WorldWideScience

Sample records for situ neutron diffraction

  1. In-situ neutron diffraction during biaxial deformation

    International Nuclear Information System (INIS)

    Van Petegem, S.; Wagner, J.; Panzner, T.; Upadhyay, M.V.; Trang, T.T.T.; Van Swygenhoven, H.

    2016-01-01

    A change in strain path may have a significant effect on the mechanical response of metals. In order to understand or even predict the macroscopic behaviour under such conditions a detailed knowledge on the microstructural evolution is crucial. Yet relatively little work has been done to quantify and understand how the inter- and intragranular strains are affected during a change in strain path. In this work we present a new multiaxial deformation rig that allows performing in situ proportional and non-proportional loading under neutron diffraction. We demonstrate the capabilities of this new setup for the case of a 316 L stainless steel. We show that the nature and magnitude of intergranular strain strongly depends on the applied stress state and demonstrate that micro yielding and internal strain recovery are responsible for the observed transient softening during a 90° strain path change. We anticipate that this new characterization method will provide previously inaccessible microstructural data that can serve as input for benchmarking current state-of-the-art crystal plasticity models.

  2. Steel research using neutron beam techniques. In-situ neutron diffraction, small-angle neutron scattering and residual stress analysis

    International Nuclear Information System (INIS)

    Sueyoshi, Hitoshi; Ishikawa, Nobuyuki; Yamada, Katsumi; Sato, Kaoru; Nakagaito, Tatsuya; Matsuda, Hiroshi; Arakaki, Yu; Tomota, Yo

    2014-01-01

    Recently, the neutron beam techniques have been applied for steel researches and industrial applications. In particular, the neutron diffraction is a powerful non-destructive method that can analyze phase transformation and residual stress inside the steel. The small-angle neutron scattering is also an effective method for the quantitative evaluation of microstructures inside the steel. In this study, in-situ neutron diffraction measurements during tensile test and heat treatment were conducted in order to investigate the deformation and transformation behaviors of TRIP steels. The small-angle neutron scattering measurements of TRIP steels were also conducted. Then, the neutron diffraction analysis was conducted on the high strength steel weld joint in order to investigate the effect of the residual stress distribution on the weld cracking. (author)

  3. Novel Experimental Setups for In Situ Neutron Diffraction

    DEFF Research Database (Denmark)

    Ahlburg, Jakob; H. Gjørup, Frederik; Mørch, Mathias

    Modern synchrotron and neutron sources provide the intensities needed for performing never-before-seen experiments. With the imminent launch of the scattering facilities MAX IV & ESS, it is interesting to explore novel setups that enable new experiments at these sites. X-ray and neutron technique...... also provide information on the magnetic structure and can probe large bulk samples, allowing the study of compacted powders for use in permanent magnets....

  4. In situ high-pressure measurement of crystal solubility by using neutron diffraction

    Science.gov (United States)

    Chen, Ji; Hu, Qiwei; Fang, Leiming; He, Duanwei; Chen, Xiping; Xie, Lei; Chen, Bo; Li, Xin; Ni, Xiaolin; Fan, Cong; Liang, Akun

    2018-05-01

    Crystal solubility is one of the most important thermo-physical properties and plays a key role in industrial applications, fundamental science, and geoscientific research. However, high-pressure in situ measurements of crystal solubility remain very challenging. Here, we present a method involving high-pressure neutron diffraction for making high-precision in situ measurements of crystal solubility as a function of pressure over a wide range of pressures. For these experiments, we designed a piston-cylinder cell with a large chamber volume for high-pressure neutron diffraction. The solution pressures are continuously monitored in situ based on the equation of state of the sample crystal. The solubility at a high pressure can be obtained by applying a Rietveld quantitative multiphase analysis. To evaluate the proposed method, we measured the high-pressure solubility of NaCl in water up to 610 MPa. At a low pressure, the results are consistent with the previous results measured ex situ. At a higher pressure, more reliable data could be provided by using an in situ high-pressure neutron diffraction method.

  5. In-situ neutron diffraction during biaxial deformation

    OpenAIRE

    Van Petegem, S.; Wagner, J.; Panzner, T.; Upadhyay, M.V.; Trang, T.T.T.; Van Swygenhoven, H.

    2016-01-01

    A change in strain path may have a significant effect on the mechanical response of metals. In order to understand or even predict the macroscopic behaviour under such conditions a detailed knowledge on the microstructural evolution is crucial. Yet relatively little work has been done to quantify and understand how the inter- and intragranular strains are affected during a change in strain path. In this work we present a new multiaxial deformation rig that allows performing in situ proportion...

  6. Deformation processes in functional materials studied by in situ neutron diffraction and ultrasonic techniques

    International Nuclear Information System (INIS)

    Sittner, P.; Novak, V.; Landa, M.; Lukas, P.

    2007-01-01

    The unique thermomechanical functions of shape memory alloys (hysteretic stress-strain-temperature responses) not their structural properties (as strength, fatigue, corrosion resistance, etc.) are primarily utilized in engineering applications. In order to better understand and predict the functional behavior, we have recently employed two dedicated non-invasive in situ experimental methods capable to follow the deformation/transformation processes in thermomechanically loaded polycrystalline samples. The in situ neutron diffraction method takes advantage of the ability of thermal neutrons to penetrate bulk samples. As a diffraction technique sensitive to interplanar spacings in crystalline solids, it provides in situ information on the changes in crystal structure, phase composition, phase stress and texture in the transforming samples. The combined in situ ultrasonic and electric resistance method follows variations of the electric resistance as well as speed and attenuation of acoustic waves propagating through the transforming sample. The acoustic waves are mainly sensitive to changes of elastic properties accompanying the deformation/transformation processes. The latter method thus follows the changes in interatomic bonds rather than changes in the interplanar lattice spacings focused in the neutron diffraction method. The methods are thus complementary. They are briefly described and selected experimental results obtained recently on NiTi alloys are presented and discussed

  7. A flow-through hydrothermal cell for in situ neutron diffraction studies of phase transformations

    International Nuclear Information System (INIS)

    O'Neill, Brian; Tenailleau, Christophe; Nogthai, Yung; Studer, Andrew; Brugger, Joel; Pring, Allan

    2006-01-01

    A flow-through hydrothermal cell for the in situ neutron diffraction study of crystallisation and phase transitions has been developed. It can be used for kinetic studies on materials that exhibit structural transformations under hydrothermal conditions. It is specifically designed for use on the medium-resolution powder diffractometer (MRPD) at ANSTO, Lucas Heights, Sydney. But it is planned to adapt the design for the Polaris beamline at ISIS and the new high-intensity powder diffractometer (Wombat) at the new Australian reactor Opal. The cell will operate in a flow-through mode over the temperature range from 25-300 deg. C and up to pressures of 100 bar. The first results of a successful transformation of pentlandite (Fe,Ni) 9 S 8 to violarite (Fe,Ni) 3 S 4 under mild conditions (pH∼4) at 120 deg. C and 3 bar using in situ neutron diffraction measurements are presented

  8. Thermodynamic modelling and in-situ neutron diffraction investigation of the (Ce + Mg + Zn) system

    International Nuclear Information System (INIS)

    Zhu, Zhijun; Gharghouri, Michael A.; Medraj, Mamoun; Lee, Soo Yeol; Pelton, Arthur D.

    2016-01-01

    Highlights: • All phase diagram and thermodynamic data critically assessed for the (Ce + Mg + Zn) system. • All phases described by optimized thermodynamic models. • In-situ neutron diffraction performed to identify phases and transition temperatures. • Assessments of other (RE + Mg + Zn) systems have been carried out simultaneously. • The final product is a thermodynamic database for multicomponent (Mg + RE + Zn) systems. - Abstract: All available phase diagram data for the (Ce + Mg + Zn) system were critically assessed. In-situ neutron diffraction (ND) experiments were performed on selected samples to identify phases and transition temperatures. A critical thermodynamic evaluation and optimization of the (Ce + Mg + Zn) system were carried out and model parameters for the thermodynamic properties of all phases were obtained. The phase transformation behaviour of selected samples was well resolved from the ND experiments and experimental data were used to refine the thermodynamic model parameters.

  9. Design of a new lithium ion battery test cell for in-situ neutron diffraction measurements

    Czech Academy of Sciences Publication Activity Database

    Roberts, M.; Biendicho, J. J.; Hull, S.; Beran, Přemysl; Gustafsson, T.; Svensson, G.; Edstrom, K.

    2013-01-01

    Roč. 226, MAR 15 (2013), s. 249-255 ISSN 0378-7753 R&D Projects: GA MŠk(XE) LM2011019 Institutional support: RVO:61389005 Keywords : neutron * Lithium * LiFePO4 * diffraction * in situ Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 5.211, year: 2013 http://www.sciencedirect.com/science/article/pii/S0378775312016515

  10. Final Technical Report: Application of in situ Neutron Diffraction to Understand the Mechanism of Phase Transitions

    Energy Technology Data Exchange (ETDEWEB)

    Chandran, Ravi [Univ. of Utah, Salt Lake City, UT (United States). Dept. of Metallurgical Engineering

    2018-02-09

    In this research, phase transitions in the bulk electrodes for Li-ion batteries were investigated using neutron diffraction (ND) as well as neutron imaging techniques. The objectives of this research is to design of a novel in situ electrochemical cell to obtain Rietveld refinable neutron diffraction experiments using small volume electrodes of various laboratory/research-scale electrodes intended for Li-ion batteries. This cell is also to be used to investigate the complexity of phase transitions in Li(Mg) alloy electrodes, either by diffraction or by neutron imaging, which occur under electrochemical lithiation and delithiation, and to determine aspects of phase transition that enable/limit energy storage capacity. Additional objective is to investigate the phase transitions in electrodes made of etched micro-columns of silicon and investigate the effect of particle/column size on phase transitions and nonequilibrium structures. An in situ electrochemical cell was designed successfully and was used to study the phase transitions under in-situ neutron diffraction in both the electrodes (anode/cathode) simultaneously in graphite/LiCoO2 and in graphite/LiMn2O4 cells each with two cells. The diffraction patterns fully validated the working of the in situ cell. Additional experimental were performed using the Si micro-columnar electrodes. The results revealed new lithiation phenomena, as evidenced by mosaicity formation in silicon electrode. These experiments were performed in Vulcan diffractometer at SNS, Oak Ridge National Laboratory. In parallel, the spatial distribution of Li during lithiation and delithiation processes in Li-battery electrodes were investigated. For this purpose, neutron tomographic imaging technique has been used for 3D mapping of Li distribution in bulk Li(Mg) alloy electrodes. It was possible to observe the phase boundary of Li(Mg) alloy indicating phase transition from Li-rich BCC β-phase to Li-lean

  11. In-situ neutron diffraction measurements of temperature and stresses during friction stir welding of 6061-T6 aluminum alloy

    International Nuclear Information System (INIS)

    Woo, Wan Chuck; Feng, Zhili; Wang, Xun-Li; Brown, D.W.; Clausen, B.; An, Ke; Choo, Hahn; Hubbard, Camden R.; David, Stan A.

    2007-01-01

    The evolution of temperature and thermal stresses during friction stir welding of Al6061-T6 was investigated by means of in-situ, time-resolved neutron diffraction technique. A method is developed to deconvolute the temperature and stress from the lattice spacing changes measured by neutron diffraction. The deep penetration capability of neutrons made it possible for the first time to obtain the temperature and thermal stresses inside a friction stir weld

  12. In-situ neutron diffraction characterization of temperature dependence deformation in α-uranium

    Science.gov (United States)

    Calhoun, C. A.; Garlea, E.; Sisneros, T. A.; Agnew, S. R.

    2018-04-01

    In-situ strain neutron diffraction measurements were conducted at temperature on specimens coming from a clock-rolled α-uranium plate, and Elasto-Plastic Self-Consistent (EPSC) modeling was employed to interpret the findings. The modeling revealed that the active slip systems exhibit a thermally activated response, while deformation twinning remains athermal over the temperature ranges explored (25-150 °C). The modeling also allowed assessment of the effects of thermal residual stresses on the mechanical response during compression. These results are consistent with those from a prior study of room-temperature deformation, indicating that the thermal residual stresses strongly influence the internal strain evolution of grain families, as monitored with neutron diffraction, even though accounting for these residual stresses has little effect on the macroscopic flow curve, except in the elasto-plastic transition.

  13. In situ observation and neutron diffraction of NiTi powder sintering

    International Nuclear Information System (INIS)

    Chen, Gang; Liss, Klaus-Dieter; Cao, Peng

    2014-01-01

    This study investigated NiTi powder sintering behaviour from elemental powder mixtures of Ni/Ti and Ni/TiH 2 using in situ neutron diffraction and in situ scanning electron microscopy. The sintered porous alloys have open porosities ranging from 2.7% to 36.0%. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH 2 compact leads to less densification yet higher chemical homogenization only after high-temperature sintering. For the first time, direct evidence of the eutectoid phase transformation of NiTi at 620 °C is reported by in situ neutron diffraction. A comparative study of cyclic stress–strain behaviours of the porous NiTi alloys made from Ni/Ti and Ni/TiH 2 compacts indicate that the samples sintered from the Ni/TiH 2 compact exhibited a much higher porosity, larger pore size, lower fracture strength, lower close-to-overall porosity ratio and lower Young’s modulus. Instead of enhanced densification by the use of TiH 2 as reported in the literature, this study shows an adverse effect of TiH 2 on powder densification in NiTi

  14. Assessment of Shape Memory Alloys - From Atoms To Actuators - Via In Situ Neutron Diffraction

    Science.gov (United States)

    Benafan, Othmane

    2014-01-01

    As shape memory alloys (SMAs) become an established actuator technology, it is important to identify the fundamental mechanisms responsible for their performance by understanding microstructure performance relationships from processing to final form. Yet, microstructural examination of SMAs at stress and temperature is often a challenge since structural changes occur with stress and temperature and microstructures cannot be preserved through quenching or after stress removal, as would be the case for conventional materials. One solution to this dilemma is in situ neutron diffraction, which has been applied to the investigation of SMAs and has offered a unique approach to reveal the fundamental micromechanics and microstructural aspects of bulk SMAs in a non-destructive setting. Through this technique, it is possible to directly correlate the micromechanical responses (e.g., internal residual stresses, lattice strains), microstructural evolutions (e.g., texture, defects) and phase transformation properties (e.g., phase fractions, kinetics) to the macroscopic actuator behavior. In this work, in situ neutron diffraction was systematically employed to evaluate the deformation and transformation behavior of SMAs under typical actuator conditions. Austenite and martensite phases, yield behavior, variant selection and transformation temperatures were characterized for a polycrystalline NiTi (49.9 at. Ni). As the alloy transforms under thermomechanical loading, the measured textures and lattice plane-level variations were directly related to the cyclic actuation-strain characteristics and the dimensional instability (strain ratcheting) commonly observed in this alloy. The effect of training on the shape memory characteristics of the alloy and the development of two-way shape memory effect (TWSME) were also assessed. The final conversion from a material to a useful actuator, typically termed shape setting, was also investigated in situ during constrained heatingcooling and

  15. In-situ neutron diffraction study of Zircaloy 4 subjected to biaxial tension

    Energy Technology Data Exchange (ETDEWEB)

    Gharghouri, M.A. [Canadian Neutron Beam Centre, Chalk River Laboratories, Chalk River, ON (Canada); McDonald, D.; Xiao, L. [Atomic Energy of Canada Limited, Chalk River, ON (Canada)

    2014-07-01

    Zircaloy-4 is widely used as fuel element cladding in nuclear reactors. Pellet-clad interaction (PCI) failure is a concern for many water reactor fuel designs. Extensive work on the mechanism of PCI failure has led to the conclusion that stress corrosion cracking (SCC) induced by iodine vapour in the temperature range relevant to fuel operation is the most probable cause of PCI failure in zirconium alloy fuel element cladding. In-situ neutron diffraction measurements performed on tubular Zircaloy-4 specimens simultaneously pulled in tension and pressurized internally will provide information on the effects of stress biaxiality on the distribution of stresses at the crystal level during loading. (author)

  16. An in situ thermo-mechanical rig for lattice strain measurement during creep using neutron diffraction

    Science.gov (United States)

    Wang, Y. Q.; Kabra, S.; Zhang, S. Y.; Truman, C. E.; Smith, D. J.

    2018-05-01

    A long-term high-temperature testing stress rig has been designed and fabricated for performing in situ neutron diffraction tests at the ENGIN-X beamline, ISIS facility in the UK. It is capable of subjecting metals to high temperatures up to 800 °C and uniaxial loading under different boundary conditions including constant load, constant strain, and elastic follow-up, each with minimum of external control. Samples are held horizontally between grips and connected to a rigid rig frame, a soft aluminium bar, and a stepper motor with forces up to 20 kN. A new three zone split electrical resistance furnace which generates a stable and uniform heat atmosphere over 200 mm length was used to heat the samples. An 8 mm diameter port at 45° to the centre of the furnace was made in order to allow the neutron beam through the furnace to illuminate the sample. The entire instrument is mounted on the positioner at ENGIN-X and has the potential ability to operate continuously while being moved in and out of the neutron diffraction beam. The performance of the rig has been demonstrated by tracking the evolution of lattice strains in type 316H stainless steel under elastic follow-up control at 550 °C.

  17. In situ X-ray and neutron diffraction study of Ba2In2O5

    International Nuclear Information System (INIS)

    Speakman, S.A.; Misture, S.T.

    2001-01-01

    Order-disorder transitions in barium indate, Ba 2 In 2 O 5 , have been studied using in-situ X-ray and neutron diffraction. At room temperature, the crystal structure is an orthorhombic brownmillerite structure. At 706 C, the crystal structure is orthorhombic, possibly of the Imma or Ibm2 space groups. At 900 C, oxygen vacancies begin to disorder. The order-disorder transition occurs slowly in two steps over a temperature range of 900 - 925 C. Above this temperature range, the crystal structure is tetragonal, most likely belonging to the space group I 4/mcm. A second order-disorder transition begins at 1040 C, and proceeds over the temperature range 1040 - 1065 C. Above this temperature range, the crystal structure is a cubic, oxygen-deficient perovskite structure, with space group Pm3m. At an undetermined temperature above 1200 C, Ba 2 In 2 O 5 begins to decompose. (orig.)

  18. Effect of external stress on deuteride (hydride) precipitation in Zircaloy-4 using in situ neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Jun-li [Department of Nuclear, Plasma, and Radiological Engineering, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); An, Ke; Stoica, Alexandru D. [Chemical and Engineering Materials Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Heuser, Brent J., E-mail: bheuser@illinois.edu [Department of Nuclear, Plasma, and Radiological Engineering, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States)

    2017-04-15

    In situ neutron diffraction is utilized to study the deuteride (hydride) precipitation behavior in a cold-worked stress-relieved (CWSR) Zircaloy-4 material upon cooling from 420 °C to room temperature with a 78 MPa external stress applied along the rolling direction (RD) of the material. Two banks detector capture the diffraction signal from two principal directions of the specimen, the normal direction (ND) and the rolling direction (RD). The evolution of deuterium concentration in zirconium solid solution along the two specimen directions is measured by studying the δ-(220) peak intensity, applying the Rietveld refinement method to the diffraction data and using the measured zirconium c-axis lattice distortion. The deuterium concentration is observed to be higher for zirconium grains in the ND than the RD. The terminal solid solubility of precipitation (TSSp) for deuterium in the solution is then described using the Arrhenius equation. It is observed that the applied stress reduces the energy term Q in the Arrhenius equation when compared with the unstressed Q values from the work of others. A model by Puls is applied to study the effect of stress on deuterium solubility, with polycrystalline hydride precipitation strain calculated using the Kearns factor representative of the studied material. The experimental result does not agree with the model prediction of Puls.

  19. In situ neutron diffraction investigation on the phase transformation sequence of kaolinite and halloysite to mullite

    Energy Technology Data Exchange (ETDEWEB)

    Tezuka, Nobuo [Department of Applied Physics, Curtin University of Technology, GPO Box U1987, Perth, WA 6845 (Australia); Low, It-Meng [Department of Applied Physics, Curtin University of Technology, GPO Box U1987, Perth, WA 6845 (Australia)]. E-mail: J.Low@curtin.edu.au; Davies, Ian J. [Department of Mechanical Engineering, Curtin University of Technology, GPO Box U1987, Perth, WA 6845 (Australia); Prior, Michael [Bragg Institute, ANSTO, PMB 1, Menai, NSW 2234 (Australia); Studer, Andrew [Bragg Institute, ANSTO, PMB 1, Menai, NSW 2234 (Australia)

    2006-11-15

    'Kaolin' is a major raw material for the fabrication of conventional ceramics. In this work the authors have investigated the thermal phase transformation of mullite from two different types of kaolin (kaolinite and halloysite), with or without alumina matrix constraint, during heating up to 1500 deg. C and then cooling using in situ neutron diffraction. Mullitization was initiated upon heating to 1200 deg. C for all specimens and followed spinel formation at 1100 deg. C. Above this temperature, however, evolution of the main phases, i.e., mullite, cristobalite and corundum, was influenced by the presence of impurities, initial type of silica, and alumina constraint. The relative amount of mullite was largest for the pure kaolinite specimen, particularly during heating, and this was attributed to the presence of a glassy phase. However, kaolinite with alumina suppressed the crystallization of cristobalite from the glassy phase upon cooling due to a reaction between alumina and amorphous silica, consequently resulting in an amount of mullite as for the pure kaolinite specimen (approximately 65 wt%). Halloysite was less active in terms of mullitization due to the lower level of initial impurities and greater amount of cristobalite, particularly for the alumina-constrained specimen. However, the final amount of mullite derived from the pure halloysite specimen was similar to that as from the kaolinite specimen.

  20. In situ neutron diffraction investigation on the phase transformation sequence of kaolinite and halloysite to mullite

    International Nuclear Information System (INIS)

    Tezuka, Nobuo; Low, It-Meng; Davies, Ian J.; Prior, Michael; Studer, Andrew

    2006-01-01

    'Kaolin' is a major raw material for the fabrication of conventional ceramics. In this work the authors have investigated the thermal phase transformation of mullite from two different types of kaolin (kaolinite and halloysite), with or without alumina matrix constraint, during heating up to 1500 deg. C and then cooling using in situ neutron diffraction. Mullitization was initiated upon heating to 1200 deg. C for all specimens and followed spinel formation at 1100 deg. C. Above this temperature, however, evolution of the main phases, i.e., mullite, cristobalite and corundum, was influenced by the presence of impurities, initial type of silica, and alumina constraint. The relative amount of mullite was largest for the pure kaolinite specimen, particularly during heating, and this was attributed to the presence of a glassy phase. However, kaolinite with alumina suppressed the crystallization of cristobalite from the glassy phase upon cooling due to a reaction between alumina and amorphous silica, consequently resulting in an amount of mullite as for the pure kaolinite specimen (approximately 65 wt%). Halloysite was less active in terms of mullitization due to the lower level of initial impurities and greater amount of cristobalite, particularly for the alumina-constrained specimen. However, the final amount of mullite derived from the pure halloysite specimen was similar to that as from the kaolinite specimen

  1. In situ neutron diffraction studies of high density amorphous ice under pressure

    International Nuclear Information System (INIS)

    Klotz, Stefan; Straessle, Th; Saitta, A M; Rousse, G; Hamel, G; Nelmes, R J; Loveday, J S; Guthrie, M

    2005-01-01

    We review recent in situ neutron diffraction studies on the structural pressure dependence and the recrystallization of dense amorphous ices up to 2 GPa. Progress in high pressure techniques and data analysis methods allows the reliable determination of all three partial structure factors of amorphous ice under pressure. The strong pressure dependence of the g OO (r) correlation function shows that the isothermal compression of high density amorphous ice (HDA) at 100 K is achieved by a contraction (∼ 20%) of the second-neighbour coordination shell leading to a strong increase in coordination. The g DD (r) and g OD (r) structure factors are, in contrast, only weakly sensitive to pressure. These data allow a comparison with structural features of the recently reported 'very high density amorphous ice' (VHDA) which indicates that VHDA at ambient pressure is very similar to compressed HDA, at least up to the second-neighbour shell. The recrystallization of HDA has been investigated in the range 0.3-2 GPa. It is shown that hydrogen-disordered phases are produced which normally grow only from the liquid, such as ice XII, and in particular ice IV. These findings are in good agreement with results on quench-recovered samples

  2. In situ observation of the reaction of scandium and carbon by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Juarez-Arellano, Erick A., E-mail: eajuarez@unpa.edu.m [Institut fuer Geowissenschaften, Universitaet Frankfurt, Altenhoeferallee 1, 60438 Frankfurt a.M. (Germany); Universidad del Papaloapan, Circuito Central 200, Parque Industrial, Tuxtepec 68301 (Mexico); Winkler, Bjorn [Institut fuer Geowissenschaften, Universitaet Frankfurt, Altenhoeferallee 1, 60438 Frankfurt a.M. (Germany); Vogel, Sven C. [Los Alamos National Laboratory, Lujan Center. Mail Stop H805, Los Alamos, NM 87545 (United States); Senyshyn, Anatoliy [Forschungsneutronenquelle Heinz Maier-Leibnitz (FRM II), Technische Universitaet Muenchen, Lichtenbergstr. 1, D-85747 Garching (Germany); Materialwissenschaft, TU Darmstadt, Petersensstr. 23, D-64287 Darmstadt (Germany); Kammler, Daniel R. [Sandia National Laboratories, Albuquerque, NM 87185 (United States); Avalos-Borja, Miguel [CNyN, UNAM, A. Postal 2681, Ensenada, B.C. (Mexico)

    2011-01-05

    Research highlights: {yields} Exist two ScC cubic phases with B1-structure type differing in site occupancy of C. {yields} A new orthorhombic scandium carbide phase is formed at 1473(50) K. {yields} The recrystallization of alpha-Sc occurs between 1000 and 1223 K. - Abstract: The formation of scandium carbides by reaction of the elements has been investigated by in situ neutron diffraction up to 1823 K. On heating, the recrystallization of {alpha}-Sc occurs between 1000 and 1223 K. The formation of Sc{sub 2}C and ScC (NaCl-B1 type structure) phases has been detected at 1323 and 1373 K, respectively. The formation of a new orthorhombic scandium carbide phase was observed at 1473(50) K. Once the scandium carbides are formed they are stable upon heating or cooling. No other phases were detected in the present study, in which the system was always carbon saturated. The thermal expansion coefficients of all phases have been determined, they are constant throughout the temperature interval studied.

