,4'-diphenyl)hexa-1,3,5-triene dicarboxylate examined using higher-order derivative spectra and powder XRD patterns.

    Science.gov (United States)

    Sonoda, Yoriko; Goto, Midori; Ichimura, Kunihiro

    2018-03-14

    Higher order derivative spectra were applied at first to one-way ZEZ-to-EEE photoisomerisation of dimethyl ester (ZEZ-DPH1) of the titled compound in a methylcyclohexane solution. Many common crossing points emerged in UV-induced derivative-spectral changes to reveal the direct ZEZ-to-EEE photoisomerisation without the transient formation of an intermediate to suggest the bicycle-pedal mechanism. The solid-state photoisomerisation was subsequently monitored by tracing changes in the fourth-order derivatives of absorption spectra of a thin crystalline layer of ZEZ-DPH1 prepared by the drop-casting method, because the distortion of absorption spectra due to light scattering is cancelled. It was suggested that the solid-state photochemical event consists of three steps: fast ZEZ-to-EEE photoisomerisation, a subsequent slow ZEZ-to-EEE photoisomerisation and very slow disappearance of the EEE-isomer. Studies on powder XRD were also carried out for a drop-cast solid layer of ZEZ-DPH1 to disclose the coexistence of a crystal form other than the original one, and the former exhibited faster ZEZ-to-EEE photoisomerisation when compared with the original crystal form. The results revealed by XRD analysis are in line with those obtained by higher-order derivative spectra, confirming the solid-state one-way photoisomerisation to take place through the bicycle-pedal process.

  3. Ultrasonic-assisted synthesis of nano lead(II) coordination polymer as precursors for preparation of lead(II) oxide nano-structures: Thermal, optical properties and XRD studies.

    Science.gov (United States)

    Ghavidelaghdam, Elham; Shahverdizadeh, Gholam Hossein; Motameni Tabatabai, Javad; Mirtamizdoust, Babak

    2018-04-01

    Nano structure of a lead (II) coordination polymer [Pb 2 (C 2 Cl 3 O 2 ) 2 (NO 3 ) 2 (C l2 H 8 N 2 ) 2 ] n (1), has been synthesized by a sonochemical method in different concentrations. The nano particles were characterized by scanning electron microscopy (SEM) X-ray powder diffraction (XRD), FT-IR spectroscopy and elemental analyses. The thermal stability of nano structure is closely investigated via thermal gravimetric (TGA), and compared with crystalline structure. The compounds are then heated to 600 °C to produce PbO nano particles. The resulting PbO is characterized through XRD and SEM analyses. Concentration of initial reagents effects on size and morphology of nano-structured compound 1 have been studied and show that low concentrations of initial reagents decreased particles size and leaded to uniform nano particles morphology. The photoluminescence properties of the prepared compound, as crystalline and as nanoparticles, have been investigated. The result showed a good correlation between the size and emission wavelength. Copyright © 2017. Published by Elsevier B.V.

  4. Cobalt ferrite nano-composite coated on glass by Doctor Blade method for photo-catalytic degradation of an azo textile dye Reactive Red 4: XRD, FESEM and DRS investigations.

    Science.gov (United States)

    Habibi, Mohammad Hossein; Parhizkar, Janan

    2015-11-05

    Cobalt ferrite nano-composite was prepared by hydrothermal route using cobalt nitrate, iron nitrate and ethylene glycol as chelating agent. The nano-composite was coated on glass by Doctor Blade method and annealed at 300 °C. The structural, optical, and photocatalytic properties have been studied by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and UV-visible spectroscopy (UV-Vis DRS). Powder XRD analysis confirmed formation of CoFe2O4 spinel phase. The estimated particle size from FESEM data was 50 nm. The calculated energy band gaps, obtained by Tauc relation from UV-Vis absorption spectra was 1.3 eV. Photocatalytic degradation of Reactive Red 4 as an azo textile was investigated in aqueous solution under irradiation showed 68.0% degradation of the dye within 100 min. The experimental enhanced activity compare to pure Fe2O3 can be ascribed to the formation of composite, which was mainly attributable to the transfer of electron and hole to the surface of composite and hinder the electron hole recombination. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Effect of annealing temperature on optical properties of binary zinc tin oxide nano-composite prepared by sol-gel route using simple precursors: structural and optical studies by DRS, FT-IR, XRD, FESEM investigations.

    Science.gov (United States)

    Habibi, Mohammad Hossein; Mardani, Maryam

    2015-02-25

    Binary zinc tin oxide nano-composite was synthesized by a facile sol-gel method using simple precursors from the solutions consisting of zinc acetate, tin(IV) chloride and ethanol. Effect of annealing temperature on optical and structural properties was investigated using X-ray diffraction (XRD), diffuse reflectance spectra (DRS), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FTIR). XRD results revealed the existence of the ZnO and SnO2 phases. FESEM results showed that binary zinc tin oxide nano-composites ranges from 56 to 60 nm in diameter at 400°C and 500°C annealing temperatures respectively. The optical band gap was increased from 2.72 eV to 3.11 eV with the increasing of the annealing temperature. FTIR results confirmed the presence of zinc oxide and tin oxide and the broad absorption peaks at 3426 and 1602 cm(-1) can be ascribed to the vibration of absorptive water, and the absorption peaks at 546, 1038 and 1410 cm(-1) are due to the vibration of Zn-O or Sn-O groups in binary zinc tin oxide. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Nuclear magnetic resonance experiments with dc SQUID amplifiers

    International Nuclear Information System (INIS)

    Heaney, M.B.

    1990-11-01

    The development and fabrication of dc SQUIDs (Superconducting QUantum Interference Devices) with Nb/Al 2 O 3 /Nb Josephson junctions is described. A theory of the dc SQUID as a radio-frequency amplifier is presented, with an optimization strategy that accounts for the loading and noise contributions of the postamplifier and maximizes the signal-to-noise ratio of the total system. The high sensitivity of the dc SQUID is extended to high field NMR. A dc SQUID is used as a tuned radio-frequency amplifier to detect pulsed nuclear magnetic resonance at 32 MHz from a metal film in a 3.5 Tesla static field. A total system noise temperature of 11 K has been achieved, at a bath temperature of 4.2 K. The minimum number of nuclear Bohr magnetons observable from a free precession signal after a single pulse is about 2 x 10 17 in a bandwidth of 25 kHz. In a separate experiment, a dc SQUID is used as a rf amplifier in a NQR experiment to observe a new resonance response mechanism. The net electric polarization of a NaClO 3 crystal due to the precessing electric quadrupole moments of the Cl nuclei is detected at 30 MHz. The sensitivity of NMR and NQR spectrometers using dc SQUID amplifiers is compared to the sensitivity of spectrometers using conventional rf amplifiers. A SQUID-based spectrometer has a voltage sensitivity which is comparable to the best achieved by a FET-based spectrometer, at these temperatures and operating frequencies

  7. Microwave tokamak experiment (MTX) first year of operation and future plans

    International Nuclear Information System (INIS)

    Jackson, M.C.

    1989-01-01

    The Microwave Tokamak Experiment (MTX) at Lawrence Livermore National Laboratory (LLNL) began plasma operations in November 1988, and our main goal is the study of electron-cyclotron heating (ECH) in plasma discharges. The MTX tokamak was relocated from the Massachusetts Institute of Technology (MIT), and we have re-created plasma parameters that are similar to those generated while the tokamak was at MIT. After stable ohmic operation was achieved, single-pulse FEL heating experiments began. During this phase, the FEL operated at low power levels on the way to its ultimate goal of 2 GW and 140 GHz with a 30-ns pulse length. We have developed a number of new diagnostics to measure these fast FEL pulses and the resulting plasma effects. In this paper, we present results that show the correlation of MTX data with MIT data, some of the operational modifications and procedures used, results to date from preliminary tokamak operations with the FEL, and our near-term operational plans. 7 refs., 8 figs., 1 tab

  8. Heteropolyhedral silver compounds containing the polydentate ligand N,N,O-E-[6-(hydroxyimino)ethyl]-1,3,7-trimethyllumazine. Preparation, spectral and XRD structural study and AIM calculations.

    Science.gov (United States)

    Jiménez-Pulido, Sonia B; Hueso-Ureña, Francisco; Fernández-Liencres, M Paz; Fernández-Gómez, Manuel; Moreno-Carretero, Miguel N

    2013-01-14

    The oxime derived from 6-acetyl-1,3,7-trimethyllumazine (1) ((E-6-(hydroxyimino)ethyl)-1,3,7-trimethylpteridine-2,4(1H,3H)-dione, DLMAceMox) has been prepared and its molecular and crystal structure determined from spectral and XRD data. The oxime ligand was reacted with silver nitrate, perchlorate, thiocyanate, trifluoromethylsulfonate and tetrafluoroborate to give complexes with formulas [Ag(2)(DLMAceMox)(2)(NO(3))(2)](n) (2), [Ag(2)(DLMAceMox)(2)(ClO(4))(2)](n) (3), [Ag(2)(DLMAceMox)(2)(SCN)(2)] (4), [Ag(2)(DLMAceMox)(2)(CF(3)SO(3))(2)(CH(3)CH(2)OH)]·CH(3)CH(2)OH (5) and [Ag(DLMAceMox)(2)]BF(4) (6). Single-crystal XRD studies show that the asymmetrical residual unit of complexes 2, 3 and 5 contains two quite different but connected silver centers (Ag1-Ag2, 2.9-3.2 Å). In addition to this, the Ag1 ion displays coordination with the N5 and O4 atoms from both lumazine moieties and a ligand (nitrato, perchlorato or ethanol) bridging to another disilver unit. The Ag2 ion is coordinated to the N61 oxime nitrogens, a monodentate and a (O,O)-bridging nitrato/perchlorato or two monodentate O-trifluoromethylsulfonato anions. The coordination polyhedra can be best described as a strongly distorted octahedron (around Ag1) and a square-based pyramid (around Ag2). The Ag-N and Ag-O bond lengths range between 2.22-2.41 and 2.40-2.67 Å, respectively. Although the structure of 4 cannot be resolved by XRD, it is likely to be similar to those described for 2, 3 and 5, containing Ag-Ag units with S-thiocyanato terminal ligands. Finally, the structure of the tetrafluoroborate compound 6 is mononuclear with a strongly distorted tetrahedral AgN(4) core (Ag-N, 2.27-2.43 Å). Always, the different Ag-N distances found clearly point to the more basic character of the oxime N61 nitrogen atom when compared with the pyrazine N5 one. A topological analysis of the electron density within the framework provided by the quantum theory of atoms in molecules (QTAIM) using DFT(M06L) levels of

  9. Electrochemical lithiation/delithiation of SnP₂O₇ observed by in situ XRD and ex situ⁷Li/³¹P NMR, and ¹¹⁹Sn Mössbauer spectroscopy.

    Science.gov (United States)

    Bezza, Ilham; Kaus, Maximilian; Riekehr, Lars; Pfaffmann, Lukas; Doyle, Stephen; Indris, Sylvio; Ehrenberg, Helmut; Solhy, Abderrahim; Saadoune, Ismael

    2016-04-21

    SnP2O7 was prepared by a sol-gel route. The structural changes of tin pyrophosphate during the electrochemical lithiation were followed by using in situ XRD measurements that reveal the existence of a crystalline phase at the beginning of the discharge process. Nevertheless, it becomes amorphous after the full discharge as a result of a conversion reaction leading to the formation of LixSny alloys. The electrochemical tests show a high capacity with high retention upon cycling. To better understand the reaction mechanism of SnP2O7 with Li, several techniques were applied, such as ex situ(119)Sn Mössbauer and ex situ(7)Li and (31)P NMR spectroscopies with which we can follow the changes in the local environment of each element during cycling.

  10. Synthesis and characterization of 64SiO2-26CaO-5P2O5-5CuO bioactive composition for the growth of hydroxyapatite layer by XRD, Raman and pH studies

    Science.gov (United States)

    Kaur, Pardeep; Singh, K. J.

    2016-05-01

    Bioactive sample with the nominal composition of 64SiO2-26CaO-5P2O5-5CuO has been prepared in the laboratory by using the sol-gel technique. The bioactivity of the prepared sample has been analyzed by using the Tris Simulated Body Fluid which has also been prepared in the laboratory. XRD and Raman techniques have been employedto probe the formation of hydroxyapatite layer. pH studies has also been undertaken to check the acidic/non-acidic behavior of sample. Growth of hydroxyapatite layer has been observed after one day on the surface of the sample. Moreover, sample has been observed to be non-acidic in nature.