  3. In-situ neutron diffraction study on work-hardening behavior in a ferrite-martensite dual phase steel

    OpenAIRE

    Morooka, Satoshi; Sato, Naoko; Ojima, Mayumi; Harjo, Stefanus; Adachi, Yoshitaka; Tomota, Yo; Umezawa, Osamu

    2011-01-01

    Strength and work-hardening in steels have been discussed from the viewpoint of heterogeneous deformation. In-situ neutron diffraction techniques made clear that the misfit strains between grains accompanied with the grain-scaled internal stress (intergranular stress). In the dual phase steel, the intergranular stress was superposed on phase stress. Both long-range internal stress and short-range one like forest dislocation hardening may cause the resistance for dislocation motion in the steels.

  4. An in situ Study of NiTi Powder Sintering Using Neutron Diffraction

    Directory of Open Access Journals (Sweden)

    Gang Chen

    2015-04-01

    Full Text Available This study investigates phase transformation and mechanical properties of porous NiTi alloys using two different powder compacts (i.e., Ni/Ti and Ni/TiH2 by a conventional press-and-sinter means. The compacted powder mixtures were sintered in vacuum at a final temperature of 1373 K. The phase evolution was performed by in situ neutron diffraction upon sintering and cooling. The predominant phase identified in all the produced porous NiTi alloys after being sintered at 1373 K is B2 NiTi phase with the presence of other minor phases. It is found that dehydrogenation of TiH2 significantly affects the sintering behavior and resultant microstructure. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH2 compact leads to less densification, yet higher chemical homogenization, after high temperature sintering but not in the case of low temperature sintering. Moreover, there is a direct evidence of the eutectoid decomposition of NiTi at ca. 847 and 823 K for Ni/Ti and Ni/TiH2, respectively, during furnace cooling. The static and cyclic stress-strain behaviors of the porous NiTi alloys made from the Ni/Ti and Ni/TiH2 compacts were also investigated. As compared with the Ni/Ti sintered samples, the samplessintered from the Ni/TiH2 compact exhibited a much higher porosity, a higher close-to-total porosity, a larger pore size and lower tensile and compressive fracture strength.

  5. A comparison of dilatometry and in-situ neutron diffraction in tracking bulk phase transformations in a martensitic stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Christien, F., E-mail: frederic.christien@univ-nantes.fr [Institut des Matériaux Jean Rouxel (IMN), Université de Nantes, CNRS, Rue Christian Pauc, BP 50609, 44306 Nantes Cedex 3 (France); Telling, M.T.F. [ISIS Facility, Rutherford Appleton Laboratory, Chilton, OX11 0QX (United Kingdom); Department of Materials, University of Oxford, Parks Road, Oxford (United Kingdom); Knight, K.S. [ISIS Facility, Rutherford Appleton Laboratory, Chilton, OX11 0QX (United Kingdom); Department of Earth Sciences, The Natural History Museum, Cromwell Road, London (United Kingdom)

    2013-08-15

    Phase transformations in the 17-4PH martensitic stainless steel have been studied using different in-situ techniques, including dilatometry and high resolution neutron diffraction. Neutron diffraction patterns were quantitatively processed using the Rietveld refinement method, allowing the determination of the temperature-dependence of martensite (α′, bcc) and austenite (γ, fcc) phase fractions and lattice parameters on heating to 1000 °C and then cooling to room temperature. It is demonstrated in this work that dilatometry doesn't permit an accurate determination of the end temperature (Ac3) of the α′ → γ transformation which occurs upon heating to high temperature. The analysis of neutron diffraction data has shown that the respective volumes of the two phases become very close to each other at high temperature, thus making the dilatometric technique almost insensitive in that temperature range. However, there is a very good agreement between neutron diffraction and dilatometry at lower temperature. The martensitic transformation occurring upon cooling has been analysed using the Koistinen–Marburger equation. The thermal expansion coefficients of the two phases have been determined in addition. A comparison of the results obtained in this work with data from literature is presented. - Highlights: • Martensite is still present at very high temperature (> 930 °C) upon heating. • The end of austenitisation cannot be accurately monitored by dilatometry. • The martensite and austenite volumes become similar at high temperature (> ∼ 850 °C)

  6. Dynamic processes of domain switching in lead zirconate titanate under cyclic mechanical loading by in situ neutron diffraction

    International Nuclear Information System (INIS)

    Pojprapai, Soodkhet; Luo, Zhenhua; Clausen, Bjorn; Vogel, Sven C.; Brown, Donald W.; Russel, Jennifer; Hoffman, Mark

    2010-01-01

    The performance of ferroelectric ceramics is governed by the ability of domains to switch. A decrease in the switching ability can lead to degradation of the materials and failure of ferroelectric devices. In this work the dynamic properties of domain reorientation are studied. In situ time-of-flight neutron diffraction is used to probe the evolution of ferroelastic domain texture under mechanical cyclic loading in bulk lead zirconate titanate ceramics. The high sensitivity of neutron diffraction to lattice strain is exploited to precisely analyze the change of domain texture and strain through a full-pattern Rietveld method. These results are then used to construct a viscoelastic model, which explains the correlation between macroscopic phenomena (i.e. creep and recovered deformation) and microscopic dynamic behavior (i.e. ferroelastic switching, lattice strain).

  7. In situ neutron diffraction and Elastic–Plastic Self-Consistent polycrystal modeling of HT-9

    International Nuclear Information System (INIS)

    Clausen, B.; Brown, D.W.; Bourke, M.A.M.; Saleh, T.A.; Maloy, S.A.

    2012-01-01

    Qualifying materials for use in reactors with fluences greater than 200 dpa (displacements per atom) requires development of advanced alloys and irradiations in fast reactors to test these alloys. Research into the mechanical behavior of these materials under reactor conditions is ongoing. In order to probe changes in deformation mechanisms due to radiation in these materials, samples of HT-9 were tested in tension in situ on the SMARTS instrument at Los Alamos Neutron Science Center. Experimental results, confirmed with modeling, show significant load sharing between the carbides and parent phase of the steel beyond yield, displaying the critical role of carbides during deformation, along with basic texture development.

  8. In situ neutron diffraction and Elastic-Plastic Self-Consistent polycrystal modeling of HT-9

    Energy Technology Data Exchange (ETDEWEB)

    Clausen, B., E-mail: clausen@lanl.gov [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Brown, D.W.; Bourke, M.A.M.; Saleh, T.A.; Maloy, S.A. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

    2012-06-15

    Qualifying materials for use in reactors with fluences greater than 200 dpa (displacements per atom) requires development of advanced alloys and irradiations in fast reactors to test these alloys. Research into the mechanical behavior of these materials under reactor conditions is ongoing. In order to probe changes in deformation mechanisms due to radiation in these materials, samples of HT-9 were tested in tension in situ on the SMARTS instrument at Los Alamos Neutron Science Center. Experimental results, confirmed with modeling, show significant load sharing between the carbides and parent phase of the steel beyond yield, displaying the critical role of carbides during deformation, along with basic texture development.

  9. In situ shape and distance measurements in neutron scattering and diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Fujiwara, Satoru; Mendelson, R.A. [Univ. of California, San Francisco, CA (United States)

    1994-12-31

    Neutron scattering combined with selective isotopic labeling and contrast matching is useful for obtaining in situ structural information about a selected particle, or particles, in a macromolecular complex. The observed intensities, however, may be distorted by inter-complex interference and by scattering-length-density fluctuations of the (otherwise) contrast-matched portions. Methods have been proposed to cancel out such distortions (Hoppe`s method, the Statistical Labeling Method, and the Triple Isotopic Substitution Method). With these methods as well as related unmixed-sample methods, structural information about the selected particles can be obtained without these distortions. We have generalized these methods so that, in addition to globular particles in solution, they can be applied to in situ structures of systems having underlying symmetry and/or net orientation as well. The information obtainable from such experiments is discussed.

  10. In situ shape and distance measurements in neutron scattering and diffraction

    International Nuclear Information System (INIS)

    Fujiwara, Satoru; Mendelson, R.A.

    1994-01-01

    Neutron scattering combined with selective isotopic labeling and contrast matching is useful for obtaining in situ structural information about a selected particle, or particles, in a macromolecular complex. The observed intensities, however, may be distorted by inter-complex interference and by scattering-length-density fluctuations of the (otherwise) contrast-matched portions. Methods have been proposed to cancel out such distortions (Hoppe's method, the Statistical Labeling Method, and the Triple Isotopic Substitution Method). With these methods as well as related unmixed-sample methods, structural information about the selected particles can be obtained without these distortions. We have generalized these methods so that, in addition to globular particles in solution, they can be applied to in situ structures of systems having underlying symmetry and/or net orientation as well. The information obtainable from such experiments is discussed

  11. An in situ neutron diffraction study of shape setting shape memory NiTi

    International Nuclear Information System (INIS)

    Benafan, O.; Padula, S.A.; Noebe, R.D.; Brown, D.W.; Clausen, B.; Vaidyanathan, R.

    2013-01-01

    A bulk polycrystalline Ni 49.9 Ti 50.1 (at.%) shape memory alloy specimen was shape set while neutron diffraction spectra were simultaneously acquired. The objective was to correlate internal stress, phase volume fraction, and texture measurements (from neutron diffraction spectra) with the macroscopic stress and shape changes (from load cell and extensometry measurements) during the shape setting procedure and subsequent shape recovery. Experimental results showed the evolution of the martensitic transformation (lattice strains, phase fractions and texture) against external constraints during both heating and cooling. Constrained heating resulted in a build-up of stresses during the martensite to austenite transformation, followed by stress relaxation due to thermal expansion, final conversion of retained martensite, and recovery processes. Constrained cooling also resulted in stress build-up arising from thermal contraction and early formation of martensite, followed by relaxation as the austenite fully transformed to martensite. Comparisons were also made between specimens pre-shape set and post-shape set with and without external constraints. The specimens displayed similar shape memory behavior consistent with the microstructure of the shape set sample, which was mostly unchanged by the shape setting process and similar to that of the as-received material

  12. Determination of Coherency and Rigidity Temperatures in Al-Cu Alloys Using In Situ Neutron Diffraction During Casting

    Science.gov (United States)

    Drezet, Jean-Marie; Mireux, Bastien; Szaraz, Zoltan; Pirling, Thilo

    2014-08-01

    The rigidity temperature of a solidifying alloy is the temperature at which the solid phase is sufficiently coalesced to transmit tensile stress. It is a major input parameter in numerical modeling of solidification processes as it defines the point at which thermally induced deformations start to generate internal stresses in a casting. This temperature has been determined for an Al-13 wt.% Cu alloy using in situ neutron diffraction during casting in a dog-bone-shaped mold. This setup allows the sample to build up internal stress naturally as its contraction is not possible. The cooling on both sides of the mold induces a hot spot at the middle of the sample that is irradiated by neutrons. Diffraction patterns are recorded every 11 s using a large detector, and the very first change of diffraction angles allows for the determination of the rigidity temperature. We measured rigidity temperatures equal to 557°C and 548°C depending on the cooling rate for grain refined Al-13 wt.% Cu alloys. At a high cooling rate, rigidity is reached during the formation of the eutectic phase. In this case, the solid phase is not sufficiently coalesced to sustain tensile load and thus cannot avoid hot tear formation.

  13. In situ Neutron Diffraction during Casting: Determination of Rigidity Point in Grain Refined Al-Cu Alloys.

    Science.gov (United States)

    Drezet, Jean-Marie; Mireux, Bastien; Szaraz, Zoltan; Pirling, Thilo

    2014-02-12

    The rigidity temperature of a solidifying alloy is the temperature at which the solid plus liquid phases are sufficiently coalesced to transmit long range tensile strains and stresses. It determines the point at which thermally induced deformations start to generate internal stresses in a casting. As such, it is a key parameter in numerical modelling of solidification processes and in studying casting defects such as solidification cracking. This temperature has been determined in Al-Cu alloys using in situ neutron diffraction during casting in a dog bone shaped mould. In such a setup, the thermal contraction of the solidifying material is constrained and stresses develop at a hot spot that is irradiated by neutrons. Diffraction peaks are recorded every 11 s using a large detector, and their evolution allows for the determination of the rigidity temperatures. We measured rigidity temperatures equal to 557 °C and 548 °C, depending on cooling rate, for a grain refined Al-13 wt% Cu alloy. At high cooling rate, rigidity is reached during the formation of the eutectic phase and the solid phase is not sufficiently coalesced, i.e. , strong enough, to avoid hot tear formation.

  14. In situ Neutron Diffraction during Casting: Determination of Rigidity Point in Grain Refined Al-Cu Alloys

    Directory of Open Access Journals (Sweden)

    Jean-Marie Drezet

    2014-02-01

    Full Text Available The rigidity temperature of a solidifying alloy is the temperature at which the solid plus liquid phases are sufficiently coalesced to transmit long range tensile strains and stresses. It determines the point at which thermally induced deformations start to generate internal stresses in a casting. As such, it is a key parameter in numerical modelling of solidification processes and in studying casting defects such as solidification cracking. This temperature has been determined in Al-Cu alloys using in situ neutron diffraction during casting in a dog bone shaped mould. In such a setup, the thermal contraction of the solidifying material is constrained and stresses develop at a hot spot that is irradiated by neutrons. Diffraction peaks are recorded every 11 s using a large detector, and their evolution allows for the determination of the rigidity temperatures. We measured rigidity temperatures equal to 557 °C and 548 °C, depending on cooling rate, for a grain refined Al-13 wt% Cu alloy. At high cooling rate, rigidity is reached during the formation of the eutectic phase and the solid phase is not sufficiently coalesced, i.e., strong enough, to avoid hot tear formation.

  15. Work Hardening, Dislocation Structure, and Load Partitioning in Lath Martensite Determined by In Situ Neutron Diffraction Line Profile Analysis

    Science.gov (United States)

    Harjo, Stefanus; Kawasaki, Takuro; Tomota, Yo; Gong, Wu; Aizawa, Kazuya; Tichy, Geza; Shi, Zengmin; Ungár, Tamas

    2017-09-01

    A lath martensite steel containing 0.22 mass pct carbon was analyzed in situ during tensile deformation by high-resolution time-of-flight neutron diffraction to clarify the large work-hardening behavior at the beginning of plastic deformation. The diffraction peaks in plastically deformed states exhibit asymmetries as the reflection of redistributions of the stress and dislocation densities/arrangements in two lath packets: soft packet, where the dislocation glides are favorable, and hard packet, where they are unfavorable. The dislocation density was as high as 1015 m-2 in the as-heat-treated state. During tensile straining, the load and dislocation density became different between the two lath packets. The dislocation character and arrangement varied in the hard packet but hardly changed in the soft packet. In the hard packet, dislocations that were mainly screw-type in the as-heat-treated state became primarily edge-type and rearranged towards a dipole character related to constructing cell walls. The hard packet played an important role in the work hardening in martensite, which could be understood by considering the increase in dislocation density along with the change in dislocation arrangement.

  16. Novel thermosyphon driven hydrothermal flow-through cell for in situ and time resolved neutron diffraction studies

    International Nuclear Information System (INIS)

    Xia, Fang; Qian, Gujie; Etschmann, Barbara; University of Adelaide, South Australia, Australia; University of Adelaide, South Australia, Australia; Studer, Andrew; Olsen, Scott

    2009-01-01

    Full text: A flow-through cell for hydrothermal phase transformation studies by in situ and time-resolved neutron diffraction has been designed and constructed. The cell has a large internal volume of 320 m L and can work at up to 300 degree Centigrade under autogeneous vapour pressures (-85 bar). The fluid flow is driven by thermosyphon which is realized by the proper design of temperature difference around the closed loop[1,2). The main body of the cell is made of stainless steel (316 type), but the sample compartment is constructed from non-scattering Ti/Zr alloy. We have successfully commissioned the cell on Australia's new high intensity powder diffractometer WOMBAT in ANSTO, using a simple transformation reaction from leucite (KAISi 2 O 6 ) to analcime (NaAISi 2 O 6H2O ) and then back from analcime to leucite. The demonstration proved that the cell is an excellent tool for probing hydrothermal phase transformations. By collecting diffraction data every 5 min, it was clearly seen that leucite was progressively transformed to analcime in a NaCI solution, and the produced analcime was progressively transformed back to leucite in a K 2 CO 3 solution.

  17. Methane storage mechanism in the metal-organic framework Cu3(btc)2: An in situ neutron diffraction study

    NARCIS (Netherlands)

    Getzschmann, J.; Senkovska, I.; Wallacher, D.; Tovar, M.; Fairen-Jimenez, D.; Düren, T.; van Baten, J.M.; Krishna, R.; Kaskel, S.

    2010-01-01

    The adsorption of deutero-methane (CD4) in Cu3(btc)2 (HKUST-1) was investigated at 77 K using high-resolution neutron powder diffraction. Rietveld refinement of the neutron data revealed a sequential filling of the rigid framework at distinct preferred adsorption sites, and showed the importance of

  18. In situ neutron diffraction study of grain-orientation-dependent phase transformation in 304L stainless steel at a cryogenic temperature

    International Nuclear Information System (INIS)

    Tao Kaixiang; Wall, James J.; Li, Hongqi; Brown, Donald W.; Vogel, Sven C.; Choo, Hahn

    2006-01-01

    In situ time-of-flight neutron diffraction was performed to investigate the martensitic phase transformation during quasistatic uniaxial compression testing of 304L stainless steel at 300 and 203 K. In situ neutron diffraction enabled the bulk measurement of intensity evolution for various hkl atomic planes during the austenite (fcc) to martensite (hcp and bcc) phase transformation. Based on the neutron diffraction patterns, the martensite phases were observed from the very beginning of the plastic deformation at 203 K. However, at 300 K, no newly formed martensite, except a small amount of preexisting hcp phase, was observed throughout the test. From the changes in the relative intensities of individual hkl atomic planes, the grain-orientation-dependent phase transformation was investigated. The preferred orientation of the newly formed martensite grains was also investigated for the sample deformed at 203 K using neutron diffraction. The results reveal the orientation relationships between the austenite and the newly formed martensites. The fcc grain family diffracting with (200) plane normal parallel to the loading axis is favored for the fcc to bcc transformation and the bcc (200) plane normals are primarily aligned along the loading direction. For the fcc to hcp transformation, the fcc grains with (111) plane normals at an angle in between about 10 deg. and 50 deg. to the loading direction are favored

  19. Optimization of spring exchange coupled ferrites, studied by in situ neutron diffraction

    DEFF Research Database (Denmark)

    Ahlburg, Jakob; Christensen, Mogens; Granados-Miralles, Cecilia

    have a spin it will also be possible to measure a magnetic signal and investigate the exchange-coupling. After the reduction the samples was furthermore investigated using powder x-ray diffraction and VSM (vibrating sample magnetometer). To understand the reaction mechanism, a series of experiments...

  20. Optimization of spring exchange coupled ferrites, studied by in situ neutron diffraction

    DEFF Research Database (Denmark)

    Ahlburg, Jakob; Christensen, Mogens; Granados-Miralles, Cecilia

    Strong permanent magnets with a high energy-product are vital for a great number of electronic devices, these can be found in transformers, loudspeakers, windmills etc. Normally the preferred type of magnets are Rare Earth Metals (REM) containing magnets. REM excels since the magnetic contributio...... with varying temperature (fixed flow) or varying flow (fixed temperature) has been performed. To optimize the exchange-coupling several experiments with fixed temperature and flow, have been performed where the conversion from spinel to metal has been varied....... reduced. These metal oxides are antiferromagnetically ordered an is therefore considered a parasitic phase. However by fine-tuning the reaction temperature and hydrogen flow rate the occurrence of the phase can be minimized. In order to distinguish between Co and Fe Neutrons are chosen. Since neutrons...

  1. In Situ Neutron Diffraction Characterization of Phases in Co-Re-Based Alloys at High Tempeatures

    Czech Academy of Sciences Publication Activity Database

    Strunz, Pavel; Mukherji, D.; Gilles, R.; Gasser, U.; Beran, Přemysl; Farkas, G.; Hofmann, M.; Karge, L.; Rösler, J.

    2015-01-01

    Roč. 128, č. 4 (2015), s. 684-688 ISSN 0587-4246. [ISPMA 13 - 13th INTERNATIONAL SYMPOSIUM ON PHYSICS OF MATERIALS. Praha, 31.08.2014 - 04.09.2014] R&D Projects: GA MŠk LM2011019; GA ČR GB14-36566G EU Projects: European Commission(XE) 283883 - NMI3-II Institutional support: RVO:61389005 Keywords : neutron scattering * gas turbine s * Co-Re based alloys Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.525, year: 2015

  2. High Temperature Deformation Mechanism in Hierarchical and Single Precipitate Strengthened Ferritic Alloys by In Situ Neutron Diffraction Studies.

    Science.gov (United States)

    Song, Gian; Sun, Zhiqian; Li, Lin; Clausen, Bjørn; Zhang, Shu Yan; Gao, Yanfei; Liaw, Peter K

    2017-04-07

    The ferritic Fe-Cr-Ni-Al-Ti alloys strengthened by hierarchical-Ni 2 TiAl/NiAl or single-Ni 2 TiAl precipitates have been developed and received great attentions due to their superior creep resistance, as compared to conventional ferritic steels. Although the significant improvement of the creep resistance is achieved in the hierarchical-precipitate-strengthened ferritic alloy, the in-depth understanding of its high-temperature deformation mechanisms is essential to further optimize the microstructure and mechanical properties, and advance the development of the creep resistant materials. In the present study, in-situ neutron diffraction has been used to investigate the evolution of elastic strain of constitutive phases and their interactions, such as load-transfer/load-relaxation behavior between the precipitate and matrix, during tensile deformation and stress relaxation at 973 K, which provide the key features in understanding the governing deformation mechanisms. Crystal-plasticity finite-element simulations were employed to qualitatively compare the experimental evolution of the elastic strain during tensile deformation at 973 K. It was found that the coherent elastic strain field in the matrix, created by the lattice misfit between the matrix and precipitate phases for the hierarchical-precipitate-strengthened ferritic alloy, is effective in reducing the diffusional relaxation along the interface between the precipitate and matrix phases, which leads to the strong load-transfer capability from the matrix to precipitate.

  3. Phase stability and oxygen non-stoichiometry of SrCo0.8Fe0.2O3-d measured by in-situ neutron diffraction

    NARCIS (Netherlands)

    McIntosh, Steven; McIntosh, S.; Vente, Jaap F.; Haije, Wim G.; Blank, David H.A.; Bouwmeester, Henricus J.M.

    2006-01-01

    The phase stability, oxygen stoichiometry and expansion properties of SrCo0.8Fe0.2O3−δ (SCF) were determined by in situ neutron diffraction between 873 and 1173 K and oxygen partial pressures of 5×10−4 to 1 atm. At a pO2 of 1 atm, SCF adopts a cubic perovskite structure, space group Pm3¯m, across

  4. In situ neutron diffraction studies of martensitic transformations in NiTi polycrystals under tension and compression stress

    Czech Academy of Sciences Publication Activity Database

    Šittner, Petr; Lukáš, Petr; Novák, Václav; Daymond, M. R.; Swallowe, G. M.

    2004-01-01

    Roč. 378, - (2004), s. 97-104 ISSN 0921-5093 Institutional research plan: CEZ:AV0Z1010914 Keywords : martensitic transformation * shape memory alloy * neutron diffraction * NiTi Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.445, year: 2004

  5. Investigation of phase transformations by in-situ neutron diffraction in a Co-Re-based high temperature alloy

    Czech Academy of Sciences Publication Activity Database

    Mukherji, D.; Strunz, Pavel; Gilles, R.; Hofmann, M.; Schmitz, F.; Rösler, J.

    2010-01-01

    Roč. 64, č. 23 (2010), s. 2608-2611 ISSN 0167-577X Institutional research plan: CEZ:AV0Z10480505 Keywords : Superalloy * Carbide * Neutron diffraction Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 2.120, year: 2010

  6. In-situ neutron diffraction study of magnetic field induced reorientation in Ni-Mn-Ga under constant stress

    Czech Academy of Sciences Publication Activity Database

    Molnár, Peter; Šittner, Petr; Novák, Václav; Prokleška, J.; Sechovsky, V.; Ouladdiaf, B.; Hanulla, S.P.; Heczko, O.

    2008-01-01

    Roč. 20, č. 10 (2008), 104224/1-104224/7 ISSN 0953-8984 R&D Projects: GA AV ČR(CZ) IAA200100627 Institutional research plan: CEZ:AV0Z10100520 Keywords : shape memory alloys * NiMnGa * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.900, year: 2008

  7. The use of deuterated ethyl acetate in highly concentrated electrolyte as a low-cost solvent for in situ neutron diffraction measurements of Li-ion battery electrodes

    International Nuclear Information System (INIS)

    Petibon, R.; Li, Jing; Sharma, Neeraj; Pang, Wei Kong; Peterson, Vanessa K.; Dahn, J.R.

    2015-01-01

    A low-cost deuterated electrolyte suitable for in situ neutron diffraction measurements of normal and high voltage Li-ion battery electrodes is reported here. Li[Ni 0.4 Mn 0.4 Co 0.2 ]O 2 /graphite (NMC(442)/graphite) pouch cells filled with 1:0.1:2 (molar ratio) of lithium bis(fluorosulfonyl) imide (LiFSi):LiPF 6 : ethyl acetate (EA) and LiFSi:LiPF 6 :deuterated EA (d8-EA) electrolytes were successfully cycled between 2.8 V and 4.7 V at 40°C for 250 h without significant capacity loss, polarization growth, or gas production. The signal-to-noise ratio of neutron powder diffraction patterns taken on NMC(442) powder with a conventional deuterated organic carbonate-based electrolyte and filled with LiFSi:LiPF 6 :d8-EA electrolyte were virtually identical. Out of all the solvents widely available in deuterated form tested in highly-concentrated systems, EA was the only one providing a good balance between cost and charge-discharge capacity retention to 4.7 V. The use of such an electrolyte blend would half the cost of deuterated solvents needed for in situ neutron diffraction measurements of Li-ion batteries compared to conventional deuterated carbonate-based electrolytes

  8. In situ room temperature tensile deformation of a 1% CrMoV bainitic steel using synchrotron and neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Weisser, M.A. [Paul Scherrer Institut, CH-5232 Villigen (Switzerland); Ecole Polytechnique Federale de Lausanne (EPFL), Institute of Materials (IMX), CH-1012 Lausanne (Switzerland); Evans, A.D.; Van Petegem, S. [Paul Scherrer Institut, CH-5232 Villigen (Switzerland); Holdsworth, S.R. [EMPA Materials Science and Technology, CH-8600 Duebendorf (Switzerland); Van Swygenhoven, H., E-mail: helena.vs@psi.ch [Paul Scherrer Institut, CH-5232 Villigen (Switzerland); Ecole Polytechnique Federale de Lausanne (EPFL), Institute of Materials (IMX), CH-1012 Lausanne (Switzerland)

    2011-06-15

    Neutron and synchrotron X-ray diffraction spectra have been acquired during room temperature tensile deformation of a creep-resistant bainitic 1% CrMoV steel, in order to study the evolution of internal microstresses and load-sharing mechanisms between the ferrite matrix and the various carbides. Cementite takes load from the plastifying matrix at the onset of macroscopic plasticity resulting in residual interphase stresses. Single peak fitting indicates an elastic anisotropic behaviour of cementite.

  9. Static tensile deformation behavior of a lean duplex stainless steel studied by in situ neutron diffraction and synchrotron radiation white x-rays

    International Nuclear Information System (INIS)

    Tsuchida, Noriyuki; Kawahata, Taiji; Ishimaru, Eiichiro; Takahashi, Akihiko; Suzuki, Hiroshi; Shobu, Takahisa

    2013-01-01

    To investigate the tensile deformation behavior of a lean duplex stainless steel (S32101) from the viewpoints of plastic deformability among phases or grains, we performed static tensile tests, in situ neutron diffraction, and white x-ray diffraction experiments at room temperature. In the static tensile tests, the S32101 steel displayed a larger uniform elongation and a better tensile strength-uniform elongation balance than a commercial SUS329J4L duplex stainless steel. A larger uniform elongation of S32101 is associated with the macroscopic work hardening behavior that a work hardening rate higher than the flow stress can maintain up until high true strains. From the experimental results of synchrotron radiation white x-ray diffraction experiments, the hard phase of S32101 was changed from the ferrite (α) phase to austenite (γ) one during tensile deformation. This led to a larger stress partitioning between the phases at the latter stage of deformation. From the experimental results of in situ neutron diffraction, it was found that the stress partitioning of the γ phase in the S32101 was the largest among the present results. Therefore, the larger work hardening rate of S32101 can be explained by the large stress partitioning of the γ phase, that between γ and α phases and γ volume fraction. (author)

  10. Advances in martensitic transformations in Cu-based shape memory alloys achieved by in situ neutron and synchrotron X-ray diffraction methods

    Czech Academy of Sciences Publication Activity Database

    Malard, B.; Šittner, Petr; Berveiller, S.; Patoor, E.

    2012-01-01

    Roč. 13, č. 3 (2012), s. 280-292 ISSN 1631-0705 R&D Projects: GA ČR GAP108/10/1296; GA ČR GAP107/12/0800 EU Projects: European Commission(XE) 262806 - SmartNets Institutional research plan: CEZ:AV0Z10100520 Keywords : stress induced martensitic transformation * Cu-based shape memory alloys * neutron diffraction * X-ray * synchrotron * in situ * multiscale analysis Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.818, year: 2012

  11. Dynamical theory of neutron diffraction

    International Nuclear Information System (INIS)

    Sears, V.F.

    1978-01-01

    We present a review of the dynamical theory of neutron diffraction by macroscopic bodies which provides the theoretical basis for the study of neutron optics. We consider both the theory of dispersion, in which it is shown that the coherent wave in the medium satisfies a macroscopic one-body Schroedinger equation, and the theory of reflection, refraction, and diffraction in which the above equation is solved for a number of special cases of interest. The theory is illustrated with the help of experimental results obtained over the past 10 years by a number of new techniques such as neutron gravity refractometry. Pendelloesung interference, and neutron interferometry. (author)

  12. Analysis of neutron diffraction spectra acquired in situ during stress-induced transformations in superelastic NiTi

    International Nuclear Information System (INIS)

    Vaidyanathan, R.; Bourke, M.A.; Dunand, D.C.

    1999-01-01

    Neutron diffraction spectra were obtained during various stages of a reversible stress-induced austenite to martensite phase transformation in superelastic NiTi. This was accomplished by neutron diffraction measurements on bulk polycrystalline NiTi samples simultaneously subjected to mechanical loading. Analysis of the data was carried out using individual lattice plane (hkl) reflections as well as by Rietveld refinement. In the Rietveld procedure, strains in austenite were described in terms of an isotropic (hkl independent) and an anisotropic (hkl dependent) component. At higher stresses, austenite lattice plane reflections exhibited nonlinear and dissimilar elastic responses which may be attributed to the transformation. The texture evolution is significant in both austenite and martensite phases during the transformation and two approaches were used to describe this evolving texture, i.e., an ellipsoidal model due to March - Dollase and a generalized spherical-harmonic approach. The respective predictions of the phase fraction evolution as a function of applied stress were compared. A methodology is thus established to quantify the discrete phase strains, phase volume fractions, and texture during such transformations. copyright 1999 American Institute of Physics

  13. Neutron Powder Diffraction in Sweden

    International Nuclear Information System (INIS)

    Tellgren, R.

    1986-01-01

    Neutron powder diffraction in Sweden has developed around the research reactor R2 in Studsvik. The article describes this facility and presents a historical review of research results obtained. It also gives some ideas of plans for future development

  14. The effect of low-temperature aging on the microstructure and deformation of uranium- 6 wt% niobium: An in-situ neutron diffraction study

    Energy Technology Data Exchange (ETDEWEB)

    Brown, D.W., E-mail: dbrown@lanl.gov [Material Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM, 87545 (United States); Bourke, M.A.M. [Material Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM, 87545 (United States); Clarke, A.J. [Department of Metallurgical and Materials Engineering, Colorado School of Mines, 1500 Illinois Street, Golden, CO, 80401 (United States); Field, R.D.; Hackenberg, R.E.; Hults, W.L. [Material Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM, 87545 (United States); Thoma, D.J. [Department of Materials Science and Engineering, University of Wisconsin Madison, Madison, WI, 3706 (United States)

    2016-12-01

    The mechanical properties of uranium-niobium alloys evolve with aging at relatively low temperatures due to subtle microstructural changes. In-situ neutron diffraction measurements during aging of a monoclinic U-6Nb alloy at temperatures to 573 K were performed to monitor these changes. Further, in-situ neutron diffraction studies during deformation of U-6Nb in the as-quenched state and after aging for two and eight hours at 473 K were completed to assess the influence of microstructural evolution on mechanical properties. With heating, large anisotropic changes in lattice parameter were observed followed by relaxation with time at the aging temperature. The lattice parameters return to nearly their initial values with cooling. The active plastic deformation mechanisms including, in order of occurrence, shape-memory de-twinning, mechanical twinning, and slip-mediated deformation do not change with prior aging. However, the resistance to motion of the as-quenched martensitic twin boundaries increases following aging, resulting in the observed increase in initial yield strength.

  15. Neutron diffraction studies of glasses

    International Nuclear Information System (INIS)

    Wright, A.C.

    1987-01-01

    A survey is given of the application of neutron diffraction to structural studies of oxide and halide glasses. As with crystalline materials, neutron and X-ray diffraction are the major structural probes for glasses and other amorphous solids, particularly in respect of intermediate range order. The glasses discussed mostly have structures which are dominated by a network in which the bonding is predominantly covalent. The examples discussed demonstrate the power of the neutron diffraction technique in the investigation of the structures of inorganic glasses. The best modern diffraction experiments are capable of providing accurate data with high real space resolution, which if used correctly, are an extremely fine filter for the various structural models proposed in the literature. 42 refs

  16. A study of nitrogenation of a NdFe12-xMox compound by in situ neutron powder diffraction

    International Nuclear Information System (INIS)

    Loong, C.; Short, S.M.; Lin, J.; Ding, Y.

    1998-01-01

    The effects on the crystal lattice of a NdFe 12-x Mo x (x congruent 1.7) during controlled nitrogenation over the 25 endash 600 degree C temperature range were studied by neutron powder diffraction. Prior to nitrogenation the sample contained a major phase of NdFe 10.3 Mo 1.7 and a minor phase (∼12vol%) of bcc-Fe. The sample inside the furnace was connected to a closed volume of ultrapure nitrogen gas while neutron data were collected over regular time intervals during sequential heating. Substantial nitrogen absorption occurred between 500 and 600 degree C. During the nitrogenation process the NdFe 12-x Mo x N y lattice expanded while the bcc-Fe lattice contracted. An increasing decomposition of the compound into bcc-Fe at 600 degree C was observed. The average size of the NdFe 12-x Mo x N y crystalline grains decreased starting at ∼300 degree C, reaching a minimum at ∼500 degree C and then increased markedly at higher temperatures. The development of lattice strains, on the other hand, showed an opposite trend, i.e., a maximum at 500 degree C. copyright 1998 American Institute of Physics

  17. Neutron diffraction and oxide research

    International Nuclear Information System (INIS)

    Hunter, B.; Howard, C.J.; Kennedy, B.J.

    1999-01-01

    Oxide compounds form a large class of interesting materials that have a diverse range of mechanical and electronic properties. This diversity and its commercial implications has had a significant impact on physics research. This is particularly evident in the fields of superconductivity magnetoresistivity and ferroelectricity, where discoveries in the last 15 years have given rise to significant shifts in research activities. Historically, oxides have been studied for many years, but it is only recently that significant effort has been diverted to the study of oxide materials for their application to mechanical and electronic devices. An important property of such materials is the atomic structure, for the determination of which diffraction techniques are ideally suited. Recent examples of structure determinations using neutron diffraction in oxide based systems are high temperature superconductors, where oxygen defects are a key factor. Here, neutron diffraction played a major role in determining the effect of oxygen on the superconducting properties. Similarly, neutron diffraction has enjoyed much success in the determination of the structures of the manganate based colossal magnetoresistive (CMR) materials. In both these cases the structure plays a pivotal role in determining theoretical models of the electronic properties. The neutron scattering group at ANSTO has investigated several oxide systems using neutron powder diffraction. Two such systems are presented in this paper; the zirconia-based materials that are used as engineering materials, and the perovskite-based oxides that include the well known cuprate superconductors and the manganate CMR materials

  18. Neutron diffraction and lattice defects

    International Nuclear Information System (INIS)

    Hamaguchi, Yoshikazu

    1974-01-01

    Study on lattice defects by neutron diffraction technique is described. Wave length of neutron wave is longer than that of X-ray, and absorption cross-section is small. Number of defects observed by ESR is up to several defects, and the number studied with electron microscopes is more than 100. Information obtained by neutron diffraction concerns the number of defects between these two ranges. For practical analysis, several probable models are selected from the data of ESR or electron microscopes, and most probable one is determined by calculation. Then, defect concentration is obtained from scattering cross section. It is possible to measure elastic scattering exclusively by neutron diffraction. Minimum detectable concentration estimated is about 0.5% and 10 20 - 10 21 defects per unit volume. A chopper and a time of flight system are used as a measuring system. Cold neutrons are obtained from the neutron sources inserted into reactors. Examples of measurements by using similar equipments to PTNS-I system of Japan Atomic Energy Research Institute are presented. Interstitial concentration in the graphite irradiated by fast neutrons is shown. Defects in irradiated MgO were also investigated by measuring scattering cross section. Study of defects in Ge was made by measuring total cross section, and model analysis was performed in comparison with various models. (Kato, T.)

  19. Neutron Diffraction and Inorganic Materials Discovery

    International Nuclear Information System (INIS)

    Rosseinsky, M.J.

    2005-01-01

    Full text: The discovery of complex inorganic materials is an important academic and technological challenge because of the opportunities these systems offer for observation of new phenomena, and the questions they pose for fundamental understanding. This presentation will illustrate the key role of neutron powder diffraction in enabling the discovery of new classes of materials, and in evaluating their properties and the conditions under which they need to be processed to optimise their behaviour in devices for applications. New chemistry is illustrated by the transition metal oxide hydrides, where both structure and ionic mobility required neutron scattering characterisation. The relationship between chemistry, structure and properties will be addressed by considering the difficulties in inducing superconductivity in analogues of magnesium diboride. The role of both neutron and X-ray diffraction in evaluating the processing of microwave dielectric ceramics will be highlighted, with the discovery of new phases shown to be a useful bonus in this type of in-situ study. (author)

  20. Neutron diffraction on pulsed sources

    International Nuclear Information System (INIS)

    Aksenov, V.L.; Balagurov, A.M.

    2016-01-01

    The possibilities currently offered and major scientific problems solved by time-of-flight neutron diffraction are reviewed. The reasons for the rapid development of the method over the last two decades has been mainly the emergence of third generation pulsed sources with a MW time-averaged power and advances in neutron-optical devices and detector systems. The paper discusses some historical aspects of time-of-flight neutron diffraction and examines the contribution to this method by F.L.Shapiro whose 100th birth anniversary was celebrated in 2015. The state of the art with respect to neutron sources for studies on output beams is reviewed in a special section. [ru

  1. Industrial applications of neutron diffraction

    International Nuclear Information System (INIS)

    Felcher, G.P.

    1989-01-01

    Neutron diffraction (or, to be more general, neutron scattering) is a most versatile and universal tool, which has been widely employed to probe the structure, the dynamics and the magnetism of condensed matter. Traditionally used for fundamental research in solid state physics, this technique more recently has been applied to problems of immediate industrial interest, as illustrated in examples covering the main fields of endeavour. 14 refs., 14 figs

  2. Quantitative analysis of tensile deformation behavior by in-situ neutron diffraction for ferrite-martensite type dual-phase steels

    International Nuclear Information System (INIS)

    Morooka, Satoshi; Umezawa, Osamu; Harjo, Stefanus; Hasegawa, Kohei; Toji, Yuki

    2012-01-01

    The yielding and work-hardening behavior of ferrite-martensite type dual-phase (DP) alloys were clearly analyzed using the in-situ neutron diffraction technique. We successfully established a new method to estimate the stress and strain partitioning between ferrite and martensite phase during loading. Although these phases exhibit the same lattice structure with similar lattice parameters, their lattice strains on (110), (200) and (211) are obviously different from each other under an applied stress. The misfit strains between those phases were clearly accompanied with the phase-scaled internal stream (phase stress). Thus, the martensite phase yielded by higher applied stress than macro-yield stress, which resulted in high work-hardening rate of the DP steel. We also demonstrated that ferrite phase fraction influenced work-hardening behavior. (author)

  3. In Situ Study of Microstructure Evolution in Solidification of Hypereutectic Al-Si Alloys with Application of Thermal Analysis and Neutron Diffraction

    Science.gov (United States)

    Sediako, Dimitry G.; Kasprzak, Wojciech

    2015-09-01

    Understanding of the kinetics of solid-phase evolution in solidification of hypereutectic aluminum alloys is a key to control their as-cast microstructure and resultant mechanical properties, and in turn, to enhance the service characteristics of actual components. This study was performed to evaluate the solidification kinetics for three P-modified hypereutectic Al-19 pct Si alloys: namely, Al-Si binary alloy and with the subsequent addition of 2.8 pct Cu and 2.8 pct Cu + 0.7 pct Mg. Metallurgical evaluation included thermodynamic calculations of the solidification process using the FactSage™ 6.2 software package, as well as experimental thermal analysis, and in situ neutron diffraction. The study revealed kinetics of solid α-Al, solid Si, Al2Cu, and Mg2Si evolution, as well as the individual effects of Cu and Mg alloying additions on the solidification path of the Al-Si system. Various techniques applied in this study resulted in some discrepancies in the results. For example, the FactSage computations, in general, resulted in 281 K to 286 K (8 °C to 13 °C) higher Al-Si eutectic temperatures than the ones recorded in the thermal analysis, which are also ~278 K (~5 °C) higher than those observed in the in situ neutron diffraction. None of the techniques can provide a definite value for the solidus temperature, as this is affected by the chosen calculation path [283 K to 303 K (10 °C to 30 °C) higher for equilibrium solidification vs non-equilibrium] for the FactSage analysis; and further complicated by evolution of secondary Al-Cu and Mg-Si phases that commenced at the end of solidification. An explanation of the discrepancies observed and complications associated with every technique applied is offered in the paper.

  4. Deformation behavior of Mg-8.5wt.%Al alloy under reverse loading investigated by in-situ neutron diffraction and elastic viscoplastic self-consistent modeling

    International Nuclear Information System (INIS)

    Wang, H.; Lee, S.Y.; Gharghouri, M.A.; Wu, P.D.; Yoon, S.G.

    2016-01-01

    The EVPSC-TDT model for polycrystal plasticity and in-situ neutron diffraction have been used to investigate the behavior of a Mg-8.5wt.%Al alloy with two starting textures: 1) a typical extrusion texture in which a majority of the grains are oriented favorably for extension twinning via compression perpendicular to the basal pole, and 2) a modified texture in which extension twinning can be activated via tension parallel to the basal pole in a majority of the grains. Using a small number of adjustable parameters, and only two macroscopic tensile stress–strain curves for calibration, the model is able to capture, quantitatively, the trends in multiple data sets, including grain-level elastic lattice strains, and diffraction peak intensity changes due to lattice re-orientation associated with twinning. For twinning, the model assumes a polar critical resolved shear stress activation criterion and assigns the stress and hardening of the parent crystal to a newly formed twin. The model allows twinning to be driven either by the stress in the parent crystal (matrix reduction), in which case all of the twin transformation strain is assigned to the matrix, or by the stress in the twin (twin propagation), in which case all of the twin transformation strain is assigned to the twin. A detailed comparison between the model predictions and the neutron diffraction data reveals that assigning all of the twin transformation strain either to the matrix or to the twin is too one-sided, leading to excessive relaxation and hardening effects. A more equitable partitioning of the twin transformation strain is necessary. It is suggested that the stress and hardening assigned to a newly formed twin is of less importance to the performance of the model than the partitioning of the twin transformation strain.

  5. In situ neutron diffraction study of the plastic deformation mechanisms of B2 ordered intermetallic alloys: NiAl, CuZn, and CeAg

    Energy Technology Data Exchange (ETDEWEB)

    Wollmershauser, J.A. [Department of Materials Science and Engineering, University of Virginia, P.O. Box 400745, 116 Engineer' s Way, Charlottesville, VA 22904-04745 (United States); Kabra, S. [Materials Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Agnew, S.R. [Department of Materials Science and Engineering, University of Virginia, P.O. Box 400745, 116 Engineer' s Way, Charlottesville, VA 22904-04745 (United States)], E-mail: sra4p@virginia.edu

    2009-01-15

    The internal stress developments of B2 compounds NiAl, CuZn, and CeAg are examined using in situ neutron diffraction. CeAg is a representative of a newly discovered class of fully ordered and ductile B2 compounds. Using polycrystal plasticity modeling to interpret the results, it is revealed that the internal stress evolution of CeAg is nearly identical to that of NiAl, indicating that they share a common primary mechanism of plastic deformation, i.e., <1 0 0>{l_brace}0 1 1{r_brace} 'cube' slip. This result reinforces the dilemma previously observed for rare-earth alloys CuY, AgY, and CuDy, since cube slip provides insufficient independent slip systems to accommodate large-scale homogenous polycrystalline deformation. There is no evidence in the diffraction data of either mechanical twinning or stress-induced phase transformation. The activity of bcc-type <1 1 1>{l_brace}11-bar0{r_brace} slip at high stresses is confirmed and a lower bound for the critical resolved shear stress is quantified.