  11. A combined experimental and computational study of 3-bromo-5-(2,5-difluorophenyl) pyridine and 3,5-bis(naphthalen-1-yl)pyridine: Insight into the synthesis, spectroscopic, single crystal XRD, electronic, nonlinear optical and biological properties

    Science.gov (United States)

    Ghiasuddin; Akram, Muhammad; Adeel, Muhammad; Khalid, Muhammad; Tahir, Muhammad Nawaz; Khan, Muhammad Usman; Asghar, Muhammad Adnan; Ullah, Malik Aman; Iqbal, Muhammad

    2018-05-01

    Carbon-carbon coupling play a vital role in the synthetic field of organic chemistry. Two novel pyridine derivatives: 3-bromo-5-(2,5-difluorophenyl)pyridine (1) and 3,5-bis(naphthalen-1-yl)pyridine (2) were synthesized via carbon-carbon coupling, characterized by XRD, spectroscopic techniques and also investigated by using density functional theory (DFT). XRD data and optimized DFT studies are found to be in good correspondence with each other. The UV-Vis analysis of compounds under study i.e. (1) and (2) was obtained by using "TD-DFT/B3LYP/6-311 + G(d,p)" level of theory to explain the vertical transitions. Calculated FT-IR and UV-Vis results are found to be in good agreement with experimental FT-IR and UV-Vis findings. Natural bond orbital (NBO) study was performed using B3LYP/6-311 + G(d,p) level to find the most stable molecular structure of the compounds. Frontier molecular orbital (FMO) analysis were performed at B3LYP/6-311 + G(d,p) level of theory, which indicates that the molecules might be bioactive. Moreover, the bioactivity of compounds (1) and (2) have been confirmed by the experimental activity in terms of zones of inhibition against bacteria and fungus. Chemical reactivity of compounds (1) and (2) was indicated by mapping molecular electrostatic potential (MEP) over the entire stabilized geometries of the compounds under study. The nonlinear optical properties were computed with B3LYP/6-311 + G(d,p) level of theory which are found greater than the value of urea due to conjugation effect. Two state model has been further employed to explain the nonlinear optical properties of compounds under investigation.

  12. Studies the alterations of biochemical and mineral contents in bone tissue of mus musculus due to aluminum toxicity and the protective action of desferrioxamine and deferiprone by FTIR, ICP-OES, SEM and XRD techniques.

    Science.gov (United States)

    Sivakumar, S; Khatiwada, Chandra Prasad; Sivasubramanian, J

    2014-05-21

    The present study has attempt to analyze the changes in the biochemical and mineral contents of aluminum intoxicated bone and determine the protective action of desferrioxamine (DFO) and deferiprone (DFP) by using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), inductively coupled plasma optical emission spectroscopy (ICP-OES), and scanning electron microscopy (SEM) techniques for four groups of animals such as control (Group I), aluminum intoxicated (Group II), Al+DFP (Group III) and Al+DFO+DFP (Group IV) treated groups respectively. The FTIR spectra of the aluminum intoxicated bone showed significant alteration in the biochemical constituents. The bands ratio at I1400/I877 significantly decreased from control to aluminum, but enhanced it by Al+DFP to Al+DFO+DFP treated bone tissue for treatments of 16 weeks. This result suggests that DFO and DFP are the carbonate inhibitor, recovered from chronic growth of bone diseases and pathologies. The alteration of proteins profile indicated by Amide I and Amide II, where peak area values decreased from control to aluminum respectively, but enhanced by treated with DFP (p.o.) and DFO+DFP (i.p.) respectively. The XRD analysis showed a decrease in crystallinity due to aluminum toxicity. Further, the Ca, Mg, and P contents of the aluminum exposed bone were less than those of the control group, and enhanced by treatments with DFO and DFP. The concentrations of trace elements were found by ICP-OES. Therefore, present study suggests that due to aluminum toxicity severe loss of bone minerals, decrease in the biochemical constituents and changes in the surface morphology. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Conservation of Moroccan manuscript papers aged 150, 200 and 800 years. Analysis by infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD), and scanning electron microscopy energy dispersive spectrometry (SEM-EDS).

    Science.gov (United States)

    Hajji, Latifa; Boukir, Abdellatif; Assouik, Jamal; Lakhiari, Hamid; Kerbal, Abdelali; Doumenq, Pierre; Mille, Gilbert; De Carvalho, Maria Luisa

    2015-02-05

    The preservation of manuscripts and archive materials is a serious problem for librarians and restorers. Paper manuscript is subjected to numerous degradation factors affecting their conservation state. This research represents an attempt to evaluate the conservation restoration process applied in Moroccan libraries, especially the alkaline treatment for strengthening weakened paper. In this study, we focused on six samples of degraded and restored paper taken from three different Moroccan manuscripts aged 150, 200 and 800 years. In addition, the Japanese paper used in restoration has been characterized. A modern paper was also analyzed as reference. A three-step analytical methodology based on infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD) and scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS) analysis was developed before and after restoration in order to determine the effect of the consolidation treatment on the paper structure. The results obtained by XRD and ATR-FTIR disclosed the presence of barium sulfate (BaSO4) in all restored paper manuscripts. The presence of calcium carbonate (CaCO3) in all considered samples was confirmed by FTIR spectroscopy. The application of de-acidification treatment causes significant changes connected with the increase of intensity mostly in the region 1426 cm(-1), assigned to the asymmetric and symmetric CO stretching mode of calcite, indicating the effectiveness of de-acidification procedure proved by the rise of the alkaline reserve content allowing the long term preservation of paper. Observations performed by SEM magnify the typical paper morphology and the structure of fibbers, highlighting the effect of the restoration process, manifested by the reduction of impurities. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Synthetic, XRD, non-covalent interactions and solvent dependent nonlinear optical studies of Sulfadiazine-Ortho-Vanillin Schiff base: (E)-4-((2-hydroxy-3-methoxy- benzylidene) amino)-N-(pyrimidin-2-yl)benzene-sulfonamide

    Science.gov (United States)

    Shahid, Muhammad; Salim, Muhammad; Khalid, Muhammad; Tahir, Muhammad Nawaz; Khan, Muhammad Usman; Braga, Ataualpa Albert Carmo

    2018-06-01

    In this study, Sulfadiazine-Ortho-Vanillin Schiff base namely (E)-4-((2-hydroxy-3-methoxybenzylidene)amino)sbnd N-(pyrimidin-2-yl)benzene-sulfonamide (BS) was synthesized. Chemical characterization and computational studies using different techniques like XRD, FT-IR, UV-Vis, NBO, FMO, and MEP have been employed. Density functional theory (DFT) calculations have been performed at M06-2X/6-311 + G(d,p) level of theory to obtain optimized geometry and vibrational wave numbers for (E)-4-((2-hydroxy-3-methoxybenzylidene)amino)sbnd N-(pyrimidin-2-yl)benzene-sulfonamide (BS). The DFT optimized geometry supports the experimental XRD parameters. Frontier molecular orbital (FMO) energies and molecular electrostatic potential (MEP) surfaces have been executed at M06-2X/6-311 + G(d,p) level of theory. NBO analysis has been carried out at M06-2X/6-311 + G(d,p) level which not only discovered the hyper conjugative interactions and stability in title molecule but also reconfirmed the existence of Nsbnd H⋯N hydrogen bonds between the dimer. The findings of small EHOMO-ELUMO gap shows less hardness and larger softness values which suggested the bioactiveness of the title molecule. Finally, the effect of solvent on nonlinear optical (NLO) properties has been executed using M06-2X level of theory and 6-311 + G (d,p) basis set. The solvent polarity enhanced the NLO response from 3.62 × 10-30 esu to 4.66 × 10-30 esu indicating the considerable NLO character hence in general may have potential applications in the development of non-linear optical materials.

  15. Synthesis, structural, spectroscopic, anti-cancer and molecular docking studies on novel 2-[(Anthracene-9-ylmethylene)amino]-2-methylpropane-1,3-diol using XRD, FTIR, NMR, UV-Vis spectra and DFT

    Science.gov (United States)

    Pavitha, P.; Prashanth, J.; Ramu, G.; Ramesh, G.; Mamatha, K.; Venkatram Reddy, Byru

    2017-11-01

    The novel titled compound 2-[(Anthracene-9-ylmethylene)amino]-2-methylpropane-1,3-diol (AMD) has been synthesized by slow evaporation technique from mixed solvent system of methanol with anthracene-9-carbaldehyde and 2-amino-2-methylpropane-1,3-diol. The synthesized molecule AMD was characterized experimentally by single crystal XRD, FTIR, NMR and UV-Vis spectra and density functional theory (DFT) computations. The structure of the crystal has been determined as orthorhombic system with space group P 21 21 21 and the cell parameters are obtained using XRD data. The optimized ground state geometry of the molecule is determined by evaluating torsional potentials as a function of angle of free rotation around Csbnd C bonds of functional groups by DFT method employing B3LYP functional with 6-311++G(d,p) basis set. All the fundamental vibrations of the molecule are assigned unambiguously using potential energy distribution (PED) obtained in the DFT computations. The rms error between the observed and scaled frequencies is 6.20 cm-1. The values of dipole moment, polarizability and hyperpolarizability are evaluated to study the NLO behavior of the molecule. The HOMO-LUMO energies and thermodynamic parameters are also determined. The molecular electrostatic surface potential (MESP) is mapped to obtain the charge density distribution. The 1H and 13C NMR chemical shifts of the molecule are calculated by the gauge independent atomic orbital (GIAO) method and compared with experimental results. UV-visible spectrum of the compound is also recorded in the region 200-800 nm to know the type of electronic transitions involved. The anti-cancer activity of AMD is determined against human breast cancer cell line MCF-7 and human prostate cancer cell line PC-3 and correlated the results with study of molecular docking against pharmacological protein IDO-1 receptor.

  16. Pixel Experiments

    DEFF Research Database (Denmark)

    Petersen, Kjell Yngve; Søndergaard, Karin; Augustesen, Christina

    2015-01-01

    Pixel Experiments The term pixel is traditionally defined as any of the minute elements that together constitute a larger context or image. A pixel has its own form and is the smallest unit seen within a larger structure. In working with the potentials of LED technology in architectural lighting...... for using LED lighting in lighting design practice. The speculative experiments that have been set-up have aimed to clarify the variables that can be used as parameters in the design of lighting applications; including, for example, the structuring and software control of light. The experiments also...... elucidate and exemplify already well-known problems in relation to the experience of vertical and horizontal lighting. Pixel Experiments exist as a synergy between speculative test setups and lighting design in practice. This book is one of four books that is published in connection with the research...

  17. TRIO experiment

    International Nuclear Information System (INIS)

    Clemmer, R.G.; Finn, P.A.; Malecha, R.F.

    1984-09-01

    The TRIO experiment is a test of in-situ tritium recovery and heat transfer performance of a miniaturized solid breeder blanket assembly. The assembly (capsule) was monitored for temperature and neutron flux profiles during irradiation and a sweep gas flowed through the capsule to an anaytical train wherein the amounts of tritium in its various chemical forms were determined. The capsule was designed to operate at different temperatures and sweep gas conditions. At the end of the experiment the amount of tritium retained in the solid was at a concentration of less than 0.1 wppM. More than 99.9% of tritium generated during the experiment was successfully recovered. The results of the experiment showed that the tritium inventories at the beginning and at the end of the experiment follow a relationship which appears to be characteristic of intragranular diffusion

  18. Classic experiments

    CERN Multimedia

    CERN. Geneva; Franklin, M

    2001-01-01

    These will be a set of lectures on classic particle physics experiments, with emphasis on how the emasurements are made. I will discuss experiments made to measure the electric charge distribution of particles, to measure the symmetries of the weak decays, to measure the magnetic moment of the muon. As well as experiments performed which discovered new particles or resonances, like the tAU2and the J/Psi. The coverage will be general and should be understandable to someone knowing little particle physics.

  19. Simulated experiments

    International Nuclear Information System (INIS)

    Bjerknes, R.

    1977-01-01

    A cybernetic model has been developed to elucidate some of the main principles of the growth regulation system in the epidermis of the hairless mouse. A number of actual and theoretical biological experiments have been simulated on the model. These included simulating the cell kinetics as measured by pulse labelling with tritiated thymidine and by continuous labelling with tritiated thymidine. Other simulated experiments included steady state, wear and tear, painting with a carcinogen, heredity and heredity and tumour. Numerous diagrams illustrate the results of these simulated experiments. (JIW)

  20. Researching experiences

    DEFF Research Database (Denmark)

    Gjedde, Lisa; Ingemann, Bruno

    In the beginning was - not the word - but the experience. This phenomenological approach provides the basis for this book, which focuses on how a person-in-situation experiences and constructs meaning from a variety of cultural visual events. This book presents video-based processual methods......, dialogue, moods, values and narratives have been investigated qualitatively with more than sixty informants in a range of projects. The processual methodological insights are put into a theoretical perspective and also presented as pragmatic dilemmas. Researching Experiences is relevant not only...