  6. Neutron diffraction and Vitamin E

    Energy Technology Data Exchange (ETDEWEB)

    Harroun, T A; Marquardt, D; Katsaras, J; Atkinson, J, E-mail: tharroun@brocku.ca

    2010-11-01

    It is generally accepted that neutron diffraction from model membrane systems is an effective biophysical technique for determining membrane structure. Here we describe an example of how deuterium labelling can elucidate the location of specific membrane soluble molecules, including a brief discussion of the technique itself. We show that deuterium labelled {alpha}-tocopherol sits upright in the bilayer, as might be expected, but at very different locations within the bilayer, depending on the degree of lipid chain unsaturation.

  7. A-site order–disorder in the NdBaMn2O5+δ SOFC electrode material monitored in situ by neutron diffraction under hydrogen flow

    KAUST Repository

    Tonus, Florent

    2017-05-11

    The A-site disordered perovskite manganite, Nd0.5Ba0.5MnO3, has been obtained by heating the A-site-ordered and vacancy ordered layered double perovskite, NdBaMn2O5, in air at 1300 °C for 5 h. Combined transmission electron microscopy (TEM) images and neutron powder diffraction (NPD) analysis at 25 °C revealed that Nd0.5Ba0.5MnO3 has a pseudotetragonal unit cell with orthorhombic symmetry (space group Imma, √2ap × 2ap × √2ap) at 20 °C with the cell dimensions a = 5.503(1) Å, b = 7.7962(4) Å, c = 5.502(1) Å, in contrast to Pm[3 with combining macron]m or Cmcm that have been previously stated from X-ray diffraction studies. The in situ neutron diffraction study carried out on Nd0.5Ba0.5MnO3 in hydrogen flow up to T ∼ 900 °C, allows monitoring the A-site cation disorder–order structural phase transition of this representative member of potential SOFC anode materials between air sintering conditions and hydrogen working conditions. Oxygen loss from Nd0.5Ba0.5MnO3 proceeds with retention of A-site disorder until the oxygen content reaches the Nd0.5Ba0.5MnO2.5 composition at 600 °C. The phase transition to layered NdBaMn2O5 and localization of the oxygen vacancies in the Nd layer proceeds at 800 °C with retention of the oxygen content. Impedance spectroscopy measurements for the oxidized A-site ordered electrode material, NdBaMn2O6, screen printed on a Ce0.9Gd0.1O2−δ (CGO) electrolyte showed promising electrochemical performance in air at 700 °C with a polarization resistance of 1.09 Ω cm2 without any optimization.

  8. Magnetic structures: neutron diffraction studies

    International Nuclear Information System (INIS)

    Bouree-Vigneron, F.

    1990-01-01

    Neutron diffraction is often an unequivocal method for determining magnetic structures. Here we present some typical examples, stressing the sequence through experiments, data analysis, interpretation and modelisation. Two series of compounds are chosen: Tb Ni 2 Ge 2 and RBe 13 (R = Gd, Tb, Dy, Ho, Er). Depending on the nature of the elements, the magnetic structures produced can be commensurate, incommensurate or even show a transition between two such phases as a function of temperature. A model, taking magnetic exchange and anisotropy into account, will be presented in the case of commensurate-incommensurate magnetic transitions in RBe 13

  9. Current-dependent electrode lattice fluctuations and anode phase evolution in a lithium-ion battery investigated by in situ neutron diffraction

    International Nuclear Information System (INIS)

    Sharma, Neeraj; Peterson, Vanessa K.

    2013-01-01

    Highlights: ► Links between time-dependent structural parameters and battery performance. ► Current-dependent evolution of the anode. ► Direct correlation of LixCoO 2 and LiC 6 structure with battery capacity. -- Abstract: This work uses real-time in situ neutron powder diffraction to study the electrode lattice response and anode phase evolution in a commercial lithium-ion battery. We show that the time-resolved lattice response of the Li x CoO 2 cathode and Li x C 6 anode under non-equilibrium conditions varies proportionally with the applied current, where higher current results in faster structural change. Higher current also reduces the Li x CoO 2 cathode c lattice parameter and the LiC 6 quantity that forms at the charged state of the battery, both of which are related to lower battery capacity. At the anode, we find that the Li x C 6 phase evolution is current-dependent

  10. In situ neutron diffraction and polycrystal plasticity modeling of a Mg–Y–Nd–Zr alloy: Effects of precipitation on individual deformation mechanisms

    International Nuclear Information System (INIS)

    Agnew, S.R.; Mulay, R.P.; Polesak, F.J.; Calhoun, C.A.; Bhattacharyya, J.J.; Clausen, B.

    2013-01-01

    In situ neutron diffraction compression tests were performed on Mg–Y–Nd–Zr alloy WE43, in the solution heat-treated, peak- and over-aged conditions. The flow curves and internal strain evolutions were modeled using polycrystal plasticity simulation, with the inclusion of an elastic phase to account for the presence of precipitates. The results reveal that prismatic plate-shaped precipitates strongly impede basal slip; the critical resolved shear strength (CRSS) of basal slip increases from 12 to 37 MPa, an increase of over 200%. However, hard deformation modes such as non-basal slip of 〈a〉 dislocations are required for macroscopic yielding. These hard modes are not as strongly affected by aging, with CRSS values which increase from 78 to 92 MPa, an increase of only 18%. The results of the study are consistent with recent modeling of the relative Orowan strengthening of individual deformation modes and the superposition of various strengthening effects (solid solution and precipitation). This finding helps to explain why the age-hardening response of Mg–Y–Nd–Zr alloys is not exceptional. It is concluded that future precipitation-strengthened alloy and process design strategies should focus on promoting high number densities of particles. The effect of aging upon twinning is surprising. The most age-hardened material exhibits more twinning than the solutionized material. To model this behavior using polycrystal plasticity, the critical stress to activate twinning (especially the strain hardening thereof) must be decreased

  11. In Situ Neutron Diffraction Analyzing Stress-Induced Phase Transformation and Martensite Elasticity in [001]-Oriented Co49Ni21Ga30 Shape Memory Alloy Single Crystals

    Science.gov (United States)

    Reul, A.; Lauhoff, C.; Krooß, P.; Gutmann, M. J.; Kadletz, P. M.; Chumlyakov, Y. I.; Niendorf, T.; Schmahl, W. W.

    2018-02-01

    Recent studies demonstrated excellent pseudoelastic behavior and cyclic stability under compressive loads in [001]-oriented Co-Ni-Ga high-temperature shape memory alloys (HT-SMAs). A narrow stress hysteresis was related to suppression of detwinning at RT and low defect formation during phase transformation due to the absence of a favorable slip system. Eventually, this behavior makes Co-Ni-Ga HT-SMAs promising candidates for several industrial applications. However, deformation behavior of Co-Ni-Ga has only been studied in the range of theoretical transformation strain in depth so far. Thus, the current study focuses not only on the activity of elementary deformation mechanisms in the pseudoelastic regime up to maximum theoretical transformation strains but far beyond. It is shown that the martensite phase is able to withstand about 5% elastic strain, which significantly increases the overall deformation capability of this alloy system. In situ neutron diffraction experiments were carried out using a newly installed testing setup on Co-Ni-Ga single crystals in order to reveal the nature of the stress-strain response seen in the deformation curves up to 10% macroscopic strain.

  12. Low temperature nickel titanium iron shape memory alloys: Actuator engineering and investigation of deformation mechanisms using in situ neutron diffraction at Los Alamos National Laboratory

    Science.gov (United States)

    Krishnan, Vinu B.

    Shape memory alloys are incorporated as actuator elements due to their inherent ability to sense a change in temperature and actuate against external loads by undergoing a shape change as a result of a temperature-induced phase transformation. The cubic so-called austenite to the trigonal so-called R-phase transformation in NiTiFe shape memory alloys offers a practical temperature range for actuator operation at low temperatures, as it exhibits a narrow temperature-hysteresis with a desirable fatigue response. Overall, this work is an investigation of selected science and engineering aspects of low temperature NiTiFe shape memory alloys. The scientific study was performed using in situ neutron diffraction measurements at the newly developed low temperature loading capability on the Spectrometer for Materials Research at Temperature and Stress (SMARTS) at Los Alamos National Laboratory and encompasses three aspects of the behavior of Ni46.8Ti50Fe3.2 at 92 K (the lowest steady state temperature attainable with the capability). First, in order to study deformation mechanisms in the R-phase in NiTiFe, measurements were performed at a constant temperature of 92 K under external loading. Second, with the objective of examining NiTiFe in one-time, high-stroke, actuator applications (such as in safety valves), a NiTiFe sample was strained to approximately 5% (the R-phase was transformed to B19' phase in the process) at 92 K and subsequently heated to full strain recovery under a load. Third, with the objective of examining NiTiFe in cyclic, low-stroke, actuator applications (such as in cryogenic thermal switches), a NiTiFe sample was strained to 1% at 92 K and subsequently heated to full strain recovery under load. Neutron diffraction spectra were recorded at selected time and stress intervals during these experiments. The spectra were subsequently used to obtain quantitative information related to the phase-specific strain, texture and phase fraction evolution using the

  13. Modern techniques of structural neutron diffraction

    International Nuclear Information System (INIS)

    Aksenov, V.L.; )

    1997-01-01

    Modern techniques of neutron diffraction for structural investigations are analyzed. The time-of-flight method and the reverse time-of-flight method are considered briefly. Characteristics of two-crystal and time-of-flight neutron diffractometers are compared. It is pointed that in the future, the great importance will be possessed the development of high-resolution Fourier neutron diffractometers [ru

  14. In Situ Neutron Diffraction of Rare-Earth Phosphate Proton Conductors Sr/Ca-doped LaPO4 at Elevated Temperatures

    Science.gov (United States)

    Al-Wahish, Amal; Al-Binni, Usama; Bridges, C. A.; Huq, A.; Bi, Z.; Paranthaman, M. P.; Tang, S.; Kaiser, H.; Mandrus, D.

    Acceptor-doped lanthanum orthophosphates are potential candidate electrolytes for proton ceramic fuel cells. We combined neutron powder diffraction (NPD) at elevated temperatures up to 800° C , X-ray powder diffraction (XRD) and scanning electron microscopy (SEM) to investigate the crystal structure, defect structure, thermal stability and surface topography. NPD shows an average bond length distortion in the hydrated samples. We employed Quasi-Elastic Neutron Scattering (QENS) and electrochemical impedance spectroscopy (EIS) to study the proton dynamics of the rare-earth phosphate proton conductors 4.2% Sr/Ca-doped LaPO4. We determined the bulk diffusion and the self-diffusion coefficients. Our results show that QENS and EIS are probing fundamentally different proton diffusion processes. Supported by the U.S. Department of Energy.

  15. Strčess-induced martensitic transformation in Cu-Al-Zn-Mn polycrystal investigated by two in -situ neutron diffraction techniques

    Czech Academy of Sciences Publication Activity Database

    Šittner, Petr; Lukáš, Petr; Neov, Dimitar; Daymond, M. R.; Novák, Václav; Swallowe, G. M.

    2002-01-01

    Roč. 324, - (2002), s. 225-234 ISSN 0921-5093 R&D Projects: GA MŠk ME 186; GA ČR GV202/97/K038; GA AV ČR IAA1010909 Institutional research plan: CEZ:AV0Z1010914 Keywords : Stress-induced martensitic transformation * Cu-Al-Zn-Mn polycrystal * neutron diffraction technique Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.107, year: 2002

  16. Report from the neutron diffraction work group

    International Nuclear Information System (INIS)

    1978-08-01

    This progress report of the neutron diffraction group at the Hahn Meitner Institute in Berlin comprises the following contributions: Three-dimensional critical properties of CsNiF 3 around the Neel point; Spin waves in CsNiF 3 with an applied magnetic field; Solitons in CsNiF 3 : Their experimental evidence and their thermodynamics; Neutron diffraction study of DAG at very low temperatures and in external magnetic field; Neutron diffraction investigation of tricritical behaviour in DyPO 4 ; Crystalline modifications and structural phase transitions of NaOH; Gitterdynamik von Cerhydrid; Investigation of the ferroelectric-ferroelastic phase transition in KH 2 PO 4 and RbH 2 PO 4 by means of γ-ray diffractometry; A γ-ray diffractometer for systematic measurements of absolute structure factors; Electron density in pyrite by combined γ-ray and neutron diffraction measurements: Thermal parameters from short wavelength neutron data; Accurate determination of temperature parameters from neutron diffraction data: Direct observation of the thermal diffuse scattering from silicon using perfect crystals; A Compton spectrometer for momentum density studies using 412 keV γ-radiation; Investigation of the electronic structure of Niobiumhydrides by means of gamma-ray Compton scattering; Interpretation of Compton profile data in position space; High resolution neutron scattering measurements on single crystals using a horizontally bent monochromator and a multidetecter; Statistical analysis of neutron diffraction studies of proteins. (orig.) [de

  17. Solving crystal structures from neutron diffraction data

    International Nuclear Information System (INIS)

    Wilson, C.C.

    1987-07-01

    In order to pursue crystal structure determination using neutron diffraction data, and given the wide experience available of solving structures using X-ray data, the codes used in X-ray structural analysis should be adapted to the different requirements of a neutron experiment. Modifications have been made to a direct methods program MITHRIL and to a Patterson methods program PATMET to incorporate into these the features of neutron rather than X-ray diffraction. While to date these modifications have been fairly straightforward and many sophistications remain to be exploited, results obtained from the neutron versions of both programs are promising. (author)

  18. Internal strain measurement using pulsed neutron diffraction at LANSCE

    International Nuclear Information System (INIS)

    Goldstone, J.A.; Bourke, M.A.M.; Shi, N.

    1994-01-01

    The presence of residual stress in engineering components can effect their mechanical properties and structural integrity. Neutron diffraction in the only technique that can make nondestructive measurements in the interior of components. By recording the change in crystalline lattice spacings, elastic strains can be measured for individual lattice reflections. Using a pulsed neutron source, all lattice reflections are recorded in each measurement, which allows for easy examination of heterogeneous materials such as metal matrix composites. Measurements made at the Manuel Lujan Jr. Neutron Scattering Center (LANSCE) demonstrate the potential at pulsed sources for in-situ stress measurements at ambient and elevated temperatures

  19. Applications of the fresnel diffraction of neutrons

    International Nuclear Information System (INIS)

    Klein, A.G.; Opat, G.I.

    1978-01-01

    The place of Fresnel diffraction in the overall scheme of neutron interference experiments is outlined and possible applications are discussed in the areas of: magnetic domain visualisation; measurement of nuclear scattering lengths with very small specimens; focussing of long wavelength neutron beams using zone plates

  20. Applications of the Fresnel diffraction of neutrons

    International Nuclear Information System (INIS)

    Klein, A.G.; Opat, G.I.

    1978-01-01

    The place of Fresnel diffraction in the overall scheme of neutron interference experiments is outlined and possible applications are discussed in the areas of: magnetic domain visualisation; measurement of nuclear scattering lengths with very small specimens; focussing of long wavelength neutron beams using zone plates

  1. Neutron forward diffraction by single crystal prisms

    Indian Academy of Sciences (India)

    We have derived analytic expressions for the deflection as well as transmitted fraction of monochromatic neutrons forward diffracted by a single crystal prism. In the vicinity of a Bragg reflection, the neutron deflection deviates sharply from that for an amorphous prism, exhibiting three orders of magnitude greater sensitivity to ...

  2. Neutron Larmor diffraction measurements for materials science

    International Nuclear Information System (INIS)

    Repper, J.; Keller, T.; Hofmann, M.; Krempaszky, C.; Petry, W.; Werner, E.

    2010-01-01

    Neutron Larmor diffraction (LD) is a high-resolution diffraction technique based on the Larmor precession of polarized neutrons. In contrast to conventional diffraction, LD does not depend on the accurate measurement of Bragg angles, and thus the resolution is independent of the beam collimation and monochromaticity. At present, a relative resolution for the determination of the crystal lattice spacing d of Δd/d∼10 -6 is achieved, i.e. at least one order of magnitude superior to conventional neutron or X-ray techniques. This work is a first step to explore the application of LD to high-resolution problems in the analysis of residual stresses, where both the accurate measurement of absolute d values and the possibility of measuring type II and III stresses may provide additional information beyond those accessible by conventional diffraction techniques. Data obtained from Inconel 718 samples are presented.

  3. ALADIN - Advanced Laue Diffraction Instruments using Neutrons

    International Nuclear Information System (INIS)

    Lemee-Cailleau, M.H.; Ouladdiaf, B.; McIntyre, G.J.

    2011-01-01

    Laue diffraction techniques have proven to be very attractive to a broad user community interested in obtaining detailed structural information on very small single-crystal samples or needing data collection speeds comparable to those available with the powder diffraction technique. However our experience has clearly demonstrated the negative effect of up-stream monochromatic instruments on the quality of Laue data. In order to obtain Laue diffraction data with a statistical accuracy similar to that achieved on a monochromatic instrument (neutron or X-rays), the project ALADIN (for Advanced Laue Diffraction Instruments using Neutrons) aims to: -) construct a Laue-dedicated thermal neutron guide, with m=2 super-mirror coating, providing access to the desirable wavelength bandwidth; -) installation of one of the ILL Laue diffractometers (VIVALDI or CYCLOPS) on this new guide. (authors)

  4. Neutron Larmor diffraction measurements for materials science

    Energy Technology Data Exchange (ETDEWEB)

    Repper, J., E-mail: julia_repper@web.de [Forschungsneutronenquelle Heinz Maier-Leibnitz (FRM II), TU Muenchen, 85747 Garching (Germany); Keller, T. [Max-Planck-Institut fuer Festkoerperforschung, 70569 Stuttgart (Germany)] [Forschungsneutronenquelle Heinz Maier-Leibnitz (FRM II), TU Muenchen, 85747 Garching (Germany); Hofmann, M. [Forschungsneutronenquelle Heinz Maier-Leibnitz (FRM II), TU Muenchen, 85747 Garching (Germany); Krempaszky, C. [Christian-Doppler-Labor fuer Werkstoffmechanik von Hochleistungslegierungen, TU Muenchen, 85747 Garching (Germany); Petry, W. [Forschungsneutronenquelle Heinz Maier-Leibnitz (FRM II), TU Muenchen, 85747 Garching (Germany); Werner, E. [Lehrstuhl fuer Werkstoffkunde und Werkstoffmechanik, TU Muenchen, 85747 Garching (Germany)

    2010-05-15

    Neutron Larmor diffraction (LD) is a high-resolution diffraction technique based on the Larmor precession of polarized neutrons. In contrast to conventional diffraction, LD does not depend on the accurate measurement of Bragg angles, and thus the resolution is independent of the beam collimation and monochromaticity. At present, a relative resolution for the determination of the crystal lattice spacing d of {Delta}d/d{approx}10{sup -6} is achieved, i.e. at least one order of magnitude superior to conventional neutron or X-ray techniques. This work is a first step to explore the application of LD to high-resolution problems in the analysis of residual stresses, where both the accurate measurement of absolute d values and the possibility of measuring type II and III stresses may provide additional information beyond those accessible by conventional diffraction techniques. Data obtained from Inconel 718 samples are presented.

  5. Quantitative phase analysis by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Chang Hee; Song, Su Ho; Lee, Jin Ho; Shim, Hae Seop [Korea Atomic Energy Research Institute, Taejon (Korea)

    1999-06-01

    This study is to apply quantitative phase analysis (QPA) by neutron diffraction to the round robin samples provided by the International Union of Crystallography(IUCr). We measured neutron diffraction patterns for mixed samples which have several different weight percentages and their unique characteristic features. Neutron diffraction method has been known to be superior to its complementary methods such as X-ray or Synchrotron, but it is still accepted as highly reliable under limited conditions or samples. Neutron diffraction has strong capability especially on oxides due to its scattering cross-section of the oxygen and it can become a more strong tool for analysis on the industrial materials with this quantitative phase analysis techniques. By doing this study, we hope not only to do one of instrument performance tests on our HRPD but also to improve our ability on the analysis of neutron diffraction data by comparing our QPA results with others from any advanced reactor facilities. 14 refs., 4 figs., 6 tabs. (Author)

  6. Interphase microstress measurements in IN 718 by cold neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Repper, J.; Link, P.; Hofmann, M.; Petry, W. [TU Muenchen, Forschungsneutronenquelle Heinz Maier-Leibnitz (FRM II), Garching (Germany); Krempaszky, C. [TU Muenchen, Christian-Doppler-Labor fuer Werkstoffmechanik von Hochleistungslegierungen, Garching (Germany); Werner, E. [TU Muenchen, Lehrstuhl fuer Werkstoffkunde und Werkstoffmechanik, Garching (Germany)

    2010-06-15

    Thermal neutron diffraction is an important and reliable method for the investigation of microscopic stresses. The measurement of Bragg reflections caused by phases of small volume fractions, however, is often intricate due to low intensities and overlapping peaks. The wavelength range of cold neutrons allows to shift the Bragg reflections to larger scattering angles resulting in an increase of relative distances between Bragg reflections. The high resolution of cold neutron diffraction technique is demonstrated by in-situ load tests in which selected Bragg reflections caused by precipitates with small volume fractions in the precipitation strengthened alloy IN 718 are observed. The accumulated microstrains show marked differences in dependence of the precipitated phases within the matrix phase. (orig.)

  7. Neutron powder diffraction under high pressure at J-PARC

    International Nuclear Information System (INIS)

    Utsumi, Wataru; Kagi, Hiroyuki; Komatsu, Kazuki; Arima, Hiroshi; Nagai, Takaya; Okuchi, Takuo; Kamiyama, Takashi; Uwatoko, Yoshiya; Matsubayashi, Kazuyuki; Yagi, Takehiko

    2009-01-01

    It is expected that high-pressure material science and the investigation of the Earth's interior will progress greatly using the high-flux pulse neutrons of J-PARC. In this article, we introduce our plans for in situ neutron powder diffraction experiments under high pressure at J-PARC. The use of three different types of high-pressure devices is planned; a Paris-Edinburgh cell, a new opposed-anvil cell with a nano-polycrystalline diamond, and a cubic anvil high-pressure apparatus. These devices will be brought to the neutron powder diffraction beamlines to conduct a 'day-one' high-pressure experiment. For the next stage of research, we propose construction of a dedicated beamline for high-pressure material science. Its conceptual designs are also introduced here.

  8. Determination of textures by neutron diffraction

    International Nuclear Information System (INIS)

    Dervin, P.; Penelle, R.

    1989-01-01

    In virtue of the low absorption coefficient of most materials in regard to neutrons, neutron diffraction is particularly well adapted for high-precision characterizing of the gross texture of massive fine-grained or coarse-grained specimens of the order of the cubic centimeter. The firt part of this paper is devoted to a description of the distribution of crystalline orientations, and the second part to experimental identification of textures [fr

  9. Neutron diffraction from lead germanate glasses

    International Nuclear Information System (INIS)

    Umesaki, Norimasa; Brunier, T.M.; Wright, A.C.; Hannon, A.C.; Scinclair, R.N.

    1993-01-01

    High resolution neutron diffraction data have been collected on the PbO-GeO 2 glasses and on GeO 2 for comparison. These neutron data have revealed the existence of 6-fold coordinated germanium (GeO 6 octahedra) by virtue of the shift in the first peak in the obtained total correlation function T(r) and increase in the coordination. The neutron results also indicate that PbO exits as PbO 4 pyramids, as found in the orthorhombic form of PbO crystal, in the studied PbO-GeO 2 glasses. (author)

  10. Crystallographic structures of absorbates and neutron diffraction

    International Nuclear Information System (INIS)

    Marti, C.; Thorel, P.

    1975-01-01

    The advantage of neutron diffraction is that it is possible to work at any pressure and therefore to study an adsorbant-adsorbate couple within a wide pressure and temperature range and at thermodynamic equilibrium. Nitrogen adsorbed on graphite and CF 4 adsorbed on graphite were measured [fr

  11. Neutron diffraction in a frustrated ferrite

    International Nuclear Information System (INIS)

    Mirebeau, I.; Iancu, G.; Gavoille, G.; Hubsch, J.

    1994-01-01

    The competition between a long range ordered ferrimagnetic lattice and small fluctuating clusters have been probed by neutron diffraction in a titanium magnesium frustrated ferrite. The description of the system is then compared to the predictions of several theoretical models for frustrated systems. 3 figs., 8 refs

  12. Neutron diffraction of γ-aluminium oxynitride

    NARCIS (Netherlands)

    Willems, H.X.; With, de G.; Metselaar, R.; Helmholdt, R.B.; Petersen, K.K.

    1993-01-01

    Neutron diffraction expts. were performed on Al oxynitride (Alon) powders with compns. corresponding to 67.5, 73 and 77.5 mol.% Al2O3. The 73 mol.% powder was produced by reacting Al2O3 and AlN powders for 3 h at 1750 Deg. After reaction the resultant powder was ground with a mortar and pestle to

  13. Neutron Powder Diffraction and Constrained Refinement

    DEFF Research Database (Denmark)

    Pawley, G. S.; Mackenzie, Gordon A.; Dietrich, O. W.

    1977-01-01

    The first use of a new program, EDINP, is reported. This program allows the constrained refinement of molecules in a crystal structure with neutron diffraction powder data. The structures of p-C6F4Br2 and p-C6F4I2 are determined by packing considerations and then refined with EDINP. Refinement is...

  14. Neutron diffraction from holographic gratings in PMMA

    International Nuclear Information System (INIS)

    Havermeyer, F.; Kraetzig, E.; Rupp, R.A.; Schubert, D.W.

    1999-01-01

    Complete text of publication follows. By definition photorefractive materials change the refractive index for light under the action of light. Using the spatially modulated light intensity pattern from the interference of two plane waves, volume phase gratings with accurately defined spacings can be produced. Depending on the material there are many physical origins for these gratings, but in most cases they are linked to a density modulation and, consequently, to a refractive index grating for neutrons. By diffraction of light or neutrons from such gratings even small refractive index changes down to Δn ∼ 10 -7 - 10 -9 can be measured. In our photopolymer system PMMA/MMA (poly(methyl methacrylate) with a content of 10-20% of the residual monomer methyl methacrylate) inhomogeneous illumination leads to local post-polymerisation processes of the residual monomer. The resulting light-optical refractive index grating is caused by the modulation of the monomer/polymer ratio as well as by the modulation of the total density. Only by the unique combination of methods for light and neutron diffraction, available at HOLONS (Holography and Neutron Scattering, instrument at the GKSS research centre), both contributions can be separated. We discuss the angular dependence of the neutron diffraction efficiency for weakly and strongly (efficiencies up to 60% have been achieved) modulated gratings and propose a simple model for the evaluation of the gratings. (author)

  15. Applications of TOF neutron diffraction in archaeometry

    Energy Technology Data Exchange (ETDEWEB)

    Kockelmann, W. [Rutherford Appleton Laboratory, ISIS Facility, Chilton (United Kingdom); Siano, S.; Bartoli, L. [Istituto di Fisica Applicata - CNR, Sesto Fiorentino (Italy); Visser, D. [Rutherford Appleton Laboratory, ISIS Facility, Chilton (United Kingdom); Netherlands Organisation for Scientific Research (NWO), Den Haag (Netherlands); Hallebeek, P. [Netherlands Institute for Cultural Heritage (ICN), Amsterdam (Netherlands); Traum, R. [Kunsthistorisches Museum Wien, Muenzkabinett, Vienna (Austria); Linke, R.; Schreiner, M. [Akademie der Bildenden Kuenste, Institut fuer Wissenschaften und Technologien in der Kunst, Vienna (Austria); Kirfel, A. [Universitaet Bonn, Mineralogisch-Petrologisches Institut, Bonn (Germany)

    2006-05-15

    Neutron radiation meets the demand for a versatile diagnostic probe for collecting information from the interior of large, undisturbed museum objects or archaeological findings. Neutrons penetrate through coatings and corrosion layers deep into centimetre-thick materials, a property that makes them ideal for non-destructive examination of objects for which sampling is impractical or unacceptable. A particular attraction of neutron techniques for archaeologists and conservation scientists is the prospect of locating hidden materials and structures inside objects. Time-of-flight (TOF) neutron diffraction allows for the examination of mineral and metal phase contents, crystal structures, grain orientations, and microstructures as well as micro- and macro strains. A promising application is texture analysis which may provide clues to the deformation history of the material, and hence to specific working processes. Here we report on instructive examples of TOF neutron diffraction, including phase analyses of medieval Dutch tin-lead spoons, texture analyses of bronze specimens as well as of 16th-century silver coins. (orig.)

  16. Neutron diffraction on polymorphic phases of phospholipids

    International Nuclear Information System (INIS)

    Adachi, Tomohiro; Furusaka, Michihiro; Otomo, Toshiya; Hatta, Ichiro

    2001-01-01

    Small angle neutron diffraction experiments were performed in DPPC and DPPC/cholesterol systems. We investigated the DPPC-d62 bilayers without cholesterol and the DPPC-d75 bilayers with 5 and 15 mol% cholesterol. For DPPC-d62 systems, in the gel and fluid phase, the reflections up to third order from lamellar structure were observed. Scattering length density profiles of these systems were generated. They show that the packing density of hydrocarbon chain in gel phase is higher than in fluid phase. We show that the neutron diffraction experiment is effective on observing the packing and the scattering length density of the hydrocarbon chain. On the other hand, for DPPC-d75/cholesterol systems, only the reflection from the ripple structure was observed. It shows that cholesterol is periodically localized in accordance with ripple structure forming a periodic bandlike structure parallel to a ridge of the ripple structure. (author)

  17. Powder Neutron Diffraction and Magnetic structures

    International Nuclear Information System (INIS)

    Vigneron, F.

    1986-01-01

    The determination of the magnetic structures of materials (ferromagnetic, antiferromagnetic, helimagnetic, .) can be achieved only by neutron diffraction. A general survey of the powder technique is given: 2-axis spectrometer and analysis of the magnetic data. For the REBe/sb13/ intermetallic compounds (RE = Rare Earth), commensurate and/or incommensurate magnetic structures are observed and discussed as a function of RE (Gd, Tb, Dy, Ho, Er)

  18. DNA hydration studied by neutron fiber diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Fuller, W.; Forsyth, V.T.; Mahendrasingam, A.; Langan, P.; Pigram, W.J. [Keele Univ. (United Kingdom)] [and others

    1994-12-31

    The development of neutron high angle fiber diffraction to investigate the location of water around the deoxyribonucleic acid (DNA) double-helix is described. The power of the technique is illustrated by its application to the D and A conformations of DNA using the single crystal diffractometer, D19, at the Institute Laue-Langevin, Grenoble and the time of flight diffractometer, SXD, at the Rutherford Appleton ISIS Spallation Neutron Source. These studies show the existence of bound water closely associated with the DNA. The patterns of hydration in these two DNA conformations are quite distinct and are compared to those observed in X-ray single crystal studies of two-stranded oligodeoxynucleotides. Information on the location of water around the DNA double-helix from the neutron fiber diffraction studies is combined with that on the location of alkali metal cations from complementary X-ray high angle fiber diffraction studies at the Daresbury Laboratory SRS using synchrotron radiation. These analyses emphasize the importance of viewing DNA, water and ions as a single system with specific interactions between the three components and provide a basis for understanding the effect of changes in the concentration of water and ions in inducing conformations] transitions in the DNA double-helix.

  19. TOF neutron diffraction study of archaeological ceramics

    International Nuclear Information System (INIS)

    Kockelmann, W.; Kirfel, A.

    1999-01-01

    Complete text of publication follows. The time-of flight (TOF) neutron diffractometer ROTAX [1] at ISIS has been used for identification and quantitative phase analysis of archaeological pottery. Neutron diffraction yields mineral phase fractions which, in parallel with information obtained from other archaeometric examination techniques, can provide a fingerprint that can be used to identify provenance and reconstruct methods of manufacturing of an archaeological ceramic product. Phase fractions obtained from a 13th century Rhenish stoneware jar compare well with those obtained from a powder sample prepared from the same fragment. This indicates that reliable results can be obtained by illuminating a large piece or even an intact ceramic object making TOF neutron diffraction a truly non-destructive examination technique. In comparison to X-ray diffraction, information from the bulk sample rather than from surface regions is obtained. ROTAX allows for a simple experimental set-up, free of sample movements. Programmes of archaeological study on ROTAX involve Russian samples (Upper-Volga culture, 5000-2000 BC), Greek pottery, (Agora/Athens, 500-300 BC), and medieval German earthenware and stoneware ceramics (Siegburg waster heap, 13-15th century). (author)

  20. DNA hydration studied by neutron fiber diffraction

    International Nuclear Information System (INIS)

    Fuller, W.; Forsyth, V.T.; Mahendrasingam, A.; Langan, P.; Pigram, W.J.

    1994-01-01

    The development of neutron high angle fiber diffraction to investigate the location of water around the deoxyribonucleic acid (DNA) double-helix is described. The power of the technique is illustrated by its application to the D and A conformations of DNA using the single crystal diffractometer, D19, at the Institute Laue-Langevin, Grenoble and the time of flight diffractometer, SXD, at the Rutherford Appleton ISIS Spallation Neutron Source. These studies show the existence of bound water closely associated with the DNA. The patterns of hydration in these two DNA conformations are quite distinct and are compared to those observed in X-ray single crystal studies of two-stranded oligodeoxynucleotides. Information on the location of water around the DNA double-helix from the neutron fiber diffraction studies is combined with that on the location of alkali metal cations from complementary X-ray high angle fiber diffraction studies at the Daresbury Laboratory SRS using synchrotron radiation. These analyses emphasize the importance of viewing DNA, water and ions as a single system with specific interactions between the three components and provide a basis for understanding the effect of changes in the concentration of water and ions in inducing conformations] transitions in the DNA double-helix

  1. Reactivity, structure and physical properties of SrCo{sub 2.5+{delta}} and La{sub 2}CoO{sub 4.0+{delta}}. In situ X-ray diffraction and neutrons study; Reactivite, structure et proprietes physiques de SrCoO{sub 2.5+{delta}} et La{sub 2}CoO{sub 4.0+{delta}}. Etude par diffraction des rayons X et des neutrons in situ

    Energy Technology Data Exchange (ETDEWEB)

    Le Toquin, R.

    2003-11-15

    This work was devoted to the study of the reactivity and more specifically the influence of the intercalated oxygen amount {delta} on the structure and physical properties of SrCoO{sub 2.5+{delta}} et La{sub 2}CoO{sub 4.0+{delta}} We controlled the oxidation level by means of reversible electrochemical red ox reaction at room temperature. Structural modifications, especially disorder, and electronic properties were studied for the first time on large orientated single crystal. In the SrCoO{sub 2.5+{delta}} system, after structural and electronic characterisation of the end phases, we studied the real structure of the brownmillerite SrCoO{sub 2.5} phase using single crystal. Moreover, we investigated structural and magnetic evolution upon red ox cycle using X-ray diffraction on 6 times twinned single crystal and in situ neutron powder diffraction. Two intermediate SrCoO{sub 2.75} and SrCoO{sub 2.82} phases have been observed. The reaction on single crystal has evidenced the evolution of domain structure. For the La{sub 2}CoO{sub 4+{delta}} system, we synthesised a large variety of single crystal with stoichiometry {delta} 0.0, 0.09, 0.12, 0.16, 0.20 and 0.25. Using single crystal X-ray and neutron diffraction, we showed a disorder-order transition of the apical and interstitial oxygen for the higher {delta} values. (author)

  2. Neutron-diffraction measurements of stress

    International Nuclear Information System (INIS)

    Holden, T.M.

    1995-01-01

    Experiments on bent steam-generator tubing have shown that different diffraction peaks, (1 1 1) or (0 0 2), give different results for the sign and magnitude of the stress and strain. From an engineering standpoint, the macroscopic stress field cannot be both positive and negative in the same volume, so this difference must be due to intergranular effects superposed on the macroscopic stress field. Uniaxial tensile test experiments with applied stresses beyond the 0.2% offset yield stress, help to understand this anomaly, by demonstrating the different strain response to applied stress along different crystallographic axes.When Zr-alloys are cooled from elevated temperatures, thermal stresses always develop, so that it is difficult to obtain a stress-free lattice spacing from which residual strains may be derived. From measurements of the temperature dependence of lattice spacing, the temperature at which the thermal stresses vanish may be found. From the lattice spacing at this temperature the stress-free lattice spacings at room temperature can be obtained readily.To interpret the measured strains in terms of macroscopic stress fields it is necessary to know the diffraction elastic constants. Neutron diffraction measurements of the diffraction elastic constants in a ferritic steel for the [1 1 0], [0 0 2] and [2 2 2] crystallographic axes, in directions parallel and perpendicular to the applied stress are compared with theoretical diffraction elastic constants. (orig.)

  3. Zeolite function studied by neutron diffraction

    International Nuclear Information System (INIS)

    Newsam, J.M.

    1988-01-01

    Some recent figures relating to industrial uses of zeolites are summarized. Recent advances in the application of neutron diffraction to zeolite science are overviewed, with particular emphasis on powder diffraction (PND) results. Single crystal neutron diffraction studies of some 17 hydrated natural and synthetic zeolites have now appeared and they provide a consistent picture of zeolite-water interactions. Complete PND studies of hydrated synthetic ABW- and SOD-framework zeolites have also been reported. Other PND studies have explored the structural consequences of non-framework cation exchange, of framework modification by dealumination, and of framework cation substitution. Relatively simple zeolite-hydrocarbon sorbate complexes that have been studied include benzene in zeolite Y, and benzene and pyridine in zeolite L. Areas that are well poised for further development include further extensions to lower symmetry systems, the use of PND data for zeolite structure solution, studies at elevated temperatures and pressures, and further studies of zeolite sorbate complexes. (author) 68 refs., 7 figs

  4. Workshop on industrial application of neutron diffraction. Stress measurement by neutron diffraction

    CERN Document Server

    Minakawa, N; Morii, Y; Oyama, Y

    2002-01-01

    This workshop was planned to make use of the neutron from the reactor and the pulse neutron source JSNS for the industrial world. Especially, this workshop focused on the stress measurement by the neutron diffraction and it was held on the Tokai JAERI from October 15 to 16, 2001. The participant total was 93 and 40 participated from the industrial world. The introduction of the residual stress development of measurement technique by the neutron diffraction method and a research of the measurement of the residual stress such as the nuclear reactor material, the ordinary structure material, the composite material, the quenching steel, the high strength material were presented and discussed in this workshop. Moreover, it was introduced for the industrial world that an internal stress measurement is important for development of new product or an improvement of a manufacturing process. The question from the industrial world about which can be measured the product form, the size, the measurement precision, the reso...

  5. Neutron diffraction studies of magnetic materials

    International Nuclear Information System (INIS)

    James, W.J.

    1987-01-01

    The ability of neutron diffraction in determining the nature and extent of magnetic ordering is illustrated for the intermetallic compounds, Y/sub 6/(Fe,Mn)/sub 23/ and ErFe/sub 3/. Substitution with other 3d transition metals influences the Fe-Fe exchange forces such as to alter, sometimes considerably, the magnetic properties, e.g., local site magnetic anisotropies in Er)Fe,Ni)/sub 3/ and thermal expansion anomalies in the R/sub 2/)Fe,Co)/sub 14/B compounds. When the 3d atoms are near neighbors in the periodic chart, their nuclear scattering lengths for neutrons are sufficiently different to permit the detection of preferential occupation of the several nonequivalent crystallographic 3d metal sites, i.e., atomic ordering, present in the R/sub 6/M/sub 23/, and R/sub 2/Fe/sub 14/B structures

  6. Status of the Neutron Imaging and Diffraction Instrument IMAT

    Science.gov (United States)

    Kockelmann, Winfried; Burca, Genoveva; Kelleher, Joe F.; Kabra, Saurabh; Zhang, Shu-Yan; Rhodes, Nigel J.; Schooneveld, Erik M.; Sykora, Jeff; Pooley, Daniel E.; Nightingale, Jim B.; Aliotta, Francesco; Ponterio, Rosa C.; Salvato, Gabriele; Tresoldi, Dario; Vasi, Cirino; McPhate, Jason B.; Tremsin, Anton S.

    A cold neutron imaging and diffraction instrument, IMAT, is currently being constructed at the ISIS second target station. IMAT will capitalize on time-of-flight transmission and diffraction techniques available at a pulsed neutron source. Analytical techniques will include neutron radiography, neutron tomography, energy-selective neutron imaging, and spatially resolved diffraction scans for residual strain and texture determination. Commissioning of the instrument will start in 2015, with time-resolving imaging detectors and two diffraction detector prototype modules. IMAT will be operated as a user facility for material science applications and will be open for developments of time-of-flight imaging methods.

  7. Time-resolved Neutron Powder Diffraction

    International Nuclear Information System (INIS)

    Pannetier, J.

    1986-01-01

    The use of a high-flux neutron source together with a large position sensitive detector (PSD) allows a powder diffraction pattern to be recorded at a time-scale of a few minutes so that crystalline systems under non-equilibrium conditions may now conveniently be investigated. This introduces a new dimension into powder diffraction (the time and transient phenomena like heterogeneous chemical reactions can now be easily studied. The instrumental parameters relevant for the design of such time-dependent experiments are briefly surveyed and the current limits of the method are discussed. The applications are illustrated by two kinds of experiment in the field of inorganic solid state chemistry: true kinetic studies of heterogeneous chemical reactions and thermodiffractometry experiments

  8. High resolution Neutron and Synchrotron Powder Diffraction

    International Nuclear Information System (INIS)

    Hewat, A.W.

    1986-01-01

    The use of high-resolution powder diffraction has grown rapidly in the past years, with the development of Rietveld (1967) methods of data analysis and new high-resolution diffractometers and multidetectors. The number of publications in this area has increased from a handful per year until 1973 to 150 per year in 1984, with a ten-year total of over 1000. These papers cover a wide area of solid state-chemistry, physics and materials science, and have been grouped under 20 subject headings, ranging from catalysts to zeolites, and from battery electrode materials to pre-stressed superconducting wires. In 1985 two new high-resolution diffractometers are being commissioned, one at the SNS laboratory near Oxford, and one at the ILL in Grenoble. In different ways these machines represent perhaps the ultimate that can be achieved with neutrons and will permit refinement of complex structures with about 250 parameters and unit cell volumes of about 2500 Angstrom/sp3/. The new European Synchotron Facility will complement the Grenoble neutron diffractometers, and extend the role of high-resolution powder diffraction to the direct solution of crystal structures, pioneered in Sweden

  9. Neutron diffraction studies of thin film multilayer structures

    International Nuclear Information System (INIS)

    Majkrzak, C.F.

    1985-01-01

    The application of neutron diffraction methods to the study of the microscopic chemical and magnetic structures of thin film multilayers is reviewed. Multilayer diffraction phenomena are described in general and in particular for the case in which one of the materials of a bilayer is ferromagnetic and the neutron beam polarized. Recent neutron diffraction measurements performed on some interesting multilayer systems are discussed. 70 refs., 5 figs

  10. In-situ time-of-flight neutron diffraction study of the structure evolution of electrode materials in a commercial battery with LiNi0.8Co0.15Al0.05O2 cathode

    Science.gov (United States)

    Bobrikov, I. A.; Samoylova, N. Yu.; Sumnikov, S. V.; Ivanshina, O. Yu.; Vasin, R. N.; Beskrovnyi, A. I.; Balagurov, A. M.

    2017-12-01

    A commercial lithium-ion battery with LiNi0.8Co0.15Al0.05O2 (NCA) cathode has been studied in situ using high-intensity and high-resolution neutron diffraction. Structure and phase composition of the battery electrodes have been probed during charge-discharge in different cycling modes. The dependence of the anode composition on the charge rate has been determined quantitatively. Different kinetics of Li (de)intercalation in the graphite anode during charge/discharge process have been observed. Phase separation of the cathode material has not been detected in whole voltage range. Non-linear dependencies of the unit cell parameters, atomic and layer spacing on the lithium content in the cathode have been observed. Measured dependencies of interatomic spacing and interlayer spacing, and unit cell parameters of the cathode structure on the lithium content could be qualitatively explained by several factors, such as variations of oxidation state of cation in oxygen octahedra, Coulomb repulsion of oxygen layers, changes of average effective charge of oxygen layers and van der Waals interactions between MeO2-layers at high level of the NCA delithiation.

  11. Pulsed Neutron Powder Diffraction for Materials Science

    Science.gov (United States)

    Kamiyama, T.

    2008-03-01

    The accelerator-based neutron diffraction began in the end of 60's at Tohoku University which was succeeded by the four spallation neutron facilities with proton accelerators at the High Energy Accelerator Research Organization (Japan), Argonne National Laboratory and Los Alamos Laboratory (USA), and Rutherford Appleton Laboratory (UK). Since then, the next generation source has been pursued for 20 years, and 1MW-class spallation neutron sources will be appeared in about three years at the three parts of the world: Japan, UK and USA. The joint proton accelerator project (J-PARC), a collaborative project between KEK and JAEA, is one of them. The aim of the talk is to describe about J-PARC and the neutron diffractometers being installed at the materials and life science facility of J-PARC. The materials and life science facility of J-PARC has 23 neutron beam ports and will start delivering the first neutron beam of 25 Hz from 2008 May. Until now, more than 20 proposals have been reviewed by the review committee, and accepted proposal groups have started to get fund. Those proposals include five polycrystalline diffractometers: a super high resolution powder diffractometer (SHRPD), a 0.2%-resolution powder diffractometer of Ibaraki prefecture (IPD), an engineering diffractometers (Takumi), a high intensity S(Q) diffractometer (VSD), and a high-pressure dedicated diffractometer. SHRPD, Takumi and IPD are being designed and constructed by the joint team of KEK, JAEA and Ibaraki University, whose member are originally from the KEK powder group. These three instruments are expected to start in 2008. VSD is a super high intensity diffractometer with the highest resolution of Δd/d = 0.3%. VSD can measure rapid time-dependent phenomena of crystalline materials as well as glass, liquid and amorphous materials. The pair distribution function will be routinely obtained by the Fourier transiformation of S(Q) data. Q range of VSD will be as wide as 0.01 Å-1stress mapping inside

  12. Bainitic transformation behavior studied by simultaneous neutron diffraction and dilatometric measurement

    International Nuclear Information System (INIS)

    Koo, Minseo; Xu, Pingguang; Tomota, Yo; Suzuki, Hiroshi

    2009-01-01

    Bainitic transformation behavior has firstly been observed using in situ neutron diffraction with an angular dispersive method for a hard bainite steel. The dilatometric measurement was carried out simultaneously with the neutron experiment where changes in (1 1 1) austenite and (1 1 0) ferrite diffraction profiles were monitored during heating, cooling and holding at a transformation temperature. The neutron experiments results agree with dilatometry results. They appear to have found that the austenite peak broadening occurs after the onset of bainitic transformation but not before.

  13. The peak in neutron powder diffraction

    International Nuclear Information System (INIS)

    Laar, B. van; Yelon, W.B.

    1984-01-01

    For the application of Rietveld profile analysis to neutron powder diffraction data a precise knowledge of the peak profile, in both shape and position, is required. The method now in use employs a Gaussian shaped profile with a semi-empirical asymmetry correction for low-angle peaks. The integrated intensity is taken to be proportional to the classical Lorentz factor calculated for the X-ray case. In this paper an exact expression is given for the peak profile based upon the geometrical dimensions of the diffractometer. It is shown that the asymmetry of observed peaks is well reproduced by this expression. The angular displacement of the experimental profile with respect to the nominal Bragg angle value is larger than expected. Values for the correction to the classical Lorentz factor for the integrated intensity are given. The exact peak profile expression has been incorporated into a Rietveld profile analysis refinement program. (Auth.)

  14. Dynamical neutron diffraction by curved crystals in the Laue geometry

    International Nuclear Information System (INIS)

    Albertini, G.; Melone, S.; Lagomarsino, S.; Mazkedian, S.; Puliti, P.; Rustichelli, F.