  1. Antimatter Experiments

    CERN Multimedia

    2004-01-01

    Antimatter should behave in identical fashion to matter if a form of spacetime symmetry called CPT invariance holds. Two experiments at CERN near Geneva are testing this hypothesis using antihydrogen atoms

  2. Pixel Experiments

    DEFF Research Database (Denmark)

    Petersen, Kjell Yngve; Søndergaard, Karin; Augustesen, Christina

    2015-01-01

    Pixel Experiments The term pixel is traditionally defined as any of the minute elements that together constitute a larger context or image. A pixel has its own form and is the smallest unit seen within a larger structure. In working with the potentials of LED technology in architectural lighting...... lighting design in practice, one quickly experiences and realises that there are untapped potentials in the attributes of LED technology. In this research, speculative studies have been made working with the attributes of LEDs in architectural contexts, with the ambition to ascertain new strategies...... for using LED lighting in lighting design practice. The speculative experiments that have been set-up have aimed to clarify the variables that can be used as parameters in the design of lighting applications; including, for example, the structuring and software control of light. The experiments also...

  3. Experiment Databases

    Science.gov (United States)

    Vanschoren, Joaquin; Blockeel, Hendrik

    Next to running machine learning algorithms based on inductive queries, much can be learned by immediately querying the combined results of many prior studies. Indeed, all around the globe, thousands of machine learning experiments are being executed on a daily basis, generating a constant stream of empirical information on machine learning techniques. While the information contained in these experiments might have many uses beyond their original intent, results are typically described very concisely in papers and discarded afterwards. If we properly store and organize these results in central databases, they can be immediately reused for further analysis, thus boosting future research. In this chapter, we propose the use of experiment databases: databases designed to collect all the necessary details of these experiments, and to intelligently organize them in online repositories to enable fast and thorough analysis of a myriad of collected results. They constitute an additional, queriable source of empirical meta-data based on principled descriptions of algorithm executions, without reimplementing the algorithms in an inductive database. As such, they engender a very dynamic, collaborative approach to experimentation, in which experiments can be freely shared, linked together, and immediately reused by researchers all over the world. They can be set up for personal use, to share results within a lab or to create open, community-wide repositories. Here, we provide a high-level overview of their design, and use an existing experiment database to answer various interesting research questions about machine learning algorithms and to verify a number of recent studies.

  4. The Experiment

    Science.gov (United States)

    Mariana Nicoara, Floare

    2016-04-01

    My name is Nicoara Floarea and I am teacher at Secondary School Calatele and I teach students from preparatory class and the second grade . They are six-eight years old. In my activity, for introducing scientific concepts to my students, I use various and active methods or traditional methods including experiments. The experiment stimulates students' curiosity, their creativity, the understanding and knowledge taught accessibility. I propose you two such experiments: The life cycle of the plants (long-term experiment, with rigorous observation time):We use beans, wheat or other; They are grown in pots and on the cotton soaked with water,keeping under students' observation protecting them ( just soak them regularly) and we waiting the plants rise. For discussions and comments of plant embryo development we use the plants which rose on the cotton soaked with water plants at the end of the first week. Last school year we had in the pot climbing beans which in May made pods. They were not too great but our experiment was a success. The students could deduce that there will develop those big beans which after drying will be planted again. The influence of light on plants (average duration experiment with the necessary observation time): We use two pots in which plants are of the same type (two geraniums), one of them is situated so as to get direct sunlight and other plant we put in a closed box. Although we wet both plants after a week we see that the plant that benefited from sunlight has turned strain in direct sunlight, developing normally in return the plant out of the box I have yellowed leaves, photosynthesis does not She has occurred . Students will understand the vital role of the Sun in plants' life, both in the classroom and in nature. The experiment is a method of teaching students extremely pleasant, with a remarkable percentage of acquiring more knowledge.

  5. VERTISOLES Y CERÁMICA INDÍGENA: UN ESTUDIO DE PROCEDENCIA BASADO EN DRX, SITIO GUAYACAS (PAYSANDÚ, URUGUAY / Vertisols and indigenous ceramics: a provenience study based on XRD from Guayacas site (Paysandú, Uruguay

    Directory of Open Access Journals (Sweden)

    Irina Capdepont

    2010-12-01

    Full Text Available El registro arqueológico más abundante de la región litoral del Uruguay para el Holoceno medio y tardío se encuentra conformado por material cerámico. La información existente sobre el mismo  proviene comúnmente de estudios macroscópicos en los que se aborda la reconstrucción de formas, tecnología y estilos decorativos. En este trabajo se exponen los resultados obtenidos mediante la aplicación de DRX sobre cerámicas de conjuntos arqueológicos del sitio Guayacas (Departamento de Paysandú. En este estudio se busca complementar el conocimiento de la primera etapa del proceso de manufactura: la selección de materia prima. Para ello, también se realizan estudios de DRX sobre sedimentos y afloramientos de la zona, así como sobre sedimentos de la excavación arqueológica. Entre los resultados obtenidos se destaca la homogeneidad entre las pastas y la ausencia de minerales de tipo illita; los suelos antropogénicos presentan esmectita, cuarzo, illita e interestratificados y los suelos naturales y afloramientos están dominados por arcillas esmectiticas más cuarzo, proponiéndose a uno de ellos como fuente potencial de abastecimiento de materia prima local. Los datos obtenidos aportan nueva información al conocimiento del área de ocupación sobre el río Daymán durante el Holoceno tardío. Palabras clave: alfarería; mineralogía; vertisoles; DRXAbstract The most abundant archaeological record in the middle and late Holocene in the litoral region of Uruguay is formed by ceramic materials. Previous information usually comes from macroscopic studies, oriented to the reconstruction of decorative styles, forms, and technology. This paper presents XRD analyses of archaeological ceramics from Guayacas site (Department of Paysandú . This study seeks to complement the knowledge about the first stage of the process of manufacture: the selection of raw materials. In order to do this, an XRD analysis is also carried out on sediments and

  6. LIMITS ON THE EVENT RATES OF FAST RADIO TRANSIENTS FROM THE V-FASTR EXPERIMENT

    International Nuclear Information System (INIS)

    Wayth, Randall B.; Tingay, Steven J.; Deller, Adam T.; Brisken, Walter F.; Thompson, David R.; Wagstaff, Kiri L.; Majid, Walid A.

    2012-01-01

    We present the first results from the V-FASTR experiment, a commensal search for fast transient radio bursts using the Very Long Baseline Array (VLBA). V-FASTR is unique in that the widely spaced VLBA antennas provide a discriminant against non-astronomical signals and a mechanism for the localization and identification of events that is not possible with single dishes or short baseline interferometers. Thus, far V-FASTR has accumulated over 1300 hr of observation time with the VLBA, between 90 cm and 3 mm wavelength (327 MHz-86 GHz), providing the first limits on fast transient event rates at high radio frequencies (>1.4 GHz). V-FASTR has blindly detected bright individual pulses from seven known pulsars but has not detected any single-pulse events that would indicate high-redshift impulsive bursts of radio emission. At 1.4 GHz, V-FASTR puts limits on fast transient event rates comparable with the PALFA survey at the Arecibo telescope, but generally at lower sensitivities, and comparable to the 'fly's eye' survey at the Allen Telescope Array, but with less sky coverage. We also illustrate the likely performance of the Phase 1 SKA dish array for an incoherent fast transient search fashioned on V-FASTR.

  7. Chlorides behavior in raw fly ash washing experiments

    International Nuclear Information System (INIS)

    Zhu Fenfen; Takaoka, Masaki; Oshita, Kazuyuki; Kitajima, Yoshinori; Inada, Yasuhiro; Morisawa, Shinsuke; Tsuno, Hiroshi

    2010-01-01

    Chloride in fly ash from municipal solid waste incinerators (MSWIs) is one of the obstructive substances in recycling fly ash as building materials. As a result, we have to understand the behavior of chlorides in recycling process, such as washing. In this study, we used X-ray absorption near edge structure (XANES) and X-ray diffraction (XRD) to study the chloride behavior in washed residue of raw fly ash (RFA). We found that a combination of XRD and XANES, which is to use XRD to identify the situation of some compounds first and then process XANES data, was an effective way to explain the chlorides behavior in washing process. Approximately 15% of the chlorine in RFA was in the form of NaCl, 10% was in the form of KCl, 51% was CaCl 2 , and the remainder was in the form of Friedel's salt. In washing experiments not only the mole percentage but also the amount of soluble chlorides including NaCl, KCl and CaCl 2 decreases quickly with the increase of liquid to solid (L/S) ratio or washing frequency. However, those of insoluble chlorides decrease slower. Moreover, Friedel's salt and its related compound (11CaO.7Al 2 O 3 .CaCl 2 ) were reliable standards for the insoluble chlorides in RFA, which are strongly related to CaCl 2 . Washing of RFA promoted the release of insoluble chlorides, most of which were in the form of CaCl 2 .

  8. In Situ XRD Studies of ZnO/GaN Mixtures at High Pressure and High Temperature: Synthesis of Zn-Rich (Ga1-xZnx)(N1-xOx) Photocatalysts

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez, J.A.; Chen, H.; Wang, L.; Bai, J.; Hanson, J.C.; Warren, J.B.; Muckerman, J.T.; Fujita, E.

    2010-02-04

    The high-pressure, high-temperature conditions for the synthesis of Zn-rich (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions from mixtures of ZnO/GaN were explored using synchrotron-based in situ time-resolved X-ray diffraction (XRD). Following a new synthetic path, (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions with a Zn content up to 75% were prepared for the first time. The structures of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions were characterized by XRD and X-ray absorption fine structure (XAFS) analyses and were in excellent agreement with the predictions of density functional calculations. These materials adopt a wurtzite crystal structure with metal-N or metal-O bond distances in the range of 1.95-1.98 {angstrom}. Although the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions seem to be stable over the full range of compositions, no ideal solid solution formation was observed. In all cases, the lattice parameters were larger than those of ideal solid solutions. The variation of the lattice parameter c showed an upward double bowing curve, as was predicted by theoretical calculations. Also, no ideal behavior was observed in the electronic properties of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions. X-ray absorption spectra at the Zn and Ga K-edges of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) systems showed significant electronic perturbations with respect to ZnO and GaN. The synthesized (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solution with a Zn content of 50% displayed the ability to absorb visible light well above 500 nm. This material has a great potential for splitting water under visible light irradiation. The availability of (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions with a high Zn content opens the door to fully explore the application of these materials in photocatalysis.

  9. In Situ XRD Studies of ZnO/GaN Mixtures at High Pressure and High Temperature: Synthesis of Zn-Rich (Ga1-xZnx)(N1-xOx) Photocatalysts

    Energy Technology Data Exchange (ETDEWEB)

    Chen, H.; Wang, L; Bai, J; Hanson, J; Warren, J; Muckerman, J; Fujita, E; Rodriguez, J

    2010-01-01

    The high-pressure, high-temperature conditions for the synthesis of Zn-rich (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions from mixtures of ZnO/GaN were explored using synchrotron-based in situ time-resolved X-ray diffraction (XRD). Following a new synthetic path, (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions with a Zn content up to {approx}75% were prepared for the first time. The structures of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions were characterized by XRD and X-ray absorption fine structure (XAFS) analyses and were in excellent agreement with the predictions of density functional calculations. These materials adopt a wurtzite crystal structure with metal-N or metal-O bond distances in the range of 1.95-1.98 {angstrom}. Although the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions seem to be stable over the full range of compositions, no ideal solid solution formation was observed. In all cases, the lattice parameters were larger than those of ideal solid solutions. The variation of the lattice parameter c showed an upward double bowing curve, as was predicted by theoretical calculations. Also, no ideal behavior was observed in the electronic properties of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions. X-ray absorption spectra at the Zn and Ga K-edges of the (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) systems showed significant electronic perturbations with respect to ZnO and GaN. The synthesized (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solution with a Zn content of 50% displayed the ability to absorb visible light well above 500 nm. This material has a great potential for splitting water under visible light irradiation. The availability of (Ga{sub 1-x}Zn{sub x})(N{sub 1-x}O{sub x}) solid solutions with a high Zn content opens the door to fully explore the application of these materials in photocatalysis.

  10. Collaborative experience

    DEFF Research Database (Denmark)

    Mortensen, Thomas Bøtker

    -Doerr, 1996) and has been shown to have a positive effect to the outcome of collaborative R&D (Sampson, 2005). Anand & Khanna (2000), furthermore, hypothesized that research joint ventures are more ambiguous than marketing joint ventures and even more the licensing and showed that the effect of collaborative......Literature review: Collaborative experience has been shown to have a positive effect on the collaborative outcome in general (Anand & Khanna, 2000; Kale, Dyer & Singh, 2002). Furthermore, it has been linked to the ability to exploit the network of the firm for learning (Powell, Koput and Smith...... experience was largest the higher the hypothesized ambiguity. Theoretically contribution: This research project aims at contributing to existing literature by arguing, that collaborative experience is a moderating variable which moderates the effects on collaborative outcome from the level of complexity...

  11. Channeling experiment

    International Nuclear Information System (INIS)

    Abelin, H.; Birgersson, L.; Widen, H.; Aagren, T.; Moreno, L.; Neretnieks, I.

    1990-07-01

    Channeling of water flow and tracer transport in real fractures in a granite body at Stripa have been investigated experimentally. The experimental site was located 360 m below the ground level. Two kinds of experiments were performed. In the single hole experiments, 20 cm diameter holes were drilled about 2.5 m into the rock in the plane of the fracture. Specially designed packers were used to inject water into the fracture in 5 cm intervals all along the fracture trace in the hole. The variation of the injection flowrates along the fracture were used to determine the transmissivity variations in the fracture plane. Detailed photographs were taken from inside the hole and the visual fracture aperture was compared with the injection flowrates in the same locations. Geostatistical methods were used to evaluate the results. Five holes were measured in great detail. In addition 7 holes were drilled and scanned by simpler packer systems. A double hole experiment was performed where two parallel holes were drilled in the same fracture plane at nearly 2 m distance. Pressure pulse tests were made between the holes in both directions. Tracers were injected in 5 locations in one hole and monitored for in many locations in the other hole. The single hole experiment and the double hole experiment show that most of the fracture planes are tight but that there are open sections which form connected channels over distances of at least 2 meters. It was also found in the double hole experiment that the investigated fracture was intersected by at least one fracture between the two holes which diverted a large amount of the injected tracers to several distant locations at the tunnel wall. (authours)

  12. Poetic Experience

    Directory of Open Access Journals (Sweden)

    Shahab Yar Khan

    2014-01-01

    Full Text Available Nature of poetic experience is hereby redefined. The present article initially deals with the perennial nature of true poetic experience and its essential relevance to the world. It attempts to elaborate the process through which a poet is uplifted in a creative moment beyond terrestrial boundaries and is aligned with the ‘state of Perfection'. The role of successive generations of audiences in rediscovering the meaning of a poetic image is defined as life principle of all great poetry. Shakespeare is discussed as the ultimate example of this principle since his popularity remains an irreversible phenomenon

  13. Evaluation of the concrete shield compositions from the 2010 criticality accident alarm system benchmark experiments at the CEA Valduc SILENE facility

    International Nuclear Information System (INIS)

    Miller, Thomas Martin; Celik, Cihangir; Dunn, Michael E; Wagner, John C; McMahan, Kimberly L; Authier, Nicolas; Jacquet, Xavier; Rousseau, Guillaume; Wolff, Herve; Savanier, Laurence; Baclet, Nathalie; Lee, Yi-kang; Trama, Jean-Christophe; Masse, Veronique; Gagnier, Emmanuel; Naury, Sylvie; Blanc-Tranchant, Patrick; Hunter, Richard; Kim, Soon; Dulik, George Michael; Reynolds, Kevin H.

    2015-01-01

    In October 2010, a series of benchmark experiments were conducted at the French Commissariat a l'Energie Atomique et aux Energies Alternatives (CEA) Valduc SILENE facility. These experiments were a joint effort between the United States Department of Energy Nuclear Criticality Safety Program and the CEA. The purpose of these experiments was to create three benchmarks for the verification and validation of radiation transport codes and evaluated nuclear data used in the analysis of criticality accident alarm systems. This series of experiments consisted of three single-pulsed experiments with the SILENE reactor. For the first experiment, the reactor was bare (unshielded), whereas in the second and third experiments, it was shielded by lead and polyethylene, respectively. The polyethylene shield of the third experiment had a cadmium liner on its internal and external surfaces, which vertically was located near the fuel region of SILENE. During each experiment, several neutron activation foils and thermoluminescent dosimeters (TLDs) were placed around the reactor. Nearly half of the foils and TLDs had additional high-density magnetite concrete, high-density barite concrete, standard concrete, and/or BoroBond shields. CEA Saclay provided all the concrete, and the US Y-12 National Security Complex provided the BoroBond. Measurement data from the experiments were published at the 2011 International Conference on Nuclear Criticality (ICNC 2011) and the 2013 Nuclear Criticality Safety Division (NCSD 2013) topical meeting. Preliminary computational results for the first experiment were presented in the ICNC 2011 paper, which showed poor agreement between the computational results and the measured values of the foils shielded by concrete. Recently the hydrogen content, boron content, and density of these concrete shields were further investigated within the constraints of the previously available data. New computational results for the first experiment are now available

  14. EXPERIENCE WITH

    African Journals Online (AJOL)

    SURGERY DEPT

    Abstract. Background:Island flap techniques currently used in urethroplasty utilize the prepuce and the dorsal penile skin. Our experience with a one-stage island flap urethroplasty for urethral strictures utilizing the ventral penile skin is described. Patients and Method: This is a longitudinal study of seventy six consecutive ...

  15. Copper(II) complex with 6-methylpyridine-2-carboxyclic acid: Experimental and computational study on the XRD, FT-IR and UV-Vis spectra, refractive index, band gap and NLO parameters.

    Science.gov (United States)

    Altürk, Sümeyye; Avcı, Davut; Başoğlu, Adil; Tamer, Ömer; Atalay, Yusuf; Dege, Necmi

    2018-02-05

    Crystal structure of the synthesized copper(II) complex with 6-methylpyridine-2-carboxylic acid, [Cu(6-Mepic) 2 ·H 2 O]·H 2 O, was determined by XRD, FT-IR and UV-Vis spectroscopic techniques. Furthermore, the geometry optimization, harmonic vibration frequencies for the Cu(II) complex were carried out by using Density Functional Theory calculations with HSEh1PBE/6-311G(d,p)/LanL2DZ level. Electronic absorption wavelengths were obtained by using TD-DFT/HSEh1PBE/6-311G(d,p)/LanL2DZ level with CPCM model and major contributions were determined via Swizard/Chemissian program. Additionally, the refractive index, linear optical (LO) and non-nonlinear optical (NLO) parameters of the Cu(II) complex were calculated at HSEh1PBE/6-311G(d,p) level. The experimental and computed small energy gap shows the charge transfer in the Cu(II) complex. Finally, the hyperconjugative interactions and intramolecular charge transfer (ICT) were studied by performing of natural bond orbital (NBO) analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. XRD and FTIR studies the effect of heat treatment and doping the transition metal oxide on LiNbO3 and LiNb3O8 nano-crystallite phases in lithium borate glass system.

    Science.gov (United States)

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

    2013-09-01

    Glasses of various compositions in the system 90 Li2B4O7-10 Nb2O5 mixed with T.M ions (where T.M is the transition metal) were prepared by quenching technique. Heat-treatment of the parent glasses was performed at 540, 570 and 620 °C, for 5 and 16 h. The glass structure evolution during the controlled crystallization was examined by XRD and FT-IR spectroscopy analysis. The crystalline phases present in the glass ceramics were identified via X-ray diffraction as a function of heat treatment. The FT-IR data propose for these glasses and heat-treated glass network structures mainly built by: di-, tri-, tetra-, penta-and ortho-borate groups. It was found that the quantitative evolution of these various borate species in the glass structures is influenced by the transition metal. A detailed discussion relating to the N4 evolution with the T.M content was made. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Capacity Fading Mechanism of the Commercial 18650 LiFePO4-Based Lithium-Ion Batteries: An in Situ Time-Resolved High-Energy Synchrotron XRD Study.

    Science.gov (United States)

    Liu, Qi; Liu, Yadong; Yang, Fan; He, Hao; Xiao, Xianghui; Ren, Yang; Lu, Wenquan; Stach, Eric; Xie, Jian

    2018-02-07

    In situ high-energy synchrotron XRD studies were carried out on commercial 18650 LiFePO 4 cells at different cycles to track and investigate the dynamic, chemical, and structural changes in the course of long-term cycling to elucidate the capacity fading mechanism. The results indicate that the crystalline structural deterioration of the LiFePO 4 cathode and the graphite anode is unlikely to happen before capacity fades below 80% of the initial capacity. Rather, the loss of the active lithium source is the primary cause for the capacity fade, which leads to the appearance of inactive FePO 4 that is proportional to the absence of the lithium source. Our in situ HESXRD studies further show that the lithium-ion insertion and deinsertion behavior of LiFePO 4 continuously changed with cycling. For a fresh cell, the LiFePO 4 experienced a dual-phase solid-solution behavior, whereas with increasing cycle numbers, the dynamic change, which is characteristic of the continuous decay of solid solution behavior, is obvious. The unpredicted dynamic change may result from the morphology evolution of LiFePO 4 particles and the loss of the lithium source, which may be the cause of the decreased rate capability of LiFePO 4 cells after long-term cycling.

  18. Authoring experience

    DEFF Research Database (Denmark)

    Knox, Jeanette Bresson Ladegaard; Svendsen, Mette Nordahl

    2015-01-01

    This article examines the storytelling aspect inphilosophizing with rehabilitating cancer patients in small Socratic dialogue groups (SDG). Recounting an experienceto illustrate a philosophical question chosen by the participantsis the traditional point of departure for the dialogicalexchange....... However, narrating is much more than abeginning point or the skeletal framework of events and itdeserves more scholarly attention than hitherto given. Storytelling pervades the whole Socratic process and impactsthe conceptual analysis in a SDG. In this article weshow how the narrative aspect became a rich...... an experiencethrough a collaborative effort, most participants hadtheir initial experience existentially refined and the chosenconcept of which the experience served as an illustrationtransformed into a moral compass to be used in self-orientationpost cancer....

  19. Dirac experiment

    International Nuclear Information System (INIS)

    Gomez, F.; Adeva, B.; Afanasev, L.; Benayoun, M.; Brekhovskikh, V.; Caragheorgheopol, G.; Cechak, T.; Chiba, M.; Constantinescu, S.; Doudarev, A.; Dreossi, D.; Drijard, D.; Ferro-Luzzi, M.; Gallas, M.V.; Gerndt, J.; Giacomich, R.; Gianotti, P.; Goldin, D.; Gorin, A.; Gortchakov, O.; Guaraldo, C.; Hansroul, M.; Hosek, R.; Iliescu, M.; Jabitski, M.; Kalinina, N.; Karpoukhine, V.; Kluson, J.; Kobayashi, M.; Kokkas, P.; Komarov, V.; Koulikov, A.; Kouptsov, A.; Krouglov, V.; Krouglova, L.; Kuroda, K.-I.; Lanaro, A.; Lapshine, V.; Lednicky, R.; Leruste, P.; Levisandri, P.; Lopez Aguera, A.; Lucherini, V.; Maki, T.; Manuilov, I.; Montanet, L.; Narjoux, J.-L.; Nemenov, L.; Nikitin, M.; Nunez Pardo, T.; Okada, K.; Olchevskii, V.; Pazos, A.; Pentia, M.; Penzo, A.; Perreau, J.-M.; Petrascu, C.; Plo, M.; Ponta, T.; Pop, D.; Riazantsev, A.; Rodriguez, J.M.; Rodriguez Fernandez, A.; Rykaline, V.; Santamarina, C.; Saborido, J.; Schacher, J.; Sidorov, A.; Smolik, J.; Takeutchi, F.; Tarasov, A.; Tauscher, L.; Tobar, M.J.; Trusov, S.; Vazquez, P.; Vlachos, S.; Yazkov, V.; Yoshimura, Y.; Zrelov, P.

    2001-01-01

    The main objective of DIRAC experiment is the measurement of the lifetime τ of the exotic hadronic atom consisting of π + and π - mesons. The lifetime of this atom is determined by the decay mode π + π - → π 0 π 0 due to the strong interaction. Through the precise relationship between the lifetime and the S-wave pion-pion scattering length difference |a 0 - a 2 | for isospin 0 and 2 (respectively), a measurement of τ with an accuracy of 10% will allow a determination of |a 0 - a 2 | at a 5% precision level. Pion-pion scattering lengths have been calculated in the framework of chiral perturbation theory with an accuracy below 5%. In this way DIRAC experiment will provide a crucial test of the chiral symmetry breaking scheme in QCD effective theories at low energies

  20. Dirac experiment

    Energy Technology Data Exchange (ETDEWEB)

    Gomez, F.; Adeva, B.; Afanasev, L.; Benayoun, M.; Brekhovskikh, V.; Caragheorgheopol, G.; Cechak, T.; Chiba, M.; Constantinescu, S.; Doudarev, A.; Dreossi, D.; Drijard, D.; Ferro-Luzzi, M.; Gallas, M.V.; Gerndt, J.; Giacomich, R.; Gianotti, P.; Goldin, D.; Gorin, A.; Gortchakov, O.; Guaraldo, C.; Hansroul, M.; Hosek, R.; Iliescu, M.; Jabitski, M.; Kalinina, N.; Karpoukhine, V.; Kluson, J.; Kobayashi, M.; Kokkas, P.; Komarov, V.; Koulikov, A.; Kouptsov, A.; Krouglov, V.; Krouglova, L.; Kuroda, K.-I.; Lanaro, A.; Lapshine, V.; Lednicky, R.; Leruste, P.; Levisandri, P.; Lopez Aguera, A.; Lucherini, V.; Maki, T.; Manuilov, I.; Montanet, L.; Narjoux, J.-L.; Nemenov, L.; Nikitin, M.; Nunez Pardo, T.; Okada, K.; Olchevskii, V.; Pazos, A.; Pentia, M.; Penzo, A.; Perreau, J.-M.; Petrascu, C.; Plo, M.; Ponta, T.; Pop, D.; Riazantsev, A.; Rodriguez, J.M.; Rodriguez Fernandez, A.; Rykaline, V.; Santamarina, C.; Saborido, J.; Schacher, J.; Sidorov, A.; Smolik, J.; Takeutchi, F.; Tarasov, A.; Tauscher, L.; Tobar, M.J.; Trusov, S.; Vazquez, P.; Vlachos, S.; Yazkov, V.; Yoshimura, Y.; Zrelov, P

    2001-04-01

    The main objective of DIRAC experiment is the measurement of the lifetime {tau} of the exotic hadronic atom consisting of {pi}{sup +} and {pi}{sup -} mesons. The lifetime of this atom is determined by the decay mode {pi}{sup +} {pi}{sup -} {yields} {pi}{sup 0} {pi}{sup 0} due to the strong interaction. Through the precise relationship between the lifetime and the S-wave pion-pion scattering length difference |a{sub 0} - a{sub 2}| for isospin 0 and 2 (respectively), a measurement of {tau} with an accuracy of 10% will allow a determination of |a{sub 0} - a{sub 2}| at a 5% precision level. Pion-pion scattering lengths have been calculated in the framework of chiral perturbation theory with an accuracy below 5%. In this way DIRAC experiment will provide a crucial test of the chiral symmetry breaking scheme in QCD effective theories at low energies.