    1977-01-01

    The Taupin dynamical theory of X-ray diffraction by deformed crystals which was previously extended to the neutron diffraction by curved crystals in the Bragg geometry, is applied to calculate neutron diffraction patterns in the Laue geometry. The theoretical results are compared with experimental data on curved silicon crystals. The agreement is quite satisfactory. In the second part a simple model recently presented to describe neutron diffraction properties in the Bragg case is extended to the Laue case. The predictions of such a model are in satisfactory agreement with the rigorous theory and the experimental results. (author)

  15. A new bridge technique for neutron tomography and diffraction measurements

    International Nuclear Information System (INIS)

    Burca, G.; James, J.A.; Kockelmann, W.; Fitzpatrick, M.E.; Zhang, S.Y.; Hovind, J.; Langh, R. van

    2011-01-01

    An attractive feature of neutron techniques is the ability to identify hidden materials and structures inside engineering components and objects of art and archaeology. Bearing this in mind we are investigating a new technique, 'Tomography Driven Diffraction' (TDD), that exploits tomography data to guide diffraction experiments on samples with complex structures and shapes. The technique can be used utilising combinations of individual tomography and diffraction instruments, such as NEUTRA (PSI, CH) and ENGIN-X (ISIS, UK), but is also suitable for new combined imaging and diffraction instruments such as the JEEP synchrotron engineering instrument (DIAMOND, UK) and the proposed IMAT neutron imaging and diffraction instrument (ISIS, UK).

  16. Phase stability study of Bi0.15Sr0.85-xAexCoO3-δ (x = 0 and Ae = Ba0.28; Ca0.17) perovskites by in-situ neutron diffraction

    International Nuclear Information System (INIS)

    Eriksson, A.K.; Eriksson, S.G.; Chapon, L.C.; Knee, C.S.

    2010-01-01

    The oxygen deficient perovskites, Bi 0.15 Sr 0.85-x Ae x CoO 3-δ , x = 0 and Ae x = Ba 0.28 , Ca 0.17 , were studied with in-situ neutron powder diffraction and combined TGA/DSC in order to investigate their behaviour at elevated temperatures in oxidising conditions. The phase stability of the I4/mmm supercell structure adopted by Bi 0.15 Sr 0.85 CoO 3-δ is shown to be dependent on temperature and the oxygen content of the phase, with three structural events, at T ∼ 250, 590 and 880 o C, detected. The first transition occurs as the perovskite supercell vanishes due to oxygen absorption; the second transition is also associated with oxidation and involves the decomposition of the perovskite phase via an exothermic process to yield a dominant hexagonal phase. Finally, at T ∼ 900 o C the perovskite phase re-forms. For the Ba and Ca containing materials the decomposition to the hexagonal phase occurs at T ∼ 600 o C and ∼ 650 o C respectively. The presence of Ca at the A-site is found to stabilise the I4/mmm supercell structure in the range RT - 650 o C. The antiferromagnetic to paramagnetic transitions occur at T N ∼ 250 o C, T N ∼ 175 o C and T N ∼ 145 o C for the samples with Ae x = Ba 0.28 , x = 0 and Ae x = Ca 0.17 , respectively.

  17. Experimental technique of stress analyses by neutron diffraction

    International Nuclear Information System (INIS)

    Sun, Guangai; Chen, Bo; Huang, Chaoqiang

    2009-09-01

    The structures and main components of neutron diffraction stress analyses spectrometer, SALSA, as well as functions and parameters of each components are presented. The technical characteristic and structure parameters of SALSA are described. Based on these aspects, the choice of gauge volume, method of positioning sample, determination of diffraction plane and measurement of zero stress do are discussed. Combined with the practical experiments, the basic experimental measurement and the related settings are introduced, including the adjustments of components, pattern scattering, data recording and checking etc. The above can be an instruction for stress analyses experiments by neutron diffraction and neutron stress spectrometer construction. (authors)

  18. Polarised neutron diffraction studies on weak ferromagnetism - a survey

    International Nuclear Information System (INIS)

    Radhakrishna, P.

    1982-10-01

    The physical basis of the phenomenon of weak ferromagnetism in certain antiferromagnetic insulators is briefly discussed. A survey of the contributions of polarised neutron diffraction towards the elucidation of different aspects of this field is presented

  19. Future directions in high-pressure neutron diffraction

    Science.gov (United States)

    Guthrie, M.

    2015-04-01

    The ability to manipulate structure and properties using pressure has been well known for many centuries. Diffraction provides the unique ability to observe these structural changes in fine detail on lengthscales spanning atomic to nanometre dimensions. Amongst the broad suite of diffraction tools available today, neutrons provide unique capabilities of fundamental importance. However, to date, the growth of neutron diffraction under extremes of pressure has been limited by the weakness of available sources. In recent years, substantial government investments have led to the construction of a new generation of neutron sources while existing facilities have been revitalized by upgrades. The timely convergence of these bright facilities with new pressure-cell technologies suggests that the field of high-pressure (HP) neutron science is on the cusp of substantial growth. Here, the history of HP neutron research is examined with the hope of gleaning an accurate prediction of where some of these revolutionary capabilities will lead in the near future. In particular, a dramatic expansion of current pressure-temperature range is likely, with corresponding increased scope for extreme-conditions science with neutron diffraction. This increase in coverage will be matched with improvements in data quality. Furthermore, we can also expect broad new capabilities beyond diffraction, including in neutron imaging, small angle scattering and inelastic spectroscopy.

  20. Investigation of Acrylic Acid at High Pressure using Neutron Diffraction

    DEFF Research Database (Denmark)

    Johnston, Blair F.; Marshall, William G.; Parsons, Simon

    2014-01-01

    This article details the exploration of perdeuterated acrylic acid at high pressure using neutron diffraction. The structural changes that occur in acrylic acid-d4 are followed via diffraction and rationalised using the Pixel method. Acrylic acid undergoes a reconstructive phase transition to a new...

  1. In situ X-ray powder diffraction, synthesis, and magnetic properties of InVO 3

    Science.gov (United States)

    Lundgren, Rylan J.; Cranswick, Lachlan M. D.; Bieringer, Mario

    2006-12-01

    We report the first synthesis and high-temperature in situ X-ray diffraction study of InVO 3. Polycrystalline InVO 3 has been prepared via reduction of InVO 4 using a carbon monoxide/carbon dioxide buffer gas. InVO 3 crystallizes in the bixbyite structure in space group Ia-3 (206) with a=9.80636(31) Å with In 3+/V 3+ disorder on the (8 b) and (24 d) cation sites. In situ powder X-ray diffraction experiments and thermal gravimetric analysis in a CO/CO 2 buffer gas revealed the existence of the metastable phase InVO 3. Bulk samples with 98.5(2)% purity were prepared using low-temperature reduction methods. The preparative methods limited the crystallinity of this new phase to approximately 225(50) Å. Magnetic susceptibility and neutron diffraction experiments suggest a spin-glass ground state for InVO 3.

  2. Prospect for application of compact accelerator-based neutron source to neutron engineering diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Ikeda, Yoshimasa, E-mail: yoshimasa.ikeda@riken.jp [Center for Advanced Photonics, RIKEN, Wako, Saitama 351-0198 (Japan); Taketani, Atsushi; Takamura, Masato; Sunaga, Hideyuki [Center for Advanced Photonics, RIKEN, Wako, Saitama 351-0198 (Japan); Kumagai, Masayoshi [Faculty of Engineering, Tokyo City University, Setagaya, Tokyo 158-8857 (Japan); Oba, Yojiro [Research Reactor Institute, Kyoto University, Kumatori, Osaka 590-0494 (Japan); Otake, Yoshie [Center for Advanced Photonics, RIKEN, Wako, Saitama 351-0198 (Japan); Suzuki, Hiroshi [Materials Sciences Research Center, Japan Atomic Energy Agency, Tokai, Ibaraki 319-1195 (Japan)

    2016-10-11

    A compact accelerator-based neutron source has been lately discussed on engineering applications such as transmission imaging and small angle scattering as well as reflectometry. However, nobody considers using it for neutron diffraction experiment because of its low neutron flux. In this study, therefore, the neutron diffraction experiments are carried out using Riken Accelerator-driven Compact Neutron Source (RANS), to clarify the capability of the compact neutron source for neutron engineering diffraction. The diffraction pattern from a ferritic steel was successfully measured by suitable arrangement of the optical system to reduce the background noise, and it was confirmed that the recognizable diffraction pattern can be measured by a large sampling volume with 10 mm in cubic for an acceptable measurement time, i.e. 10 min. The minimum resolution of the 110 reflection for RANS is approximately 2.5% at 8 μs of the proton pulse width, which is insufficient to perform the strain measurement by neutron diffraction. The moderation time width at the wavelength corresponding to the 110 reflection is estimated to be approximately 30 μs, which is the most dominant factor to determine the resolution. Therefore, refinements of the moderator system to decrease the moderation time by decreasing a thickness of the moderator or by applying the decoupler system or application of the angular dispersive neutron diffraction technique are important to improve the resolution of the diffraction experiment using the compact neutron source. In contrast, the texture evolution due to plastic deformation was successfully observed by measuring a change in the diffraction peak intensity by RANS. Furthermore, the volume fraction of the austenitic phase in the dual phase mock specimen was also successfully evaluated by fitting the diffraction pattern using a Rietveld code. Consequently, RANS has been proved to be capable for neutron engineering diffraction aiming for the easy access

  3. An automatic control unit for A neutron diffraction crystal spectrometer

    International Nuclear Information System (INIS)

    Adib, M.; Abbas, Y.; Mostafa, M.; Hamouda, I.

    1982-01-01

    An automatic transistorized unit has been designed and constructed to control the operation of the double axis crystal spectrometer installed in front of one of the horizontal channels of the ET-RR-1 reactor. The function of the automatic unit is to store the diffracted neutrons at a certain angle with respect to the direction of the incident neutron beam in a selected channel of a 1024-multichannel analyzer for a certain preadjusted time period. AT the end of this time period the unit rotates the spectrometer's arm to another angle, selects the next channel of the MCA and provides the measurement of the diffracted neutron for the same time period. Such a sequence is repeated automatically over all angles required for the neutron diffraction pattern of the sample under investigation. As a result, the stored information at the MCA provides the neutron diffraction pattern as a function of channel number, where each channel corresponds to a certain scattering angle. The stored distribution at MCA can be obtained through the analyzer read out unit. The designed automatic unit has the possibility of providing the neutron diffraction pattern using a 6-digit scaler and a printer

  4. Automatic control unit for A neutron diffraction crystal spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Adib, M.; Abbas, Y.; Mostafa, M.; Hamouda, I.

    1982-01-01

    An automatic transistorized unit has been designed and constructed to control the operation of the double axis crystal spectrometer installed in front of one of the horizontal channels of the ET-RR-1 reactor. The function of the automatic unit is to store the diffracted neutrons at a certain angle with respect to the direction of the incident neutron beam in a selected channel of a 1024-multichannel analyzer for a certain preadjusted time period. AT the end of this time period the unit rotates the spectrometer's arm to another angle, selects the next channel of the MCA and provides the measurement of the diffracted neutron for the same time period. Such a sequence is repeated automatically over all angles required for the neutron diffraction pattern of the sample under investigation. As a result, the stored information at the MCA provides the neutron diffraction pattern as a function of channel number, where each channel corresponds to a certain scattering angle. The stored distribution at MCA can be obtained through the analyzer read out unit. The designed automatic unit has the possibility of providing the neutron diffraction pattern using a 6-digit scaler and a printer.

  5. Diffraction and single-crystal elastic constants of Inconel 625 at room and elevated temperatures determined by neutron diffraction

    International Nuclear Information System (INIS)

    Wang, Zhuqing; Stoica, Alexandru D.; Ma, Dong; Beese, Allison M.

    2016-01-01

    In this work, diffraction and single-crystal elastic constants of Inconel 625 have been determined by means of in situ loading at room and elevated temperatures using time-of-flight neutron diffraction. Theoretical models proposed by Voigt, Reuss, and Kroner were used to determine single-crystal elastic constants from measured diffraction elastic constants, with the Kroner model having the best ability to capture experimental data. The magnitude of single-crystal elastic moduli, computed from single-crystal elastic constants, decreases and the single crystal anisotropy increases as temperature increases, indicating the importance of texture in affecting macroscopic stress at elevated temperatures. The experimental data reported here are of great importance in understanding additive manufacturing of metallic components as: diffraction elastic constants are required for computing residual stresses from residual lattice strains measured using neutron diffraction, which can be used to validate thermomechanical models of additive manufacturing, while single-crystal elastic constants can be used in crystal plasticity modeling, for example, to understand mechanical deformation behavior of additively manufactured components.

  6. Diffraction and single-crystal elastic constants of Inconel 625 at room and elevated temperatures determined by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Zhuqing [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States); Stoica, Alexandru D. [Chemical and Engineering Materials Division, Neutron Sciences Directorate, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Ma, Dong, E-mail: dongma@ornl.gov [Chemical and Engineering Materials Division, Neutron Sciences Directorate, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Beese, Allison M., E-mail: amb961@psu.edu [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States)

    2016-09-30

    In this work, diffraction and single-crystal elastic constants of Inconel 625 have been determined by means of in situ loading at room and elevated temperatures using time-of-flight neutron diffraction. Theoretical models proposed by Voigt, Reuss, and Kroner were used to determine single-crystal elastic constants from measured diffraction elastic constants, with the Kroner model having the best ability to capture experimental data. The magnitude of single-crystal elastic moduli, computed from single-crystal elastic constants, decreases and the single crystal anisotropy increases as temperature increases, indicating the importance of texture in affecting macroscopic stress at elevated temperatures. The experimental data reported here are of great importance in understanding additive manufacturing of metallic components as: diffraction elastic constants are required for computing residual stresses from residual lattice strains measured using neutron diffraction, which can be used to validate thermomechanical models of additive manufacturing, while single-crystal elastic constants can be used in crystal plasticity modeling, for example, to understand mechanical deformation behavior of additively manufactured components.

  7. High temperature neutron diffraction study of LaPO4

    International Nuclear Information System (INIS)

    Mishra, S.K.; Mittal, R.; Ningthoujam, R.S.; Vatsa, R.K.; Hansen, T.

    2016-01-01

    We report high temperature powder neutron diffractions study in LaPO 4 using high-flux D20 neutron diffractometer in the Institut Laue-Langevin, France. The measurements were carried out in high resolution mode (incident neutron wavelength 1.36 A) at various temperature upto 900°C. CarefuI inspection of temperature dependence of diffraction data showed appearance and disappearance of certain Bragg's reflections above 1273 K. It is a signature of structural phase transition. Rietveld refinement of the powder diffraction data revealed that diffraction patterns at and above 800°C could be indexed using the monoclinic structure with P21/n space group. Detail analysis for identify the water molecules is under investigation. (author)

  8. In-Situ Neutron Diffraction Under Tensile Loading of Powder-in-Tube Cu/Nb$_{3}$Sn Composite Wires Effect of Reaction Heat Treatment on Texture, Internal Stress State and Load Transfer

    CERN Document Server

    Scheuerlein, C; Thilly, L

    2007-01-01

    The strain induced degradation of Nb$_{3}$Sn superconductors can hamper the performance of high field magnets. We report elastic strain measurements in the different phases of entire non-heat treated and fully reacted Nb$_{3}$Sn composite strands as a function of uniaxial stress during in-situ deformation under neutron beam. After the reaction heat treatment the Cu matrix loses entirely its load carrying capability and the applied stress is transferred to the remaining Nb-Ta alloy and to the brittle (Nb-Ta)3Sn phase, which exhibits a preferential grain orientation parallel to the strand axis.

  9. Extinction correction in white X-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Tomiyoshi, S.; Yamada, M.; Watanabe, H.

    1980-01-01

    Extinction effects in white-beam X-ray and neutron diffraction are considered. In white-beam diffraction, a small deviation of the wavelength from the Bragg condition Δlambda is a variable which represents the line profile of the diffraction peaks, so that by using the new parameter Δlambda the theory is converted to one in white-beam diffraction. It is shown that for a convex crystal, primary extinction agrees with the results calculated already for monochromatic diffraction. The same relation is shown to hold in secondary extinction. It is concluded that extinction theory derived for monochromatic diffraction is applicable without any modification in white-beam diffraction. (Auth.)

  10. Structure and texture investigations by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Vratislav, S [Ceske Vysoke Uceni Technicke, Prague (Czechoslovakia). Fakulta Jaderna a Fysikalne Inzenyrska

    1982-01-01

    Analysis of the KSN-2 neutron diffractometer parameters helped improve the KSN-2 resolution to 7.5x10/sup -3/. Structure analysis of compounds with elementary cell volume down to 5 nm/sup 3/ can now be performed. Resolution analysis of the neutron powder diffractometer and its conclusions are described, results of the structure determination of zeolites and the magnetic structure determination of perovskites are given. The three-dimensional distribution function and its use in calculating the elastic modulus of aluminium sheets are mentioned.

  11. Neutron diffraction study of the stress distribution in steel matrix around active NiTi inserts

    Czech Academy of Sciences Publication Activity Database

    Davydov, Vadim; Lukáš, Petr; Vrána, Miroslav; Malard, B.; Pilch, Jan; Maximov, V.; Šittner, Petr

    2010-01-01

    Roč. 527, č. 15 (2010), s. 3310-3316 ISSN 0921-5093 R&D Projects: GA ČR GAP107/10/0824; GA AV ČR(CZ) IAA200100627 Institutional research plan: CEZ:AV0Z10480505; CEZ:AV0Z10100520 Keywords : In-situ neutron diffraction * Shape memory alloys * Residual stresses Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 2.090, year: 2010

  12. Thermal diffuse scattering in angular-dispersive neutron diffraction

    International Nuclear Information System (INIS)

    Popa, N.C.; Willis, B.T.M.

    1998-01-01

    The theoretical treatment of one-phonon thermal diffuse scattering (TDS) in single-crystal neutron diffraction at fixed incident wavelength is reanalysed in the light of the analysis given by Popa and Willis [Acta Cryst. (1994), (1997)] for the time-of-flight method. Isotropic propagation of sound with different velocities for the longitudinal and transverse modes is assumed. As in time-of-flight diffraction, there exists, for certain scanning variables, a forbidden range in the one-phonon TDS of slower-than-sound neutrons, and this permits the determination of the sound velocity in the crystal. A fast algorithm is given for the TDS correction of neutron diffraction data collected at a fixed wavelength: this algorithm is similar to that reported earlier for the time-of-flight case. (orig.)

  13. Neutron diffraction measurements of residual stresses in NPP construction materials

    International Nuclear Information System (INIS)

    Hinca, R.; Bokuchava, G.

    2001-01-01

    Neutron diffraction is one of the most powerful methods for condensed matter studies. This method is used for non-destructive determination of residual stresses in material. The fundamental aspects of neutron diffraction are discussed, together with a brief description of the experimental facility. The principal advantage of using neutrons rather than the more conventional X-rays is the fact that neutron can penetrate deeply (2-4 cm for steel and more than 10 cm for aluminium) into metals to determine internal parameters within the bulk of materials. We present results of measurements residual stresses in NPP construction material - austenitic stainless steel (Cr-18%, Ni-10%, Ti-1%) coated with high-nickel alloy. (authors)

  14. The structure of pumice by neutron diffraction

    International Nuclear Information System (INIS)

    Floriano, M.A.; Venezia, A.M.; Deganello, G.; Svensson, E.C.; Root, J.H.

    1994-01-01

    Small-angle neutron scattering (SANS) and wide-angle neutron scattering (WANS) measurements on pumice, an amorphous natural aluminosilicate used as support for metals in the preparation of catalysts, are reported. The SANS spectrum indicates the presence of a broad size distribution of pores and the absence of volume fractality. Surface fractality, however, cannot be ruled out. The structure of pumice, suggested by the pair-correlation function derived from the WANS spectrum and simulated by a random-network structure model, is very similar to that of vitreous silica, consisting mainly of SiO 4- 4 tetrahedra interconnected by bridging O atoms with additional local disorder generated by the replacement, on average, of one in ten Si atoms by aluminium. (orig.)

  15. High pressure neutron powder diffraction at LANSCE

    International Nuclear Information System (INIS)

    Von Dreele, R.B.

    1994-01-01

    By making use of the recently developed ''Paris-Edinburgh'' high pressure cell, the author has successfully performed neutron powder experiments to 10GPa at ambient temperature. Results for the structural compression of the high Tc 1223-Hg superconductor to 9.2 GPa, the compression and possible hydrogen bond formation in brucite, Mg(OD) 2 , to 9.3 GPa, and the molecular reorientation in nitromethane to 5.5 GPa will be presented

  16. Applications of neutron powder diffraction in materials research

    International Nuclear Information System (INIS)

    Kennedy, S.J.

    1996-01-01

    The aim of this article is to provide an overview of the applications of neutron powder diffraction in materials science. The technique is introduced with particular attention to comparison with the X-ray powder diffraction technique to which it is complementary. The diffractometers and special environment ancillaries operating around the HIFAR research reactor at the Australian Nuclear Science and Technology Organisation (ANSTO) are described. Applications of the technique which the advantage of the unique properties of thermal neutrons have been selected from recent materials studies undertaken at ANSTO

  17. Maximizing Macromolecule Crystal Size for Neutron Diffraction Experiments

    Science.gov (United States)

    Judge, R. A.; Kephart, R.; Leardi, R.; Myles, D. A.; Snell, E. H.; vanderWoerd, M.; Curreri, Peter A. (Technical Monitor)

    2002-01-01

    A challenge in neutron diffraction experiments is growing large (greater than 1 cu mm) macromolecule crystals. In taking up this challenge we have used statistical experiment design techniques to quickly identify crystallization conditions under which the largest crystals grow. These techniques provide the maximum information for minimal experimental effort, allowing optimal screening of crystallization variables in a simple experimental matrix, using the minimum amount of sample. Analysis of the results quickly tells the investigator what conditions are the most important for the crystallization. These can then be used to maximize the crystallization results in terms of reducing crystal numbers and providing large crystals of suitable habit. We have used these techniques to grow large crystals of Glucose isomerase. Glucose isomerase is an industrial enzyme used extensively in the food industry for the conversion of glucose to fructose. The aim of this study is the elucidation of the enzymatic mechanism at the molecular level. The accurate determination of hydrogen positions, which is critical for this, is a requirement that neutron diffraction is uniquely suited for. Preliminary neutron diffraction experiments with these crystals conducted at the Institute Laue-Langevin (Grenoble, France) reveal diffraction to beyond 2.5 angstrom. Macromolecular crystal growth is a process involving many parameters, and statistical experimental design is naturally suited to this field. These techniques are sample independent and provide an experimental strategy to maximize crystal volume and habit for neutron diffraction studies.

  18. Design and Rationale for an In Situ Cryogenic Deformation Capability at a Neutron Source

    International Nuclear Information System (INIS)

    Livescu, V.; Clausen, B.; Sisneros, T.; Bourke, M.A.M.; Woodruff, T.R.; Vaidyanathan, R.; Notardonato, W.U.

    2004-01-01

    When performed in conjunction with neutron diffraction, in situ loading offers unique insights on microstructural deformation mechanisms. This is by virtue of the penetration and phase sensitivity of neutrons. At Los Alamos National Laboratory room and high temperature (up to 1500 deg. C) polycrystalline constitutive response is modeled using finite element and self-consistent models. The models are compared to neutron diffraction measurements. In doing so the implications of slip and creep to microstructural response have been explored. Recently we have been considering low temperature phenomena. This includes changes in deformation mechanisms such as the increased predilection for twinning over slip. Since this is associated with measurable texture changes as well as microstructural strain effects, it is well suited for study using neutron diffraction. This paper outlines the design and rationale for a cryogenic loading capability that will be used on the Spectrometer for MAterials Research at Temperature and Stress (SMARTS) at the Los Alamos Neutron Science Center (LANSCE)

  19. Dynamic theory of neutron diffraction from a moving grating

    Energy Technology Data Exchange (ETDEWEB)

    Bushuev, V. A., E-mail: vabushuev@yandex.ru [Moscow State University (Russian Federation); Frank, A. I.; Kulin, G. V. [Joint Institute for Nuclear Research (Russian Federation)

    2016-01-15

    A multiwave dynamic theory of diffraction of ultracold neutrons from a moving phase grating has been developed in the approximation of coupled slowly varying amplitudes of wavefunctions. The effect of the velocity, period, and height of grooves of the grating, as well as the spectral angular distribution of the intensity of incident neurons, on the discrete energy spectrum and the intensity of diffraction reflections of various orders has been analyzed.