  1. Russian experience

    International Nuclear Information System (INIS)

    Trabalka, J.R.

    1981-01-01

    Soviet research in terrestrial decontamination appears to have paralleled that of the US in many respects. However, the probability exists that long-term evaluations of decontamination techniques (over 10 to 20 years) have been carried out at one nuclear accident site (a marked divergence from US experience). The area of aquatic decontamination seems to offer the most intriguing possibilities for new information acquisition from the USSR; at this point only its potential importance can be speculated upon

  2. Polarization experiments

    International Nuclear Information System (INIS)

    Halzen, F.

    1977-02-01

    In a theoretical review of polarization experiments two important points are emphasized: (a) their versatility and their relevance to a large variety of aspects of hadron physics (tests of basic symmetries; a probe of strong interaction dynamics; a tool for hadron spectroscopy); (b) the wealth of experimental data on polarization parameters in pp and np scattering in the Regge language and in the diffraction language. (author)

  3. Experiments expectations

    OpenAIRE

    Gorini, B; Meschi, E

    2014-01-01

    This paper presents the expectations and the constraints of the experiments relatively to the commissioning procedure and the running conditions for the 2015 data taking period. The views about the various beam parameters for the p-p period, like beam energy, maximum pileup, bunch spacing and luminosity limitation in IP2 and IP8, are discussed. The goals and the constraints of the 2015 physics program are also presented, including the heavy ions period as well as the special...

  4. Media experiences

    DEFF Research Database (Denmark)

    Buhl, Mie

    2010-01-01

    The paper discusses mediated experiences from the perspective of the visual modality in combination with the multimodal interaction. ICT-studies has a rapid influx of new words and concepts. Digital technology led to a need to describe the convergence of images, text and sound has taken various w...... to educational practices as still more advanced technology emerge and intertwine the scientific areas in new and cross-disciplinary frameworks....

  5. Diagnostics for Pioneer I imploding plasma experiments

    International Nuclear Information System (INIS)

    Lee, P.H.Y.; Benjamin, R.F.; Brownell, J.H.

    1985-01-01

    The Pioneer I series of imploding plasma experiments are aimed at collapsing a thin aluminum foil with a multimegampere, submicrosecond electrical pulse produced by an explosive flux compression generator and fast plasma compression opening switch. Anticipated experimental conditions are bounded by implosion velocities of 2 x 10 7 cm/s and maximum plasma temperatures of 100 eV. A comprehensive array of diagnostics have been deployed to measure implosion symmetry (gated microchannel plate array and other time-resolved imaging), temperature of the imploding plasma (visible/uv spectroscopy), stagnation geometry (x-ray pinhole imaging), radiation emission characteristics at pinch (XRD's, fast bolometry), and electrical drive history (Rogowski loops, Faraday rotation current detectors, and capacitive voltage probes). Diagnostic performance is discussed and preliminary results are presented

  6. TRISTAN experiment

    International Nuclear Information System (INIS)

    Iwata, Seigi

    1994-01-01

    Any successor to PETRA and PEP colliders was expected to extend the energy range to the region where the weak interaction effect becomes sizable in annihilation process. The aim was to reach the level, at which the all round study of the standard model can be performed in a clean system of e + e - collision. Also it was aimed to explore the energy region where top quark pair production is likely. Considering the available site for accelerator construction and the expected size of the electroweak interference effect, the target energy was set at 60 GeV at the lowest. TRISTAN-1 experiment is a big initial step in the long range physics program. The laboratory established the plan to move on to TRISTAN-2 (B Factory) project. The TRISTAN accelerator including the main storage ring, the time sequence of storage ring operation, three experimental groups of AMY, TOPAZ and VENUS, and so on are explained. The experiments on basic annihilation process, the search for new particles, the electroweak interaction, QCD studies and so on are reported. The optimum TRISTAN ring was estimated as 3 km in diameter, but the largest possible size in the site was 1/3 of that. Hard decision was made to equip the ring with unusually many accelerating RF cavities and to apply superconducting technology. (K.I.)

  7. Experimenting with a design experiment

    Directory of Open Access Journals (Sweden)

    Bakker, Judith

    2012-12-01

    Full Text Available The design experiment is an experimental research method that aims to help design and further develop new (policy instruments. For the development of a set of guidelines for the facilitation of citizens’ initiatives by local governments, we are experimenting with this method. It offers good opportunities for modeling interventions by testing their instrumental validity –the usefulness for the intended practical purposes. At the same time design experiments are also useful for evaluating the empirical validity of theoretical arguments and the further development of these arguments in the light of empirical evidence (by using e.g. the technique of pattern matching. We describe how we have applied this methodology in two cases and discuss our research approach. We encountered some unexpected difficulties, especially in the cooperation with professionals and citizens. These difficulties complicate the valid attribution of causal effects to the use of the new instrument. However, our preliminary conclusion is that design experiments are useful in our field of study

    El experimento de diseño es un método de investigación experimental que tiene como objetivo diseñar y desarrollar posteriormente nuevas herramientas (políticas. En este artículo experimentamos con este método para desarrollar un conjunto de directrices que permitan a los gobiernos locales facilitar las iniciativas ciudadanas. El método ofrece la oportunidad de modelar las intervenciones poniendo a prueba su validez instrumental (su utilidad para el fin práctico que se proponen. Al mismo tiempo, los experimentos de diseño son útiles también para evaluar la validez empírica de las discusiones teóricas y el posterior desarrollo de esas discusiones a la luz de la evidencia empírica (usando, por ejemplo, técnicas de concordancia de patrones. En este trabajo describimos cómo hemos aplicado este método a dos casos y discutimos nuestro enfoque de

  8. Operating experience

    International Nuclear Information System (INIS)

    McRae, L.P.; Six, D.E.

    1991-01-01

    In 1987, Westinghouse Hanford Company began operating a first-generation integrated safeguards system in the Plutonium Finishing Plant storage vaults. This Vault Safety and Inventory System is designed to integrate data into a computer-based nuclear material inventory monitoring system. The system gathers, in real time, measured physical parameters that generate nuclear material inventory status data for thousands of stored items and sends tailored report to the appropriate users. These data include canister temperature an bulge data reported to Plant Operations and Material Control and Accountability personnel, item presence and identification data reported to Material Control and Accountability personnel, and unauthorized item movement data reported to Security response forces and Material Control and Accountability personnel. The Westinghouse Hanford Company's experience and operational benefits in using this system for reduce radiation exposure, increase protection against insider threat, and real-time inventory control are discussed in this paper

  9. Management Experiences

    Directory of Open Access Journals (Sweden)

    Gheorghe Popovici

    2016-12-01

    Full Text Available The paper presents the results of the survey about the changes in modern management, identified from the experience of Romanian managers. By this online study one presents both the obstacles encountered and the recommendations for such a type of management that the present and future mangers must take into account. What motivated the respondent Romanian managers most to open their own business is the independence it offered them. They work in the field they have liked since they were young. The second reason was the perspective to have an additional income from the business development. The third argument in favour of opening a business is the possibility to assure the balance between personal life and career.

  10. X-ray diffraction without sample preparation: Proof-of-principle experiments

    International Nuclear Information System (INIS)

    Hansford, Graeme M.

    2013-01-01

    The properties of a novel X-ray diffraction (XRD) technique having very low sensitivity to the sample morphology were previously elucidated through theoretical considerations and model simulations (Hansford, 2011). This technique opens up the possibility of mineralogical analysis by XRD without sample preparation. Here, the results of proof-of-principle experimental tests are presented. Two sets of experiments were performed using a vacuum chamber equipped with an X-ray tube source, sample holder and charge-coupled detector. Firstly, a pressed-powder pellet of α-quartz was placed in three different positions relative to the X-ray source and detector. The changes in position represent gross sample movements which would be inconceivable in conventional XRD analysis. The resulting back-reflection energy-dispersive spectra show a very high degree of correspondence other than an overall intensity factor dependent on the distance between the sample and detector. Secondly, the back-reflection spectrum of an unprepared limestone hand specimen, having mm-scale surface morphology, was compared to the spectrum of a calcite pressed-powder pellet. The correspondence of the diffraction peaks in the spectra demonstrate that the limestone is comprised dominantly of calcite. In both cases, the claims of the earlier paper are fully supported by the results of these experimental tests. -- Highlights: • Proof-of-principle tests of a novel X-ray diffraction (XRD) method were conducted. • Very low sensitivity to sample position and orientation was demonstrated. • Insensitivity to sample morphology is inferred. • A simple analysis of an unprepared limestone hand specimen was performed. • This technique enables mineralogical analysis by XRD without sample preparation

  11. Kinetic and morphological differentiation of ettringites in plain and blended Portland cements with metakaolin and the ASTM C 452-68 test. Part II: Morphological differentiation by SEM and XRD analysis

    Directory of Open Access Journals (Sweden)

    Talero, R.

    2009-03-01

    Full Text Available The same cementitious materials (OPCs, SRPCs and matekaolin, MK, the same blended cements and the same ASTM C 452-68 test than in Part I, were used. Other complementary determinations were: chemical analysis of cementing materials, SEM and XRD analysis of ettringites and specific properties of some cement tested and of their pastes.The experimental results have also demonstrated that when 7.0% SO3, equivalent to 15.05% of gypsum, was added to the M pozzolan-containing Portland cement and tested with the ASTM C 452-68 method, it was not found to behave aggressively but rather as “setting regulator ”, because the increase in mechanical strengths over time and setting times in these mixes were, therefore, similar to the pattern observed in any PC. However, when the gypsum content was raised to triple than that amount (21.0% SO3, it behaved aggressively. In both cases, logically, ettringite from both origins were involved in the resulting beneficial or adverse behavior.En esta Parte II se utilizaron los mismos materiales cementíceos (CPO, CPRS, y metakaolín, MK, los mismos cementos de mezcla y el mismo método de ensayo ASTM C 452-68 que en la Parte I. Otras determinaciones complementarias fueron: análisis químico de los materiales cementíceos, análisis por DRX y SEM de ettringitas y propiedades específicas de algunos cementos ensayados y de sus pastas.Los resultados experimentales obtenidos han demostrado también que, el 7.0% de SO3 presente en los 30 cementos de mezcla con MK, ensayados conforme el método ASTM C 452-68, no se comporta como agresivo sino como ”regulador de fraguado”, porque los tiempos de fraguado y el aumento de resistencias mecánicas fueron como los de cualquier CP. De aquí que algunos de esos cementos de mezcla puedan ser considerados “cementos hidráulicos expansivos”, el resto, no. Sin embargo, cuando la cantidad de yeso aportada fue el triple (21,0% SO3, se comportó como agresivo, motivo por el cual

  12. Injection Methods and Instrumentation for Serial X-ray Free Electron Laser Experiments

    Science.gov (United States)

    James, Daniel

    Scientists have used X-rays to study biological molecules for nearly a century. Now with the X-ray free electron laser (XFEL), new methods have been developed to advance structural biology. These new methods include serial femtosecond crystallography, single particle imaging, solution scattering, and time resolved techniques. The XFEL is characterized by high intensity pulses, which are only about 50 femtoseconds in duration. The intensity allows for scattering from microscopic particles, while the short pulses offer a way to outrun radiation damage. XFELs are powerful enough to obliterate most samples in a single pulse. While this allows for a "diffract and destroy" methodology, it also requires instrumentation that can position microscopic particles into the X-ray beam (which may also be microscopic), continuously renew the sample after each pulse, and maintain sample viability during data collection. Typically these experiments have used liquid microjets to continuously renew sample. The high flow rate associated with liquid microjets requires large amounts of sample, most of which runs to waste between pulses. An injector designed to stream a viscous gel-like material called lipidic cubic phase (LCP) was developed to address this problem. LCP, commonly used as a growth medium for membrane protein crystals, lends itself to low flow rate jetting and so reduces the amount of sample wasted significantly. This work discusses sample delivery and injection for XFEL experiments. It reviews the liquid microjet method extensively, and presents the LCP injector as a novel device for serial crystallography, including detailed protocols for the LCP injector and anti-settler operation.

  13. The formation and structure of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 6.4}: XRD Rietveld, Mössabuer and XPS analyses

    Energy Technology Data Exchange (ETDEWEB)

    Al-Rawas, A.D., E-mail: arawas@squ.edu.om [Department of Physics, Sultan Qaboos University, P.O. Box 36, 123 Al-Khoud, Muscat (Oman); Widatallah, H.M.; Al-Harthi, S.H. [Department of Physics, Sultan Qaboos University, P.O. Box 36, 123 Al-Khoud, Muscat (Oman); Johnson, C. [Chemistry Department, Open University, Walton Hall, Milton Keynes MK7 6AA (United Kingdom); Gismelseed, A.M.; Elzain, M.E.; Yousif, A.A. [Department of Physics, Sultan Qaboos University, P.O. Box 36, 123 Al-Khoud, Muscat (Oman)

    2015-05-15

    Highlights: • The formation of mechano-synthesized nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} is investigated. • Pre-milling the reactants substantially lowers the formation temperature. • The core and surface structures were studied. • XRD and {sup 57}Fe Mössbauer spectroscopic analyses indicate the δ-value to be 0.60. • XPS shows a complex surface structure for the mechanosynthesized Sr{sub 3}Fe{sub 2}O{sub 7−δ} nanoparticles. - Abstract: The influence of ball milling and subsequent sintering of a 3:1 molar mixture of SrCO{sub 3} and α-Fe{sub 2}O{sub 3} on the formation of Sr{sub 3}Fe{sub 2}O{sub 7−δ} double perovskite is investigated with different analytical techniques. Milling the mixture for 110 h leads to the formation of SrCO{sub 3}-α-Fe{sub 2}O{sub 3} nanocomposites and the structural deformation of α-Fe{sub 2}O{sub 3} via the incorporation of Sr{sup 2+} ions. Subsequent sintering of the pre-milled reactants’ mixture has led to the partial formation of an SrFeO{sub 3} perovskite-related phase in the temperature range 400–600 °C. This was followed by the progressive development of an Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase that continued to increase with increasing sintering temperature until a single-phased nanocrystalline Sr{sub 3}Fe{sub 2}O{sub 7−δ} phase was attained at 950 °C (12 h). This temperature is ∼350 °C lower than the temperature at which the material is prepared conventionally using the ceramic method. The evolution of different structural phases during the reaction process is discussed. Rietveld refinement of the X-ray diffraction data shows a value of 0.60 for the oxygen deficiency δ, in consistency with the Fe{sup 3+}/Fe{sup 4+} ratio derived from the {sup 57}Fe Mössbauer data recorded at both 300 K and 78 K. The Mössbauer data suggests that the Sr{sub 3}Fe{sub 2}O{sub 6.4} nanoparticles are superparamagnetic with blocking temperatures below 78 K. The surfaces of the Sr{sub 3}Fe{sub 2}O{sub 6

  14. Self-organization of single filaments and diffusive plasmas during a single pulse in dielectric-barrier discharges

    International Nuclear Information System (INIS)

    Babaeva, Natalia Yu; Kushner, Mark J

    2014-01-01

    Self-organization of filaments in dielectric-barrier discharges (DBDs) probably has many origins. However, the dominant cause is proposed to be the accumulation of charge on the surfaces of the bounding dielectrics that reinforces successive discharge pulses to occur at the same locations. A secondary cause is the electrostatic repulsion of individual plasma filaments. Self-organization typically develops over many discharge pulses. In this paper, we discuss the results of a computational investigation of plasma filaments in overvoltage DBDs that, under select conditions, display self-organized patterns (SOPs) of plasma density during a single discharge pulse. (Overvoltage refers to the rapid application of a voltage in excess of the quasi-dc breakdown voltage.) The origin of the SOPs is a synergistic relationship between the speed of the surface-ionization waves that propagate along each dielectric and the rate at which avalanche occurs across the gap. For our test conditions, SOPs were not observed at lower voltages and gradually formed at higher voltages. The same conditions that result in SOPs, i.e. the application of an overvoltage, also produce more diffuse discharges. A transition from a single narrow filament to a more diffuse structure was observed as overvoltage was approached. The sensitivity of SOPs to the orientation and permittivity of the bounding dielectrics is discussed. (paper)

  15. Chlorides behavior in raw fly ash washing experiments.

    Science.gov (United States)

    Zhu, Fenfen; Takaoka, Masaki; Oshita, Kazuyuki; Kitajima, Yoshinori; Inada, Yasuhiro; Morisawa, Shinsuke; Tsuno, Hiroshi

    2010-06-15

    Chloride in fly ash from municipal solid waste incinerators (MSWIs) is one of the obstructive substances in recycling fly ash as building materials. As a result, we have to understand the behavior of chlorides in recycling process, such as washing. In this study, we used X-ray absorption near edge structure (XANES) and X-ray diffraction (XRD) to study the chloride behavior in washed residue of raw fly ash (RFA). We found that a combination of XRD and XANES, which is to use XRD to identify the situation of some compounds first and then process XANES data, was an effective way to explain the chlorides behavior in washing process. Approximately 15% of the chlorine in RFA was in the form of NaCl, 10% was in the form of KCl, 51% was CaCl(2), and the remainder was in the form of Friedel's salt. In washing experiments not only the mole percentage but also the amount of soluble chlorides including NaCl, KCl and CaCl(2) decreases quickly with the increase of liquid to solid (L/S) ratio or washing frequency. However, those of insoluble chlorides decrease slower. Moreover, Friedel's salt and its related compound (11CaO.7Al(2)O(3).CaCl(2)) were reliable standards for the insoluble chlorides in RFA, which are strongly related to CaCl(2). Washing of RFA promoted the release of insoluble chlorides, most of which were in the form of CaCl(2). Copyright 2010 Elsevier B.V. All rights reserved.

  16. Particle physics experiments 1983

    International Nuclear Information System (INIS)

    Stuart, G.W.

    1983-01-01

    The report describes work carried out in 1983 on experiments approved by the Particle Physics Experiments Selection Panel. The contents consist of unedited contributions from each experiment. (author)

  17. Design of modern experiments

    International Nuclear Information System (INIS)

    Park, Sung Hweon

    1984-03-01

    This book is for researchers and engineers, which is written to focus on practical design of experiments. It gives descriptions of conception of design of experiments, basic statistics theory, one way design of experiment, two-way layout without repetition, two-way layout with repetition, partition, a correlation analysis and regression analysis, latin squares, factorial design, design of experiment by table of orthogonal arrays, design of experiment of response surface, design of experiment on compound, Evop, and design of experiment of taguchi.

  18. Data acquisition. GRAAL experiment. Hybrid reactor experiment. AMS experiment

    International Nuclear Information System (INIS)

    Barancourt, D.; Barbier, G.; Bosson, G.; Bouvier, J.; Gallin-Martel, L.; Meillon, B.; Stassi, P.; Tournier, M.

    1997-01-01

    The main activity of the data acquisition team has consisted in hardware and software developments for the GRAAL experiment with the trigger board, for the 'Reacteurs Hybrides' group with an acquisition board ADCVME8V and for the AMS experiment with the monitoring of the aerogel detector. (authors)

  19. Particle physics experiments 1989

    International Nuclear Information System (INIS)

    Bairstow, R.

    1990-01-01

    This report describes work carried out in 1989 on experiments approved by the Particle Physics Experiments Selection Panel of Rutherford Appleton Laboratory. The contents consist of unedited contributions from each experiment. (author)

  20. Particle physics experiments 1987

    International Nuclear Information System (INIS)

    Stuart, G.W.

    1988-01-01

    This report describes work carried out in 1987 on experiments approved by the Particle Physics Experiments Selection Panel (United Kingdom). The contents consist of unedited contributions from each experiment. (author)

  1. Particle physics experiments

    International Nuclear Information System (INIS)

    Stuart, G.W.

    1986-01-01

    The report of the Rutherford Appleton Laboratory describes the work carried out in 1985 on experiments approved by the Particle Physics Experiments Selection Panel. The contents consist of unedited contributions from each experiment. (author)

  2. Particle physics experiments 1986

    International Nuclear Information System (INIS)

    Stuart, G.W.

    1987-01-01

    The paper presents research work carried out in 1986 on 52 elementary particle experiments approved by the Particle Physics Experiments Selection Panel. Most of the experiments were collaborative and involved research groups from different countries. About half of the experiments were conducted at CERN, the remaining experiments employed the accelerators: LAMPT, LEP, PETRA, SLAC, and HERA. The contents consist of unedited contributions from each experiment. (U.K.)

  3. Simfuel dissolution studies in granitic groundwater leaching experiments at VTT

    International Nuclear Information System (INIS)

    Ollila, K.

    1992-12-01

    The dissolution behaviour of an irradiated analogue of spent nuclear fuel, SIMFUEL, was studied in synthetic granitic groundwater. The release of uranium and the minor components was monitored during static (bach) leaching experiments in oxic and anoxic (N 2 ) atmosphere at 25 deg C. Molybdenum, ruthenium, barium and zirconium showed a trend to congruent dissolution behaviour with UO 2 matrix towards the end of the experimental time (540 days) under anoxic conditions. Under oxic conditions, molybdenum and strontium had higher release rates relative to the matrix (the exp. time of 220 days). The presence of particulate material in the leachates in anoxic atmosphere was shown by SEM/EDX and XRD analyses. The material retained on membrane after filtration consisted of Ca-rich and U-rich particles in addition to finely divided material. Calcite (CaCO 3 ) and uranium oxide were identified. (orig.)

  4. Synthesis and in vitro Experiment of Biomaterial Tricalcium Phosphate

    Directory of Open Access Journals (Sweden)

    X.V Bui

    2016-12-01

    as an ideal candidate for bone graft in hard tissue engineering due to its high biocompatibility, bioactivity and bone bonding. The preparation, as well as the application of this powder material, has been the important topic of research in material science. In this paper, β-tricalcium phosphate (β-TCP, a component that has chemical formulation similar to bone structure, was synthesized by the precipitate method and then calcinated at 1000oC for 5 h. The physico-chemical properties of synthetic material were examined by XRD, FT-IR and SEM methods. In vitro experience was also carried by soaking β-TCP simulated body fluid powder in a different period of time. Obtained results confirmed the quality of β-TCP synthetic material and its bioactivity.

  5. Kinetics and structural changes of Li-rich layered oxide 0.5Li2MnO3·0.5LiNi(0.292)Co(0.375)Mn(0.333)O2 material investigated by a novel technique combining in situ XRD and a multipotential step.

    Science.gov (United States)

    Shen, Chong-Heng; Huang, Ling; Lin, Zhou; Shen, Shou-Yu; Wang, Qin; Su, Hang; Fu, Fang; Zheng, Xiao-Mei

    2014-08-13

    Li-rich layered oxide 0.5Li2MnO3·0.5LiNi0.292Co0.375Mn0.333O2 was prepared by an aqueous solution-evaporation route. X-ray powder diffraction (XRD) showed that the as-synthesized material was a solid solution consisting of layered α-NaFeO2-type LiMO2 (M = Ni, Co, Mn) and monoclinic Li2MnO3. The superlattice spots in the selected area electron diffraction pattern indicated the ordering of lithium ions with transition metal (TM) ions in TM layers in this Li-rich layered oxide. Electrochemical performance testing showed that the as-synthesized material could deliver an initial discharge capacity of 267.7 mAh/g, with a capacity retention of 88.5% after 33 cycles. A new combination technique, multipotential step in situ XRD (MPS in situ XRD) measurement, was applied for the first time to investigate the Li-rich layered oxide. Using this approach, the relationships between kinetics and structural variations can be obtained simutaneously. In situ XRD results showed that the c parameter decreased from 3.70 to 4.30 V and increased from 4.30 to 4.70 V, whereas the a parameter underwent a decrease above 4.30 V during the first charge process. Below 3.90 V during the first discharge process, a slight decrease in the c parameter was found along with an increase in the a parameter. During the first charge process, the value of the coefficient of diffusion for lithium ions (DLi+) decreased to its mininum at 4.55 V, which might be associated with Ni(2+) migration, as indicated by both Ni occupancy in 3b sites (Ni3b%) in the Li(+) layers and complicated chemical reactions. Remarkably, a lattice distortion might occur within the local domain in the host stucture during the first discharge process, indicated by a slight splitting of the (003) diffraction peak at 3.20 V.