  20. Preferred orientations in niobium determined by neutrons diffraction

    International Nuclear Information System (INIS)

    Ueno, S.I.N.

    1979-01-01

    Neutron diffraction has been utilized to study textures developed in polycrystalline niobium, cold rolled to 60%, 80% and 95% in tickness and cold rolled to 95% in thickness and annealed at 800 0 C for 15, 30, 60 and 120 minutes in a vacuum of 10 -4 TORR [pt

  1. Neutron diffraction studies of high-T/sub c/ superconductors

    International Nuclear Information System (INIS)

    Jorgensen, J.D.

    1988-03-01

    Neutron powder diffraction techniques have been used extensively for the study of high-T/sub c/ oxide superconductors because of the need to locate oxygen atoms and accurately determine the oxygen site occupancies, and the difficulty in obtaining single crystals. For example, in the case of YBa 2 Cu 3 O/sub 7-δ/, neutron powder diffraction and Rietveld structural refinement were used to obtain the first complete structural information. Subsequent experiments focussed on determining the relationship of superconducting properties to the number and distribution of oxygen vacancies on the Cu-O sublattice with measurements being done on samples in thermodynamic equilibrium, at high temperature in controlled oxygen atmospheres, and on metastable, oxygen-deficient samples produced by quenching. Neutron powder diffraction has also been used to determine the structures of compounds in which the properties have been modified by substitution on the Y, Ba, or Cu sites. This paper briefly reviews some of the neutron powder diffraction results in these areas. 17 refs

  2. Physics and chemistry of materials from neutron diffraction and spectroscopy

    International Nuclear Information System (INIS)

    Dahlborg, U.; Lovesey, S.W.; Uppsala Univ.

    1990-11-01

    A short introduction to the powerful techniques of neutron diffraction and spectroscopy is illustrated largely with achievements by Swedish researchers in the past few years. Background material on sources and instrumentation is included, together with a directory of facilities routinely available to the Swedish scientific community. (author)

  3. Neutron diffraction on a large block mosaic crystal

    International Nuclear Information System (INIS)

    Kim Chir Sen; Nitts, V.V.

    1985-01-01

    The neutron diffraction by the mosaic single crystal with size of crystallites sufficient to achieve the primary extinction saturation is considered. Two cases where the proportionality between the reflection intensity and the structure amplitude is performed are analysed. Such a dependence is convenient for structure investigations. The difficulties connected with the accounting of the extinction are eliminated considerably

  4. Investigation of Methacrylic Acid at High Pressure Using Neutron Diffraction

    DEFF Research Database (Denmark)

    Marshall, William G.; Urquhart, Andrew; Oswald, Iain D. H.

    2015-01-01

    This article shows that pressure can be a low-intensity route to the synthesis of polymethacrylic acid. The exploration of perdeuterated methacrylic acid at high pressure using neutron diffraction reveals that methacrylic acid exhibits two polymorphic phase transformations at relatively low...

  5. Lattice strain measurements on sandstones under load using neutron diffraction

    Science.gov (United States)

    Frischbutter, A.; Neov, D.; Scheffzük, Ch.; Vrána, M.; Walther, K.

    2000-11-01

    Neutron diffraction methods (both time-of-flight- and angle-dispersive diffraction) are applied to intracrystalline strain measurements on geological samples undergoing uniaxial increasing compressional load. The experiments were carried out on Cretaceous sandstones from the Elbezone (East Germany), consisting of >95% quartz which are bedded but without crystallographic preferred orientation of quartz. From the stress-strain relation the Young's modulus for our quartz sample was determined to be (72.2±2.9) GPa using results of the neutron time-of-flight method. The influence of different kinds of bedding in sandstones (laminated and convolute bedding) could be determined. We observed differences of factor 2 (convolute bedding) and 3 (laminated bedding) for the elastic stiffness, determined with angle dispersive neutron diffraction (crystallographic strain) and with strain gauges (mechanical strain). The data indicate which geological conditions may influence the stress-strain behaviour of geological materials. The influence of bedding on the stress-strain behaviour of a laminated bedded sandstone was indicated by direct residual stress measurements using neutron time-of-flight diffraction. The measurements were carried out six days after unloading the sample. Residual strain was measured for three positions from the centre to the periphery and within two radial directions of the cylinder. We observed that residual strain changes from extension to compression in a different manner for two perpendicular directions of the bedding plane.

  6. Neutron Diffraction Investigation of MnAs under High Pressure

    DEFF Research Database (Denmark)

    Andresen, A.F; Fjellvag, H; Lebech, Bente

    1984-01-01

    Powdered MnAs has been investigated by neutron diffraction in a pressure cryostat, at hydrostatic pressures up to 13 kbar and temperatures down to 4.2 K. It has been found that in the orthorhombic MnP type structure, which under pressure is retained at low temperature, a spiral magnetic structure...

  7. Neutron diffraction experiments on ordered silver nuclei at Picokelvin temperatures

    International Nuclear Information System (INIS)

    Annila, A.J.; Hakonen, P.J.; Lounasmaa, O.V.; Nummila, K.K.; Oja, A.S.; Tuoriniemi, J.T.; Clausen, K.N.; Lindgaard, P.-A.; Siemensmeyer, K.; Steiner, M.; Weinfurter, H.; Viertioe, H.E.

    1990-08-01

    Nuclear spins in silver constitute an ideal antiferromagnetic spin - 1/2 model system in an fcc lattice. The nuclei are well localized and the interactions coupling the spins can be calculated from first principles. Strong quantum effects are expected owing to spin - 1/2. The magnetic phase diagram of the system has been investigated by several theoretical methods. In the present study the feasibility of neutron diffraction experiments on nuclear magnetic order in silver is discussed. The requirements for cryogenics and for neutron equipment are based on experience with current NMR measurements on sivler and with neutron diffraction work on copper. It is concluded that an experiment using an isotopically enriched specimen of either 107 Ag or 109 Ag is feasible but difficult. (author) 1 tab., 16 ills., 38 refs

  8. Quantitative multiphase analysis of archaeological bronzes by neutron diffraction

    CERN Document Server

    Siano, S; Celli, M; Pini, R; Salimbeni, R; Zoppi, M; Kockelmann, W A; Iozzo, M; Miccio, M; Moze, O

    2002-01-01

    In this paper, we report the first investigation on the potentials of neutron diffraction to characterize archaeological bronze artifacts. The preliminary feasibility of phase and structural analysis was demonstrated on standardised specimens with a typical bronze alloy composition. These were realised through different hardening and annealing cycles, simulating possible ancient working techniques. The Bragg peak widths that resulted were strictly dependent on the working treatment, thus providing an important analytical element to investigate ancient making techniques. The diagnostic criteria developed on the standardised specimens were then applied to study two Etruscan museum pieces. Quantitative multiphase analysis by Rietveld refinement of the diffraction patterns was successfully demonstrated. Furthermore, the analysis of patterns associated with different artifact elements also yielded evidence for some peculiar perspective of the neutron diffraction diagnostics in archeometric applications. (orig.)

  9. Deformation behavior of Mg-alloy-based composites at different temperatures studied by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Farkas, Gergely [Department of Metal Physics, Charles University, Ke Karlovu, 5, CZ-121 16 Prague (Czech Republic); Nuclear Physics Institute, v. v. i., 250 68 Řež (Czech Republic); Máthis, Kristian [Department of Metal Physics, Charles University, Ke Karlovu, 5, CZ-121 16 Prague (Czech Republic); Pilch, Ján [Nuclear Physics Institute, v. v. i., 250 68 Řež (Czech Republic); Minárik, Peter [Department of Metal Physics, Charles University, Ke Karlovu, 5, CZ-121 16 Prague (Czech Republic); Lukáš, Petr [Nuclear Physics Institute, v. v. i., 250 68 Řež (Czech Republic); Vinogradov, Alexei, E-mail: alexei.vinogradov@ntnu.no [Department of Mechanical and Industrial Engineering, Norwegian University of Science and Technology - NTNU, Trondheim N-7491 (Norway); Institute of Advanced Technologies, Togliatti State University, 445020 (Russian Federation)

    2017-02-08

    The influence of the reinforcement short Saffil fibers on the deformation behavior of Mg-Al-Ca alloy-based composite with two different fiber plane orientations is investigated and clarified using in-situ neutron diffraction at room and elevated temperatures. The measured lattice strain evolution points to a more efficient reinforcing effect of fibers at parallel fiber plane orientation, which decreases at elevated temperature. A significant decrement of compressive lattice strain was incidentally observed in the matrix in the direction of load axis when deformation due to the elevated temperature occurred. Electron microscopy revealed the influence of the temperature and fiber orientation on fiber cracking. The EBSD observations corroborated neutron diffraction results highlighting significant twin growth at elevated testing temperatures.

  10. Fabrication of vanadium cans for neutron diffraction experiments

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Chin man; Baik, Sung Hoon; Park, Sun Kyu

    1999-12-01

    The laser weld technique of vanadium developed to experiment for neutron diffraction of HANARO. The demands for this laser welding technique were applied to process control in vanadium film welding and to fabricate various sizing vanadium cans. The vanadium can had a advantage to have less coherent in neutron. KAERI developed the fabrication jig of 6-12 mm diameter cans using 0.125 mm vanadium thin film, and investigated the laser welding procedure for making the various diameter and length of vanadium cans using the fabricated jigs and Nd:YAG laser. (author)

  11. High-resolution neutron-diffraction measurements to 8 kbar

    Science.gov (United States)

    Bull, C. L.; Fortes, A. D.; Ridley, C. J.; Wood, I. G.; Dobson, D. P.; Funnell, N. P.; Gibbs, A. S.; Goodway, C. M.; Sadykov, R.; Knight, K. S.

    2017-10-01

    We describe the capability to measure high-resolution neutron powder diffraction data to a pressure of at least 8 kbar. We have used the HRPD instrument at the ISIS neutron source and a piston-cylinder design of pressure cell machined from a null-scattering titanium zirconium alloy. Data were collected under hydrostatic conditions from an elpasolite perovskite La?NiMnO?; by virtue of a thinner cell wall on the incident-beam side of the cell, it was possible to obtain data in the instrument's highest resolution back-scattering detector banks up to a maximum pressure of 8.5 kbar.

  12. Structure of amorphous selenium studied by neutron diffraction

    DEFF Research Database (Denmark)

    Hansen, Flemming Yssing; Knudsen, Torben Steen; Carneiro, K.

    1975-01-01

    Neutron diffraction measurements on amorphous selenium have been performed at 293 and 80 K. Careful analyses of the instrumental corrections were made to avoid systematic errors in the measured structure factor S (kappa) in the wave vector region 0 ? kappa ? 12 Å−1. As a result of the data...... treatment, the neutron scattering cross sections of selenium are determined to be sigmacoh = 8.4±0.1 b and sigmainc = 0.1±0.1 b. Using the fact that S (kappa) for large kappa's is determined by the short distances in the sample, a new method for extrapolation of the experimental S (kappa) until convergence....... Finally, we give a brief discussion of the different models for the structure of amorphous selenium, taking both diffraction measurements and thermodynamic considerations into account. The Journal of Chemical Physics is copyrighted by The American Institute of Physics....

  13. In situ X-ray and neutron diffraction of the Ruddlesden-Popper compounds (RE2-xSrx)0.98(Fe0.8Co0.2)1-yMgyO4-δ (RE=La, Pr): Structure and CO2 stability

    DEFF Research Database (Denmark)

    Chatzichristodoulou, Christodoulos; Hauback, B.C.; Hendriksen, Peter Vang

    2013-01-01

    The crystal structure of the Ruddlesden-Popper compounds (La 1.0Sr1.0)0.98Fe0.8Co 0.2O4-δ and (La1.2Sr0.8) 0.98(Fe0.8Co0.2)0.8Mg 0.2O4-δ was investigated at 1000 °C in N 2 (aO2=1×10-4) by in-situ powder neutron diffraction. In-situ powder X-ray diffraction (PXD) was also employed to investigate....... The equivalent pseudo-cubic thermal and chemical expansion coefficients are in agreement with values determined by dilatometry. The chemical stability in CO2 containing environments of various Ruddlesden-Popper compounds with chemical formula (RE2-xSr x)0.98(Fe0.8Co0.2) 1-yMgyO4-δ (RE=La, Pr), as well...

  14. Neutron diffraction by monocrystals of inorganic and elementary organic compounds

    International Nuclear Information System (INIS)

    Becker, G.; Hauser, H.D.

    1992-01-01

    The phase of preparation and X-ray structural analysis of the compounds has been completed following the synthetical preparation of compounds sensitive to oxidation and pyrolysis, in this case: phosphonic acid, potassium silanide, lithium dihydrogenphosphide * DME, bis[lithium-tri(tert.butyl)alanate], dibromophenylbismuthate, potassium tetrahydride aluminate, and phosphinic acid. The work was started is neutron diffraction experiments for detecting the positions of the hydrogen and carbon atoms, in order to analyse space group problems. (BBR) [de

  15. Neutron diffraction study of α-iron titanium cerium hydride

    International Nuclear Information System (INIS)

    Lin Hong; Niu Shiwen; Gou Cheng

    1987-01-01

    The results of the neutron scattering method shows that the crystal structure of Fe 0.94 TiCe 0.06 H 0.03 is the same as that of the FeTiH 0.02 . However, its diffraction peak intensities drop by 47-58%, the background increased markedly about 2 times and the lattice constant increase by 5%

  16. Practical conditions in the neutron diffraction under high pressure

    International Nuclear Information System (INIS)

    Kamigaki, Kazuo; Ohashi, Masayoshi

    1993-01-01

    Practical analysis is made on some conditions in utilizing neutrons for the study of atomistic structure of materials under high pressure. Investigation is made on the geometrical conditions; size of the specimen, width of slits, and the rate of extra-scattering. Experiments are performed on the effects of absorption by high pressure cell and the disturbance due to an overlapping of diffraction peaks. An observation is presented on the pressure-induced transformation in RbBr. (author)

  17. Neutron diffraction utilizing the T-O-F method

    Energy Technology Data Exchange (ETDEWEB)

    Niimura, N [Tohoku Univ., Sendai (Japan). Lab. of Nuclear Science

    1974-12-01

    Characteristic features of the TOF (time of flight) neutron diffraction are summarized. In this method, i) all the reciprocal points on the rod passing through the origin in the reciprocal space can be scanned by each burst of white neutrons, ii) it is easy to measure high index reflections at the large scattering angle, iii) each reflection is not affected by the higher-order harmonics, and iv) it is easy to measure the physical properties depending on the neutron wavelength. The pulse neutron generator as well as the data acquisition system in the Laboratory of Nuclear Science of Tohoku University is described. The TOF method seems to be very powerful if it is applied to accurate structure analysis. The data correction methods are discussed. The TOF method is prospective to the study of transient phenomena. In this method one can apply to the crystalline sample an external field pulsed with the same frequency as the neutrons. By using this method, the transient state of the polarization reversal of the ferroelectric NaNO/sub 2/ has been observed. The magnetically pulsed neutron TOF spectrometer is briefly introduced after a review of the chopper history.

  18. Neutron diffraction for studying the influence of the relative humidity on the carbonation process of cement pastes

    International Nuclear Information System (INIS)

    Galan, I; Andrade, C; Castellote, M; Rebolledo, N; Sanchez, J; Toro, L; Puente, I; Campo, J; Fabelo, O

    2011-01-01

    The effect of humidity on hydrated cement carbonation has been studied by means of in-situ neutron diffraction measurements. The evolution of the main crystalline phases in the bulk of the sample, portlandite and calcite, has been monitored during the process. Data obtained from neutron diffraction allow the quantification of the phases involved. The results highlight the great influence of humidity on carbonation. At very low humidity there are almost no changes. Between 53 and 75% relative humidity, portlandite decrease and calcite increase data can be fitted to exponential decay functions. At very high humidity portlandite remains nearly constant while calcite increases slightly with time, almost linearly.

  19. Residual stress measurements by means of neutron diffraction

    International Nuclear Information System (INIS)

    Pintschovius, L.; Jung, V.; Macherauch, E.; Voehringer, O.

    1983-01-01

    A new method for the analysis of multiaxial residual stress states is presented, which is based on high resolution neutron diffraction. It is analogous to X-ray stress analysis, but the use of neutrons instead of X-rays allows the analysis of the stress distributions also in the interior of technical components in a non-destructive way. To prove the feasibility of the method, investigations of the loading stress distributions of an aluminium bar subjected to purely elastic bending were performed. Limiting factors due to the volume of the internal probe region and the sample thickness are discussed. Complete neutron residual stress analyses were carried out for a plastically deformed bending bar and a transformation-free water-quenched steel cylinder. The results are in fairly good agreement with theoretical expectations and with X-ray control measurements at the surface of the objects. (Auth.)

  20. Engineering related neutron diffraction measurements probing strains, texture and microstructure

    Energy Technology Data Exchange (ETDEWEB)

    Clausen, Bjorn [Los Alamos National Laboratory; Brown, Donald W [Los Alamos National Laboratory; Tome, Carlos N [Los Alamos National Laboratory; Balogh, Levente [Los Alamos National Laboratory; Vogel, Sven C [Los Alamos National Laboratory

    2010-01-01

    Neutron diffraction has been used for engineering applications for nearly three decades. The basis of the technique is powder diffraction following Bragg's Law. From the measured diffraction patterns information about internal, or residual, strain can be deduced from the peak positions, texture information can be extracted from the peak intensities, and finally the peak widths can provide information about the microstructure, e.g. dislocation densities and grain sizes. The strains are measured directly from changes in lattice parameters, however, in many cases it is non-trivial to determine macroscopic values of stress or strain from the measured data. The effects of intergranular strains must be considered, and combining the neutron diffraction measurements with polycrystal deformation modeling has proven invaluable in determining the overall stress and strain values of interest in designing and dimensioning engineering components. Furthelmore, the combined use of measurements and modeling has provided a tool for elucidating basic material properties, such as critical resolved shear stresses for the active deformation modes and their evolution as a function of applied deformation.

  1. Profile analysis of neutron powder diffraction data at ISIS

    International Nuclear Information System (INIS)

    David, W.I.F.; Ibberson, R.M.; Matthewman, J.C.

    1992-05-01

    The aim of this manual is to document the current suite of time-of-flight neutron powder diffraction profile refinement programs available to ISIS users. Aspects of data collation and normalisation specific to the individual diffraction instruments are dealt with elsewhere. It will be assumed the user has produced a suitable data file (.DAT file) containing the profile data consisting of point by point values of the corrected diffraction profile across the pattern. The analysis of neutron powder diffraction data at ISIS by profile refinement utilises a suite of ''in-house'' written and supported programs based on the Cambridge Crystallography Subroutine Library (CCSL). A quick scan through the CCSL manual will give the user a general feel for the procedure to adopt in the use of the library and hence of the profile codes. The instructions documented in this handbook are complementary to those in the more specialist CCSL manual, and consequently go into no great detail regarding technical details of any of the CCSL routines. The programs may be run from each individual user account, for example [USER01], once the appropriate login procedure has been set-up by the instrument scientists. The programs are mostly activated by one line commands and only a basic knowledge of a VAX editor should be required; details can be found in the ''VAX primer'' available from Computer Support. (Author)

  2. Location of adsorbed species in NO-reduction catalysts by high resolution neutron powder diffraction

    International Nuclear Information System (INIS)

    Fowkes, A.J.; Rosseinsky, M.J.

    1999-01-01

    Complete text of publication follows. Catalysts containing copper ion exchanged into zeolites are attracting considerable attention due to their efficiency for both NO decomposition and the selective catalytic reduction of NO x in so-called lean-burn conditions in automotive exhausts. This presentation will describe the application of in-situ high resolution neutron powder diffraction to study active sites in a Cu-zeolite Y catalyst active for NO decomposition. The study under NO pressure reveals the location of two distinct copper sites for sorption. The influence of copper oxidation state on the structure of both the pristine and NO-loaded zeolites will be discussed. (author)

  3. Refractive and diffractive neutron optics with reduced chromatic aberration

    Energy Technology Data Exchange (ETDEWEB)

    Poulsen, S.O., E-mail: stefan.poulsen@northwestern.edu [NEXMAP, Department of Physics, Technical University of Denmark, Anker Engelunds Vej 1, 2800 Kgs. Lyngby (Denmark); Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208 (United States); Poulsen, H.F. [NEXMAP, Department of Physics, Technical University of Denmark, Anker Engelunds Vej 1, 2800 Kgs. Lyngby (Denmark); Bentley, P.M. [European Spallation Source ESS AB, Box 176, 221 00 Lund (Sweden)

    2014-12-11

    Thermal neutron beams are an indispensable tool in physics research. The spatial and the temporal resolution attainable in experiments are dependent on the flux and collimation of the neutron beam which remain relatively poor, even for modern neutron sources. These difficulties may be mitigated by the use of optics for focusing and imaging. Refractive and diffractive optical elements, e.g. compound refractive lenses and Fresnel zone plates, are attractive due to their low cost, and simple alignment. These optical elements, however, suffer from chromatic aberration, which limit their effectiveness to highly monochromatic beams. This paper presents two novel concepts for focusing and imaging non-monochromatic thermal neutron beams with well-known optical elements: (1) a fast mechanical transfocator based on a compound refractive lens, which actively varies the number of individual lenses in the beam path to focus and image a time-of-flight beam, and (2) a passive optical element consisting of a compound refractive lens, and a Fresnel zone plate, which may focus and image both continuous and pulsed neutron beams.

  4. Polycrystalline deformation in engineering materials: Insights from neutron diffraction during loading

    International Nuclear Information System (INIS)

    Bourke, M.; Brown, D.

    1999-01-01

    In-situ measurements using the non-destructive penetration of neutrons are commonplace at neutron sources and permit investigations within environmental chambers at stress, pressure, or temperature. Many of these studies explore the microstructural performance of engineering materials under service conditions. For example, by measuring phase strains during the application of static loads, neutron diffraction provides insight into failure, relaxation and load transfer mechanisms. Mechanical loading of a sample on a neutron spectrometer is usually performed with a customized load frame (small enough to fit into the typically limited available space) with the load axis horizontal. Diffraction data are recorded using detectors that surround the sample and strains are determined from changes in the measured interplanar lattice spacings in directions determined by the scattering geometry. These elastic strains indicate how the applied stress is shared throughout the microstructure. During a test, conventional strain gauges also record the macroscopic strain; that is the sum of the plastic and elastic contributions. Beyond yield the plastic contribution usually dominates the total strain but the elastic phase strains respond to the applied stress at any given load and provide clues about which phase (in a multiphase system) or which crystal orientation (in a single phase polycrystal) dictates failure

  5. The adsorption of methanol and water on SAPO-34: in situ and ex situ X-ray diffraction studies

    DEFF Research Database (Denmark)

    Wragg, David S.; Johnsen, Rune; Norby, Poul

    2010-01-01

    The adsorption of methanol on SAPO-34 has been studied using a combination of in situ synchrotron powder X-ray diffraction to follow the process and ex situ high resolution powder diffraction to determine the structure. The unit cell volume of SAPO-34 is found to expand by 0.5% during methanol ad...