  6. Concrete/Febex Bentonite Interaction: Results On Short-Term Column Experiments

    Energy Technology Data Exchange (ETDEWEB)

    Escribano, A.; Turrero, M.J.; Torres, E.; Martin, P.L. [CIEMAT, Environmental Department, Avda. Complutense, 22, 28040 Madrid (Spain)

    2008-07-01

    Interaction between the alkaline pore fluids from the concrete engineered barriers and the bentonite at the repository conditions may generate products that can diffuse through the porous structure of the bentonite affecting their properties. A comprehensive study based on series of short term experiments is being performed to provide experimental evidences on the physical, chemical and mineralogical changes during the concrete-compacted bentonite interaction. Samples were analyzed by XRD, SEM-EDS and FTIR. Measurements of swelling capacity, specific surface area and chemical analysis for cation exchange capacity and soluble salts analyses were also performed. (authors)

  7. Concrete/Febex Bentonite Interaction: Results On Short-Term Column Experiments

    International Nuclear Information System (INIS)

    Escribano, A.; Turrero, M.J.; Torres, E.; Martin, P.L.

    2008-01-01

    Interaction between the alkaline pore fluids from the concrete engineered barriers and the bentonite at the repository conditions may generate products that can diffuse through the porous structure of the bentonite affecting their properties. A comprehensive study based on series of short term experiments is being performed to provide experimental evidences on the physical, chemical and mineralogical changes during the concrete-compacted bentonite interaction. Samples were analyzed by XRD, SEM-EDS and FTIR. Measurements of swelling capacity, specific surface area and chemical analysis for cation exchange capacity and soluble salts analyses were also performed. (authors)

  8. Particle physics experiments 1982

    International Nuclear Information System (INIS)

    Rousseau, M.D.; Stuart, G.

    1983-01-01

    Work carried out in 1982 on 52 experiments approved by the Particle Physics Experiments Selection Panel is described. Each experiment is listed under title, collaboration, technique, accelerator, year of running, status and spokesman. Unedited contributions are given from each experiment. (U.K.)

  9. Framework of product experience

    NARCIS (Netherlands)

    Desmet, P.; Hekkert, P.

    2007-01-01

    In this paper, we introduce a general framework for product experience that applies to all affective responses that can be experienced in human-product interaction. Three distinct components or levels of product experiences are discussed: aesthetic experience, experience of meaning, and emotional

  10. Adaptive structures flight experiments

    Science.gov (United States)

    Martin, Maurice

    The topics are presented in viewgraph form and include the following: adaptive structures flight experiments; enhanced resolution using active vibration suppression; Advanced Controls Technology Experiment (ACTEX); ACTEX program status; ACTEX-2; ACTEX-2 program status; modular control patch; STRV-1b Cryocooler Vibration Suppression Experiment; STRV-1b program status; Precision Optical Bench Experiment (PROBE); Clementine Spacecraft Configuration; TECHSAT all-composite spacecraft; Inexpensive Structures and Materials Flight Experiment (INFLEX); and INFLEX program status.

  11. Renewed lab banks on experience

    International Nuclear Information System (INIS)

    Herzig, Janine

    2007-01-01

    South Australia has huge uranium resources, Amdel has opened a new mineral processing facility in Wingfield, Adelaide. The facility originally was focused solely on mineral processing activities, that included crushing, screening, flotation and leaching. There are plans to open a dedicated uranium processing materials facility in Wingfield. A unique part of Amdel's geo-analytical business is the x-ray diffraction (XRD), and asbestos identification capability

  12. Reversible photo-induced trap formation in mixed-halide hybrid perovskites for photovoltaics† †Electronic supplementary information (ESI) available: Experimental details, PL, PDS spectra and XRD patterns. See DOI: 10.1039/c4sc03141e Click here for additional data file.

    Science.gov (United States)

    Hoke, Eric T.; Slotcavage, Daniel J.; Dohner, Emma R.; Bowring, Andrea R.

    2015-01-01

    We report on reversible, light-induced transformations in (CH3NH3)Pb(BrxI1–x)3. Photoluminescence (PL) spectra of these perovskites develop a new, red-shifted peak at 1.68 eV that grows in intensity under constant, 1-sun illumination in less than a minute. This is accompanied by an increase in sub-bandgap absorption at ∼1.7 eV, indicating the formation of luminescent trap states. Light soaking causes a splitting of X-ray diffraction (XRD) peaks, suggesting segregation into two crystalline phases. Surprisingly, these photo-induced changes are fully reversible; the XRD patterns and the PL and absorption spectra revert to their initial states after the materials are left for a few minutes in the dark. We speculate that photoexcitation may cause halide segregation into iodide-rich minority and bromide-enriched majority domains, the former acting as a recombination center trap. This instability may limit achievable voltages from some mixed-halide perovskite solar cells and could have implications for the photostability of halide perovskites used in optoelectronics. PMID:28706629

  13. The ERASMUS experiment archive

    Science.gov (United States)

    Isakeit, Dieter; Sabbatini, Massimo; Carey, William

    2005-08-01

    The Erasmus Experiment Archive is an electronic database, accessible through the Internet, that collects in a single reference repository scientific, technical and operational information regarding the experiments performed in the experiment facilities which fall under the responsibility of the ESA Directorate of Human Spaceflight, Microgravity and Exploration. The archive is operated, filled with content and kept up-to-date by the Erasmus User Centre. which forms part of the Directorate. The archive shares its records and is interoperable with similar experiment archives of the partner agencies NASA USA) and JAXA (Japan) through a mutually agreed standard for experiment records called the International Distributed Experiment Archive (IDEA).

  14. Experiment WA1 (CDHS Neutrino Experiment)

    CERN Multimedia

    CERN PhotoLab

    1977-01-01

    Experiment WA1, also known under CDHS (CERN, Dortmund, Heidelberg, Saclay; spokesman Jack Steinberger), was the first neutrino experiment on the SPS, in its West Area. Magnetized iron (with a toroidal field) forms the core of the detector. On its outside we see drift chambers and photomultipliers (detecting the light from the plastic scintillators further in). Peter Schilly is wearing a white coat. See also CERN Annual Report 1976, p.57.

  15. Neutron delayed choice experiments

    International Nuclear Information System (INIS)

    Bernstein, H.J.

    1986-01-01

    Delayed choice experiments for neutrons can help extend the interpretation of quantum mechanical phenomena. They may also rule out alternative explanations which static interference experiments allow. A simple example of a feasible neutron test is presented and discussed. (orig.)

  16. Particle physics experiments 1984

    International Nuclear Information System (INIS)

    Stuart, G.

    1985-01-01

    The Rutherford Appleton laboratory report describes work carried out in 1984 on experiments approved by the Particle Physics selection panel. The contents consist of unedited contributions from each experiment. (author)

  17. GARP Atlantic Tropical Experiment

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — The GARP Atlantic Tropical Experiment (GATE) was the first major international experiment of the Global Atmospheric Research Program (GARP). It was conducted over...

  18. Double beta decay: experiments

    International Nuclear Information System (INIS)

    Fiorini, Ettore

    2006-01-01

    The results obtained so far and those of the running experiments on neutrinoless double beta decay are reviewed. The plans for second generation experiments, the techniques to be adopted and the expected sensitivities are compared and discussed

  19. Organic chemistry experiment

    International Nuclear Information System (INIS)

    Mun, Seok Sik

    2005-02-01

    This book deals with organic chemistry experiments, it is divided five chapters, which have introduction, the way to write the experiment report and safety in the laboratory, basic experiment technic like recrystallization and extraction, a lot of organic chemistry experiments such as fischer esterification, ester hydrolysis, electrophilic aromatic substitution, aldol reaction, benzoin condensation, wittig reaction grignard reaction, epoxidation reaction and selective reduction. The last chapter introduces chemistry site on the internet and way to find out reference on chemistry.

  20. The Experiment Factory: standardizing behavioral experiments

    Directory of Open Access Journals (Sweden)

    Vanessa V Sochat

    2016-04-01

    Full Text Available The administration of behavioral and experimental paradigms for psychology research is hindered by lack of a coordinated effort to develop and deploy standardized paradigms. While several frameworks (de Leeuw (2015; McDonnell et al. (2012; Mason and Suri (2011; Lange et al. (2015 have provided infrastructure and methods for individual research groups to develop paradigms, missing is a coordinated effort to develop paradigms linked with a system to easily deploy them. This disorganization leads to redundancy in development, divergent implementations of conceptually identical tasks, disorganized and error-prone code lacking documentation, and difficulty in replication. The ongoing reproducibility crisis in psychology and neuroscience research (Baker (2015; Open Science Collaboration (2015 highlights the urgency of this challenge: reproducible research in behavioral psychology is conditional on deployment of equivalent experiments. A large, accessible repository of experiments for researchers to develop collaboratively is most efficiently accomplished through an open source framework. Here we present the Experiment Factory, an open source framework for the development and deployment of web-based experiments. The modular infrastructure includes experiments, virtual machines for local or cloud deployment, and an application to drive these components and provide developers with functions and tools for further extension. We release this infrastructure with a deployment (http://www.expfactory.org that researchers are currently using to run a set of over 80 standardized web-based experiments on Amazon Mechanical Turk. By providing open source tools for both deployment and development, this novel infrastructure holds promise to bring reproducibility to the administration of experiments, and accelerate scientific progress by providing a shared community resource of psychological paradigms.

  1. Future of neutrino experiments

    Indian Academy of Sciences (India)

    them are under construction. The next generation double beta decay experiments are sensitive to the inverted mass hierarchy. In order to explore the normal mass hierarchy, the sensitivity of the experiments still needs to be improved substantially. For example, see [32] for more details of the double beta decay experiments.

  2. Particle physics experiments 1988

    International Nuclear Information System (INIS)

    Bairstow, R.

    1989-01-01

    This report describes work carried out in 1988 on experiments approved by the Particle Physics Experiments Selection Panel. The contents consist of unedited contributions from each experiment. More than forty projects at different accelerators (SPS, ISIS, PETRA, LAMPF, LEP, HERA, BNL, ILL, LEAR) are listed. Different organisations collaborate on different projects. A brief progress report is given. References to published articles are given. (author)

  3. The Game Experience Questionnaire

    NARCIS (Netherlands)

    IJsselsteijn, W.A.; de Kort, Y.A.W.; Poels, K.

    2013-01-01

    This document contains the English version of the Game Experience Questionnaire. The development and testing of the Game Experience Questionnaire is described in project Deliverable 3.3. The Game Experience Questionnaire has a modular structure and consists of : 1. The core questionnaire 2. The

  4. Facile synthesis of the Li-rich layered oxide Li1.23Ni0.09Co0.12Mn0.56O2 with superior lithium storage performance and new insights into structural transformation of the layered oxide material during charge-discharge cycle: in situ XRD characterization.

    Science.gov (United States)

    Shen, Chong-Heng; Wang, Qin; Fu, Fang; Huang, Ling; Lin, Zhou; Shen, Shou-Yu; Su, Hang; Zheng, Xiao-Mei; Xu, Bin-Bin; Li, Jun-Tao; Sun, Shi-Gang

    2014-04-23

    In this work, the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 was synthesized through a facile route called aqueous solution-evaporation route that is simple and without waste water. The as-prepared Li1.23Ni0.09Co0.12Mn0.56O2 oxide was confirmed to be a layered LiMO2-Li2MnO3 solid solution through ex situ X-ray diffraction (ex situ XRD) and transmission electron microscopy (TEM). Electrochemical results showed that the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material can deliver a discharge capacity of 250.8 mAhg(-1) in the 1st cycle at 0.1 C and capacity retention of 86.0% in 81 cycles. In situ X-ray diffraction technique (in situ XRD) and ex situ TEM were applied to study structural changes of the Li-rich oxide Li1.23Ni0.09Co0.12Mn0.56O2 material during charge-discharge cycles. The study allowed observing experimentally, for the first time, the existence of β-MnO2 phase that is appeared near 4.54 V in the first charge process, and a phase transformation of the β-MnO2 to layered Li0.9MnO2 is occurred in the initial discharge process by evidence of in situ XRD pattrens and selected area electron diffraction (SAED) patterns at different states of the initial charge and discharge process. The results illustrated also that the variation of the in situ X-ray reflections during charge-discharge cycling are clearly related to the changes of lattice parameters of the as-prepared Li-rich oxide during the charge-discharge cycles.

  5. Virtual neutron scattering experiments

    DEFF Research Database (Denmark)

    Overgaard, Julie Hougaard; Bruun, Jesper; May, Michael

    2017-01-01

    . In the last week of the course, students travel to a large-scale neutron scattering facility to perform real neutron scattering experiments. Through student interviews and survey answers, we argue, that the virtual training prepares the students to engage more fruitfully with experiments by letting them focus......We describe how virtual experiments can be utilized in a learning design that prepares students for hands-on experiments at large-scale facilities. We illustrate the design by showing how virtual experiments are used at the Niels Bohr Institute in a master level course on neutron scattering...

  6. Experiments in physical chemistry

    CERN Document Server

    Wilson, J M; Denaro, A R

    1968-01-01

    Experiments in Physical Chemistry, Second Edition provides a compilation of experiments concerning physical chemistry. This book illustrates the link between the theory and practice of physical chemistry. Organized into three parts, this edition begins with an overview of those experiments that generally have a simple theoretical background. Part II contains experiments that are associated with more advanced theory or more developed techniques, or which require a greater degree of experimental skill. Part III consists of experiments that are in the nature of investigations wherein these invest

  7. Virtual neutron scattering experiments

    DEFF Research Database (Denmark)

    Overgaard, Julie Hougaard; Bruun, Jesper; May, Michael

    2016-01-01

    We describe how virtual experiments can be utilized in a learning design that prepares students for hands-on experiments at large-scale facilities. We illustrate the design by showing how virtual experiments are used at the Niels Bohr Institute in a master level course on neutron scattering....... In the last week of the course, students travel to a large-scale neutron scattering facility to perform real neutron scattering experiments. Through student interviews and survey answers, we argue, that the virtual training prepares the students to engage more fruitfully with experiments by letting them focus...... on physics and data rather than the overwhelming instrumentation. We argue that this is because they can transfer their virtual experimental experience to the real-life situation. However, we also find that learning is still situated in the sense that only knowledge of particular experiments is transferred...

  8. The Belle II Experiment

    CERN Document Server

    Kahn, J

    2017-01-01

    Set to begin data taking at the end of 2018, the Belle II experiment is the next-generation B-factory experiment hosted at KEK in Tsukuba, Japan. The experiment represents the cumulative effort from the collaboration of experimental and detector physics, computing, and software development. Taking everything learned from the previous Belle experiment, which ran from 1998 to 2010, Belle II aims to probe deeper than ever before into the field of heavy quark physics. By achieving an integrated luminosity of 50 ab−1 and accumulating 50 times more data than the previous experiment across its lifetime, along with a rewritten analysis framework, the Belle II experiment will push the high precision frontier of high energy physics. This paper will give an overview of the key components and development activities that make the Belle II experiment possible.

  9. Infrared spectra, Raman laser, XRD, DSC/TGA and SEM ...

    Indian Academy of Sciences (India)

    Administrator

    cussed and the X-ray diffraction, scanning electron microscopy (SEM) and atomic force microscope (AFM) ... acetamide as a simple organic compound at high tempera- ture has less ..... properties of selenium surface, AFM-microscopy tapping.

  10. 3-Iodobenzaldehyde: XRD, FT-IR, Raman and DFT studies.

    Science.gov (United States)

    Kumar, Chandraju Sadolalu Chidan; Parlak, Cemal; Tursun, Mahir; Fun, Hoong-Kun; Rhyman, Lydia; Ramasami, Ponnadurai; Alswaidan, Ibrahim A; Keşan, Gürkan; Chandraju, Siddegowda; Quah, Ching Kheng

    2015-06-15

    The structure of 3-iodobenzaldehyde (3IB) was characterized by FT-IR, Raman and single-crystal X-ray diffraction techniques. The conformational isomers, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of 3IB were examined using density functional theory (DFT) method, with the Becke-3-Lee-Yang-Parr (B3LYP) functional and the 6-311+G(3df,p) basis set for all atoms except for iodine. The LANL2DZ effective core basis set was used for iodine. Potential energy distribution (PED) analysis of normal modes was performed to identify characteristic frequencies. 3IB crystallizes in monoclinic space group P21/c with the O-trans form. There is a good agreement between the theoretically predicted structural parameters, and vibrational frequencies and those obtained experimentally. In order to understand halogen effect, 3-halogenobenzaldehyde [XC6H4CHO; X=F, Cl and Br] was also studied theoretically. The free energy difference between the isomers is small but the rotational barrier is about 8kcal/mol. An atypical behavior of fluorine affecting conformational preference is observed. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. In-Situ XRD during Electrochemical CO Reduction on Cu

    DEFF Research Database (Denmark)

    Bertheussen, Erlend; Scott, Søren Bertelsen; Hogg, Thomas

    2018-01-01

    Almost all-successful CO2 and CO reduction catalysts to higher chain carbons are based on copper1, however various facets and pre-treatments of copper have shown to give a wide variety of product selectivity.2,3 Currently there are many unanswered questions regarding active sites and mechanisms t...

  12. CVD diamond coatings on titanium : Characterisation by XRD techniques

    Energy Technology Data Exchange (ETDEWEB)

    Cappuccio, G [CNR, Frascati, Rome (Italy). Istituto di Strutturistica Chimica; [INFN-LNF, Frascati, Rome (Italy). Laboratorio Dafne Luce

    1996-09-01

    Here, the authors report an analysis carried out on diamond coatings on titanium substrates to show the potentially of x-ray diffraction techniques in the structural characterisation both of diamond thin films and of the other phases (TiC and TiH{sub 2}) present in the interfacial layer. It should be noted that the composition and microstructure of the interface layers strongly affect the characteristics of the diamond films, particularly adhesion, which is one of the most important elements determining the final quality of the coating.

  13. RBS and XRD analysis of silicon doped titanium diboride films

    International Nuclear Information System (INIS)

    Mollica, S.; Sood, D.K.; Ghantasala, M.K.; Kothari, R.

    1999-01-01

    Titanium diboride is a newly developed material suitable for protective coatings. Its high temperature oxidation resistance at temperatures of 700 deg C and beyond is limited due to its poor oxidative behaviour. This paper presents a novel approach to improving the coatings' oxidative characteristics at temperatures of 700 deg C by doping with silicon. Titanium diboride films were deposited onto Si(100) wafer substrates using a DC magnetron sputtering system. Films were deposited in two different compositions, one at pure TiB 2 and the other with 20 % Si doping. These samples were vacuum annealed at 700 deg C at 1x10 -6 Torr to investigate the anaerobic behaviour of the material at elevated temperatures and to ensure that they were crystalline. Samples were then oxidised in air at 700 deg C to investigate their oxidation resistance. Annealing the films at 700 deg C in air results in the oxidation of the film as titanium and boron form TiO 2 and B 2 O 3 . Annealing is seen to produce only minor changes in the films. There is some silicon diffusion from the substrate at elevated temperatures, which is related to the porous nature of the deposited film and the high temperature heat treatments. However, silicon doped films showed relatively less oxidation characteristics after annealing in air compared with the pure TiB 2 samples

  14. stainless steel by SEM-XRD and image analysis

    Directory of Open Access Journals (Sweden)

    Robinson Constanzo-R.

    2014-01-01

    Full Text Available El objetivo de este trabajo fue realizar un análisis cualitativ o de la distribución de un electrodepósito de cobre en el inter ior de electrodos porosos (EP de acero inoxidable y carbono grafito. Para ello, se reali zaron pruebas de electrodepositación de cobre a nivel de labora torio, con un posterior análisis de cortes de muestras de acero y grafito vía Microscopía Estereoscópica, Microscopía SEM-DRX y Análisis de Imagen, los cuales mostraron que el cobre no se deposita en forma uniforme al interior del electrodo. En el electrodo de acero, la penetra ción del depósito en el espesor fue alrededor de 50%, mientras que para el grafito a lrededor de 90%. En forma general, se observó un aumento de la cantidad de depósito hacia el extremo frente al ánodo y con sitios de difer ente crecimiento en depósito de cobre. Esto demuestra una distr ibución de corriente y potencial, función de parámetros físicos de electrodo y de la s características fisicoquímicas e hidrodinámicos del electroli to.

  15. Ball milling of chalcopyrite: Moessbauer spectroscopy and XRD studies

    International Nuclear Information System (INIS)

    Pollak, H.; Fernandes, M.; Levendis, D.; Schonig, L.

    1999-01-01

    The aim of this project is to study the behavior of chalcopyrite under ball milling for extended periods in order to determine how it's decompose or transform. Tests were done with chalcopyrite mixed with iron and zinc with and without surfactant. The use of surfactants has various effects such as avoiding oxidation and clustering of the fine particles. In all case magnetic chalcopyrite is transformed into a paramagnetic component showing a disordered structure, thus revealing that Cu atoms have replaced Fe atoms. In the case of ball milling in air, chalcopyrite is decomposed with the lost of iron, while in milling under surfactants, iron enters into the chalcopyrite structure. (author)

  16. Infrared spectra, Raman laser, XRD, DSC/TGA and SEM ...

    Indian Academy of Sciences (India)

    Ga2O3, Se metal, SnO, Sb2O3, HgO and PbCO3 are formed upon the reaction of acetamide aqueous solutions with Ga(NO3)3, SeO2, SnCl2, SbCl3, HgCl2 and Pb(NO3)2, respectively, at 90°C. Different amorphous or crystalline phases can be obtained depending upon the experimental conditions (molar ratios, metal salts ...

  17. Powder XRD studies on n-C28H58

    Indian Academy of Sciences (India)

    Unknown

    d-values of C28 alkane in βm and βo phases were computer generated through an ... identification of phase, to which a given peak belonged. The areas enveloped ... ced orientational preferences, thus promoting (i) lamellar formations and (ii) ...

  18. Diagnostics for pellet experiments

    International Nuclear Information System (INIS)

    Johnson, R.R.

    1978-01-01

    The target diagnostics which are being used and planned in current laser driven ICF Experiments are described. Most of these diagnostics can be easily applied to future ion-beam fusion experiments. The status of laser fusion diagnostics has been much improved in the last 5 years and further improvements can be expected and should be available when the first ICF experiments using ion beams are performed. As an example, x-ray temporal and spatial resolutions are now approximately 5 psec and 3 μm, which is approximately a factor of 4 better than the resolution reported in the first implosion experiments. As one plans ahead for ion-beam fusion experiments it should be emphasized that high yield experiments are easier to diagnose provided adequate shielding is employed. However, in the event that the first high yield experiments fail it will be necessary to have diagnostics available to determine where the problems lie. In laser fusion it is interesting to note that higher laser powers are required now for breakeven experiments than first anticipated, mainly because some aspects of the laser-interaction physics were not recognized until the experiments were carefully diagnosed. Thus as has been pointed out, it may be necessary to increase the energy of the ion-beam driver to enable us to do breakeven experiments with high confidence

  19. Popper's Thought Experiment Reinvestigated

    Science.gov (United States)

    Richardson, Chris; Dowling, Jonathan

    2012-02-01

    Karl Popper posed an interesting thought experiment in 1934. With it, he meant to question the completeness of quantum mechanics. He claimed that the notion of quantum entanglement leads to absurd scenarios that cannot be true in real life and that an implementation of his thought experiment would not give the results that QM predicts. Unfortunately for Popper, it has taken until recently to perform experiments that test his claims. The results of the experiments do not refute QM as Popper predicted, but neither do they confirm what Popper claimed QM predicted. Kim and Shih implemented Popper's thought experiment in the lab. The results of the experiment are not clear and have instigated many interpretations of the results. The results show some correlation between entangled photons, but not in the way that Popper thought, nor in the way a simple application of QM might predict. A ghost-imaging experiment by Strekalov, et al. sheds light on the physics behind Popper's thought experiment, but does not try to directly test it. I will build the physics of Popper's thought experiment from the ground up and show how the results of both of these experiments agree with each other and the theory of QM, but disprove Popper.

  20. A.C. impedance, XRD, DSC, SEM and charge/discharge studies on Al2O3, TiO2, SiO2 dispersoid LiPF6/PVC/PVdF-co-HFP composite polymer electrolytes by phase inversion

    Science.gov (United States)

    Vickraman, P.; Gopukumar, S.

    2017-07-01

    The PVC/PVdF-co-HFP composite polymer electrolyte membranes (CPEMs) by varying blend ratios 1:1, 1:2, and 2:1 with fixed content of Al2O3, TiO2 and SiO2 having soaked in 0.5 M LiPF6 in EC/DEC (1:1) v/v) have been prepared by phase inversion. CPEMs of higher ionic conductivity (not dependent on electrolyte uptake as observed in our study) ASA4 (3.61×10-4 Scm-1), TSA3 (1.53×10-4 Scm-1), and SSA3 (4.81×10-4 Scm-1) have been only chosen for XRD, DSC, SEM and electrochemical studies. In XRD, crystalline peaks (phases) of PVdF have been noted with/without change in intensity as well as FWHM which correspond to type of filler interaction with host matrix. In DSC, it is observed that shifts in baseline, melting endotherms, and area under the endotherms indicating the thermal hist ory of PVC (Tg = 82 ° C) and melting of VdF crystallites varied with nature of the filler dispersoid. In SEM, the coagulated fibrils of the polymer coiled with the sponge like structure has been mapped. The charge/discharge studies are carried out on these CPEMs at C/10 rate in the voltage range 2.8 V - 4.2 V, and it is noted that the TSA3 showed better cycling performance with good capacity retention i.e., 50 cycles with 66% capacity retention than ASA4 of 28 cycles with 65% and SSA3 of 5 cycles with 56%. In the present study Coulombic efficiency is concerned only for first cycle and it is noted that the TSA3 showed 71% than 66% and 62% respectively for SSA3 and ASA4.