  6. Levitation apparatus for neutron diffraction investigations on high temperature liquids

    International Nuclear Information System (INIS)

    Hennet, Louis; Pozdnyakova, Irina; Bytchkov, Aleksei; Cristiglio, Viviana; Palleau, Pierre; Fischer, Henry E.; Cuello, Gabriel J.; Johnson, Mark; Melin, Philippe; Zanghi, Didier; Brassamin, Severine; Brun, Jean-Francois; Price, David L.; Saboungi, Marie-Louise

    2006-01-01

    We describe a new high temperature environment based on aerodynamic levitation and laser heating designed for neutron scattering experiments up to 3000 deg. C. The sample is heated to the desired temperature with three CO 2 lasers from different directions in order to obtain a homogeneous temperature distribution. The apparent temperature of the sample is measured with an optical pyrometer, and two video cameras are employed to monitor the sample behavior during heating. The levitation setup is enclosed in a vacuum-tight chamber, enabling a high degree of gas purity and a reproducible sample environment for structural investigations on both oxide and metallic melts. High-quality neutron diffraction data have been obtained on liquid Y 3 Al 5 O 12 and ZrNi alloy for relatively short counting times (1.5 h)

  7. Magnetic neutron diffraction of MnO thin films

    International Nuclear Information System (INIS)

    Neubeck, W.; Vettier, C.; Mannix, D.; Bernhoeft, N.; Hiess, A.; Ranno, L.; Givord, D.

    1999-01-01

    We report on magnetic neutron diffraction carried out on various epitaxial MnO(III) thin films grown on sapphire and MgO substrates. In all samples, of masses between 5 and 50 μg, magnetic Bragg peaks have been observed. The films exhibit what appears to be continuous phase-transitions in contrast to the strongly discontinuous transition exhibited by bulk samples. In addition, the Neel temperature of films prepared on sapphire substrates is strongly enhanced above that of the bulk whilst that of the film grown on MgO is depressed. The possibility to measure magnetic excitations in such thin film systems is discussed in the light of promising test results obtained from an inelastic magnetic neutron scattering experiment on the IN8 spectrometer. (authors)

  8. Neutron diffraction technique as a method for material studies

    International Nuclear Information System (INIS)

    Belhorma, B.; Labrim, H.; Gandou, Z.

    2010-01-01

    The Morocco's first Nuclear Research has been constructed in CNESTEN. The reactor divergence has been tested, and the nominal power of 2MW was successfully achieved. The reactor has 4 beam ports two of them are projected for neutron scattering. Such technique allows studying the crystallographic and magnetic structures of materials using the thermal neutrons produced in the reactor. the powder diffractometer has been designed. Component reception and installation procedures are in progress. The second experiment consists on small angle neutron scattering that allows the study of soft matter and polymers in the range of 1-50 nm. The third technique that can complete the two previous is the 4-circle neutron spectrometry which is designed mainly to study structural properties of the mono-crystalline material and texture.This technique is complementary to the X-ray diffraction already available in CNESTEN. Some applications of this technique are: --to determine the crystallographic and magnetic structure of polycrystalline materials.-- to study the texture in metals and alloys.-- to perform holography measurement

  9. Residual stress measurement in socket welded joints by neutron diffraction

    International Nuclear Information System (INIS)

    Hayashi, Makoto; Ishiwata, Masayuki; Minakawa, Noriaki; Funahashi, Satoru.

    1995-01-01

    Neutron diffraction measurements of lattice spacings provide the spatial map of residual stress near welds in ferritic steel socket joints. The high tensile stress greater than 200 MPa was found in the fusion and heat-affected zones in the hoop direction. However, the highest tensile stress in the axial direction at the weld root was about 110 MPa relatively lower than the expected value from the fatigue test results. The balancing compressive stress was found near the surface of the socket weld fusion zone. Heat treatment at 625degC for 2 hours was sufficient for the relief of residual stress in socket welds. (author)

  10. Membrane structure: neutron diffraction and small angle scattering studies

    International Nuclear Information System (INIS)

    Zaccai, G.

    1985-01-01

    The author considers a molecule in a beam of radiation of wavelength lambda. Two extreme ways are shown in which on can have many identical molecules in a sample: a crystal in which they are related to each other by the symmetry of a lattice, and complete disorder in which there is no correlation between molecules. The detailed crystallographic analysis of isomorphous replacement is examined. Neutron diffraction experiments with specific deuteration are performed to characterize interactions of cholesterol with lipid bilayers. Retinal rod outer segment disk membranes and the purple membrane of H. halobium are examined

  11. Thermal expansion study of simulated DUPIC fuel using neutron diffraction

    International Nuclear Information System (INIS)

    Kang, Kweon Ho; Ryu, H. J.; Bae, J. H.; Kim, H. S.; Song, K. C.; Yang, M. S.; Choi, Y. N.; Han, Y. S.; Oh, H. S.

    2001-07-01

    The lattice parameters of simulated DUPIC fuel and UO2 were measured from room temperature to 1273 K using neutron diffraction to investigate the thermal expansion and density variation with temperature. The lattice parameter of simulated DUPIC fuel is lower than that of UO2 and the linear thermal expansion of simulated DUPIC fuel is higher than that of UO2. For the temperature range from 298 to 1273 K, the average linear thermal expansion coefficients for UO2 and simulated DUPIC fuel are 10.471 ''10-6 and 10.751 ''10-6 K-1, respectively

  12. Neutron diffraction potentialities at the IBR-2 pulsed reactor for nondestructive testing of structural materials

    International Nuclear Information System (INIS)

    Balagurov, A.M.; Bokuchava, G.D.; Papushkin, I.V.; Sumin, V.V.; Venter, A.M.

    2010-01-01

    Neutron diffraction is widely used for investigations of residual and applied stresses in bulk materials and components. The most important factor in these investigations is the high penetration depth of neutrons (up to 2 cm for steel). At the IBR-2 pulsed reactor in Dubna the Fourier stress diffractometer (FSD) has been constructed to optimize the internal stress measurements. The FSD design satisfies the requirements of high luminosity, high resolution and specific sample environment. The collimator system guarantees a minimum gauge volume of 2x2x2 mm. A mechanical testing machine allows in-situ tension or compression measurements up to a load of 20 kN and sample temperatures up to 800 deg C. In the paper the current status of FSD is reported and potentialities are demonstrated with several examples of investigations performed

  13. Effect of loading mode on lattice strain measurements via neutron diffraction

    International Nuclear Information System (INIS)

    Skippon, T.; Clausen, B.; Daymond, M.R.

    2013-01-01

    The study of lattice strain evolution during uniaxial deformation via in situ neutron diffraction is a well established technique for characterizing the deformation behavior of metals. However, the relatively low flux of neutron facilities results in count times on the order of several minutes, requiring experimenters to choose between either applying a very slow strain rate, or loading the sample incrementally rather than continuously. Here we investigate the effects on lattice strain data obtained by using stress, strain, and position controlled incremental loading, as well as continuous loading, on samples of Zircaloy-2 under uniaxial compression. It was found that both qualitative and quantitative differences arise in the lattice strain behavior of certain grain families, particularly {101 ¯ 0} and {112 ¯ 0}, while other grain families show no discernible effect. The differences in lattice strain evolution brought on by the variation in loading modes are believed to be the result of thermally activated dislocation motion

  14. Neutron diffraction measurements at the INES diffractometer using a neutron radiative capture based counting technique

    Energy Technology Data Exchange (ETDEWEB)

    Festa, G. [Centro NAST, Universita degli Studi di Roma Tor Vergata, Roma (Italy); Pietropaolo, A., E-mail: antonino.pietropaolo@roma2.infn.it [Centro NAST, Universita degli Studi di Roma Tor Vergata, Roma (Italy); Grazzi, F.; Barzagli, E. [CNR-ISC Firenze (Italy); Scherillo, A. [CNR-ISC Firenze (Italy); ISIS facility Rutherford Appleton Laboratory (United Kingdom); Schooneveld, E.M. [ISIS facility Rutherford Appleton Laboratory (United Kingdom)

    2011-10-21

    The global shortage of {sup 3}He gas is an issue to be addressed in neutron detection. In the context of the research and development activity related to the replacement of {sup 3}He for neutron counting systems, neutron diffraction measurements performed on the INES beam line at the ISIS pulsed spallation neutron source are presented. For these measurements two different neutron counting devices have been used: a 20 bar pressure squashed {sup 3}He tube and a Yttrium-Aluminum-Perovskite scintillation detector. The scintillation detector was coupled to a cadmium sheet that registers the prompt radiative capture gamma rays generated by the (n,{gamma}) nuclear reactions occurring in cadmium. The assessment of the scintillator based counting system was done by performing a Rietveld refinement analysis on the diffraction pattern from an ancient Japanese blade and comparing the results with those obtained by a {sup 3}He tube placed at the same angular position. The results obtained demonstrate the considerable potential of the proposed counting approach based on the radiative capture gamma rays at spallation neutron sources.

  15. Precise structural analysis of methane hydrate by neutron diffraction

    International Nuclear Information System (INIS)

    Igawa, Naoki; Hoshikawa, Akinori; Ishii, Yoshinobu

    2006-01-01

    Methane hydrate has attracted great interest as an energy resource to replace natural gas since this material is deposited in the seafloor and the deposits are estimated to exceed those of natural gas. Understanding the physical proprieties, such as the temperature dependence of the crystal structure, helps to specify the optimum environmental temperature and pressure during drilling, transport, and storage of methane hydrate. Clathrate hydrates consisted of encaging atomic and/or molecular species as a guest and host water formed by a hydrogen bonding. Although many studies on the clathrate hydrate including methane hydrate were reported, no detailed crystallographic property has yet been cleared. We focused on the motion of methane in the clathrate hydrate by the neutron diffraction. The crystal structure of the methane hydrate was analyzed by the applying the combination of the Rietveld refinement and the maximum entropy method (MEM) to neutron powder diffraction. Temperature dependence of the scattering-length density distribution maps revealed that the motion of methane molecules differs between the shapes of dodecahedron and tetrakaidecahedron. (author)

  16. Neutron magnetic multiple diffraction in a natural magnetite crystal

    International Nuclear Information System (INIS)

    Mazzocchi, V.L.; Parente, C.B.R.

    1988-09-01

    Neutron multiple diffraction has been employed in the study of the magnetism in magnetite (Fe 3 O 4 ). Magnetite has a crystallographic structure of an inverted spinel with tetrahedral A sites occupied solely by trivalent Fe 3+ ions and octahedral B sites occupied both by divalent Fe 2+ ions and the remaining Fe 3+ ions in random distribution. At room temperature magnetite is a Neel A-B ferrimagnet where the ions on the A, B sites are coupled antiferromagneticaly. This coupling disappears at T sup c approx. or approx.= 580 0 C. Employing a natural single crystal of magnetite experimental neutron multiple diffraction patterns were obtained for the primary reflection 111 at room temperature and 703 0 C. This reflection is almost entirely magnetic in origin resulting in 'Aufhellung' patterns below T c and mixed 'Aufhellung-Umweganregung' patterns above T c . Theoretical patterns were calculated employing the iterative method for the approximation of intensities by a Taylor series and compared to the experimental results. (author) [pt

  17. Kinetic studies of methane-ethane mixed gas hydrates by neutron diffraction and Raman spectroscopy.

    Science.gov (United States)

    Murshed, M Mangir; Kuhs, Werner F

    2009-04-16

    In situ formations of CH(4)-C(2)H(6) mixed gas hydrates were made using high flux neutron diffraction at 270 K and 5 MPa. For this purpose, a feed gas composition of CH(4) and C(2)H(6) (95 mol% CH(4)) was employed. The rates of transformation of spherical grains of deuterated ice Ih into hydrates were measured by time-resolved neutron powder diffraction on D20 at ILL, Grenoble. Phase fractions of the crystalline constituents were obtained from Rietveld refinements. A concomitant formation of structure type I (sI) and structure type II (sII) hydrates were observed soon after the gas pressure was applied. The initial fast formation of sII hydrate reached its maximum volume and started declining very slowly. The formation of sI hydrate followed a sigmoid growth kinetics that slowed down due to diffusion limitation. This observation has been interpreted in terms of a kinetically favored nucleation of the sII hydrate along with a slow transformation into sI. Both powder diffraction and Raman spectroscopic results suggest that a C(2)H(6)-rich sII hydrate was formed at the early part of the clathration, which slowly decreased to approximately 3% after a reaction of 158 days as confirmed by synchrotron XRD. The final persistence of a small portion of sII hydrate points to a miscibility gap between CH(4)-rich sI and C(2)H(6)-rich sII hydrates.

  18. Magnetostructural transition in Fe5SiB2 observed with neutron diffraction

    Czech Academy of Sciences Publication Activity Database

    Cedervall, J.; Kontos, S.; Hansen, T. C.; Balmes, O.; Martinez-Casado, F. J.; Matěj, Z.; Beran, Přemysl; Svedlindh, P.; Gunnarsson, K.; Sahlberg, M.

    2016-01-01

    Roč. 235, MAR (2016), s. 113-118 ISSN 0022-4596 Institutional support: RVO:61389005 Keywords : magnetism * X-ray diffraction * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.299, year: 2016

  19. A new approach of quantum mechanics for neutron single-slit diffraction

    International Nuclear Information System (INIS)

    Wu Xiangyao; Yang Jinghai; Liu Xiaojing; Wang Li; Liu Bing; Fan Xihui; Guo Yiqing

    2007-01-01

    Phenomena of electron, neutron, atomic and molecular diffraction have been studied in many experiments, and these experiments are explained by many theoretical works. We study neutron single-slit diffraction with a quantum mechanical approach. It is found that the obvious diffraction patterns can be obtained when the single slit width a is in the range of 3λ-60λ. We also find a new quantum effect of the thickness of single-slit which can make a large impact on the diffraction pattern. The new quantum effect predicted in our work can be tested by the neutron single-slit diffraction experiment. (authors)

  20. Neutron diffraction study of TiCxNyHz

    International Nuclear Information System (INIS)

    Khidirov, I.

    1996-01-01

    Neutron diffraction study of titanium carbonitridohydride is carried out. It is shown that TiC x N y H z may have a disordered, on ordered and a partially ordered structure depending on the composition. Both in the ordered and in the disordered structure the atoms of carbon and nitrogen are located in octahedron interstices only. Under (C+N)/Ti > 0.70 the atoms of hydrogen are located in octahedron interstices only. Under (C+N)/Ti < 0.50 and under high temperatures the atoms of hydrogen occupy both octahedron and tetrahedron interstices; under low temperatures the transition of some hydrogen atoms from tetrahedron into octahedron interstices is observed. 15 refs.; 1 fig.; 1 tab

  1. Neutron diffraction studies of amphipathic helices in phospholipid bilayers

    Energy Technology Data Exchange (ETDEWEB)

    Bradshaw, J.P.; Gilchrist, P.J. [Univ. of Edinburgh (United Kingdom); Duff, K.C. [Univ. of Edinburgh Medical School (United Kingdom); Saxena, A.M. [Brookhaven National Laboratory, Upton, NY (United States)

    1994-12-31

    The structural feature which is thought to facilitate the interaction of many peptides with phospholipid bilayers is the ability to fold into an amphipathic helix. In most cases the exact location and orientation of this helix with respect to the membrane is not known, and may vary with factors such as pH and phospholipid content of the bilayer. The growing interest in this area is stimulated by indications that similar interactions can contribute to the binding of certain hormones to their cell-surface receptors. We have been using the techniques of neutron diffraction from stacked phospholipid bilayers in an attempt to investigate this phenomenon with a number of membrane-active peptides. Here we report some of our findings with three of these: the bee venom melittin; the hormone calcitonin; and a synthetic peptide representing the ion channel fragment of influenza A M2 protein.

  2. A neutron diffraction study of ancient Greek ceramics

    International Nuclear Information System (INIS)

    Siouris, I.M.; Walter, J.

    2006-01-01

    Non-destructive neutron diffraction studies were performed on three 2nd-century BC archaeological pottery fragments from the excavation site of Neos Scopos, Serres, in North Greece. In all the 273 K diagrams quartz and feldspars phase fractions are dominant. Diopside and iron oxide phases were also identifiable. The diopside content is found to decrease with increasing quartz-feldspar compositions. Iron oxides containing minerals were found to be present and the phase compositions reflect upon the coloring of the samples. However, the different content compositions of the phases may suggest different regions of the original clay materials as well as different preparation techniques. The firing temperatures were determined to be in the range of 900-1000 deg. C

  3. Neutron diffraction studies of amphipathic helices in phospholipid bilayers

    International Nuclear Information System (INIS)

    Bradshaw, J.P.; Gilchrist, P.J.; Duff, K.C.; Saxena, A.M.

    1994-01-01

    The structural feature which is thought to facilitate the interaction of many peptides with phospholipid bilayers is the ability to fold into an amphipathic helix. In most cases the exact location and orientation of this helix with respect to the membrane is not known, and may vary with factors such as pH and phospholipid content of the bilayer. The growing interest in this area is stimulated by indications that similar interactions can contribute to the binding of certain hormones to their cell-surface receptors. We have been using the techniques of neutron diffraction from stacked phospholipid bilayers in an attempt to investigate this phenomenon with a number of membrane-active peptides. Here we report some of our findings with three of these: the bee venom melittin; the hormone calcitonin; and a synthetic peptide representing the ion channel fragment of influenza A M2 protein

  4. Structural studies of liquid alcohols by neutron diffraction

    International Nuclear Information System (INIS)

    Montague, D.G.; Cummings, S.

    1984-01-01

    Neutron diffraction measurements have been made on methyl alcohol at room temperature for an incident wavelength of 0.94 A. Cross sections have been obtained for CD 3 OD, CD 3 OH, and mixtures of these compounds. These data are subtracted to obtain the separated structure factors for intermolecular H 0 H 0 , the hydroxyl components, and the non-hydroxyl components. The Fourier transformations of the structure factors show components of both intra- and intermolecular distribution functions. Width parameters obtained from model fits are too large for thermal vibrations and are interpreted as geometrical broadening due to the stretching of bonds, variations in bond angles, and rotation of the methyl group. Differences in the real space distribution function between hydrogen and deuterium are noted. (author)

  5. In situ X-ray and neutron diffraction of the Ruddlesden–Popper compounds (RE2−xSrx)0.98(Fe0.8Co0.2)1−yMgyO4−δ (RE=La, Pr): Structure and CO2 stability

    International Nuclear Information System (INIS)

    Chatzichristodoulou, C.; Hauback, B.C.; Hendriksen, P.V.

    2013-01-01

    The crystal structure of the Ruddlesden–Popper compounds (La 1.0 Sr 1.0 ) 0.98 Fe 0.8 Co 0.2 O 4−δ and (La 1.2 Sr 0.8 ) 0.98 (Fe 0.8 Co 0.2 ) 0.8 Mg 0.2 O 4−δ was investigated at 1000 °C in N 2 (a O2 =1×10 −4 ) by in-situ powder neutron diffraction. In-situ powder X-ray diffraction (PXD) was also employed to investigate the temperature dependence of the lattice parameters of the compounds in air and the oxygen activity dependence of the lattice parameters at 800 °C and 1000 °C. The thermal and chemical expansion coefficients, determined along the two crystallographic directions of the tetragonal unit cell, are highly anisotropic. The equivalent pseudo-cubic thermal and chemical expansion coefficients are in agreement with values determined by dilatometry. The chemical stability in CO 2 containing environments of various Ruddlesden–Popper compounds with chemical formula (RE 2−x Sr x ) 0.98 (Fe 0.8 Co 0.2 ) 1−y Mg y O 4−δ (RE=La, Pr), as well as their stability limit in H 2 /H 2 O=4.5 were also determined by in-situ PXD for x=0.9, 1.0 and y=0, 0.2. - Graphical abstract: Influence of electronic configuration on bond length, lattice parameters and anisotropic thermal and chemical expansion. Highlights: ► The thermal and chemical expansion coefficients are largely anisotropic. ► The expansion of the perovskite layers is constrained along the a direction. ► The studied compositions show remarkable thermodynamic stability upon reduction. ► The thermal and chemical expansion coefficients are lower than related perovskites. ► The investigated materials decompose in CO 2 containing atmospheres

  6. Study of ethanol-lysozyme interactions using neutron diffraction

    International Nuclear Information System (INIS)

    Lehmann, M.S.; Mason, S.A.; McIntyre, G.J.

    1985-01-01

    Single-crystal neutron diffraction has been used to observe the interactions between deuterated ethanol (CD3CD2OH) and lysozyme in triclinic crystals of hen egg white lysozyme soaked in 25% (v/v) ethanol solutions. A total of 6047 observed reflections to a resolution of 2 A were used, and 13 possible ethanol sites were identified. The three highest occupied sites are close to locations for bromoethanol found in an earlier study by Yonath et al. [Yonath, A., Podjarny, A., Honig, B., Traub, W., Sielecki, A., Herzberg, O., and Moult, J. (1978) Biophys. Struct. Mech. 4, 27-36]. Structure refinements including a model for the flat solvent lead to a final crystallographic agreement factor of 0.097. Comparison with earlier neutron studies on triclinic lysozyme showed that neither the molecular structure nor the thermal motions were affected significantly by the ethanol. A detailed analysis of the ethanol-lysozyme contacts showed 61% of these to be with hydrophobic sites, in agreement with the dominant hydrophobic nature of ethanol. This, together with the fact that the molecular structure of lysozyme is not perturbed, suggests a model for denaturation of lysozyme by alcohol, which proceeds via a dehydration of the protein at high alcohol concentration

  7. Principles of the measurement of residual stress by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Webster, G A; Ezeilo, A N [Imperial Coll. of Science and Technology, London (United Kingdom). Dept. of Mechanical Engineering

    1996-11-01

    The presence of residual stresses in engineering components can significantly affect their load carrying capacity and resistance to fracture. In order to quantify their effect it is necessary to know their magnitude and distribution. Neutron diffraction is the most suitable method of obtaining these stresses non-destructively in the interior of components. In this paper the principles of the technique are described. A monochromatic beam of neutrons, or time of flight measurements, can be employed. In each case, components of strain are determined directly from changes in the lattice spacings between crystals. Residual stresses can then be calculated from these strains. The experimental procedures for making the measurements are described and precautions for achieving reliable results discussed. These include choice of crystal planes on which to make measurements, extent of masking needed to identify a suitable sampling volume, type of detector and alignment procedure. Methods of achieving a stress free reference are also considered. A selection of practical examples is included to demonstrate the success of the technique. (author) 14 figs., 1 tab., 18 refs.

  8. Principles of the measurement of residual stress by neutron diffraction

    International Nuclear Information System (INIS)

    Webster, G.A.; Ezeilo, A.N.

    1996-01-01

    The presence of residual stresses in engineering components can significantly affect their load carrying capacity and resistance to fracture. In order to quantify their effect it is necessary to know their magnitude and distribution. Neutron diffraction is the most suitable method of obtaining these stresses non-destructively in the interior of components. In this paper the principles of the technique are described. A monochromatic beam of neutrons, or time of flight measurements, can be employed. In each case, components of strain are determined directly from changes in the lattice spacings between crystals. Residual stresses can then be calculated from these strains. The experimental procedures for making the measurements are described and precautions for achieving reliable results discussed. These include choice of crystal planes on which to make measurements, extent of masking needed to identify a suitable sampling volume, type of detector and alignment procedure. Methods of achieving a stress free reference are also considered. A selection of practical examples is included to demonstrate the success of the technique. (author) 14 figs., 1 tab., 18 refs

  9. Mapping residual and internal stress in materials by neutron diffraction

    International Nuclear Information System (INIS)

    Withers, Ph.J.

    2007-01-01

    Neutron diffraction provides one of the few means of mapping residual stresses deep within the bulk of materials and components. This article reviews the basic scientific methodology by which internal strains and stresses are inferred from recorded diffraction peaks. Both conventional angular scans and time-of-flight measurements are reviewed and compared. Their complementarity with analogous synchrotron X-ray methods is also highlighted. For measurements to be exploited in structural integrity calculations underpinning the safe operation of engineering components, measurement standards have been defined and the major findings are summarised. Examples are used to highlight the unique capabilities of the method showing how it can provide insights ranging from the basic physics of slip mechanisms in hexagonal polycrystalline materials, through the materials optimisation of stress induced transformations in smart nano-materials, to the industrial introduction of novel friction welding processes exploiting stress residual measurements transferred from prototype sub-scale tests to the joining of full-scale aero-engine assemblies. (author)

  10. Direct observation of crystal texture by neutron diffraction topography

    International Nuclear Information System (INIS)

    Tomimitsu, Hiroshi

    1982-02-01

    This document reports the development and the applications of the neutron diffraction topography (NDT), which have been carried out at JAERI in these 10 years. This describes how the substructure of Cu-5%Ge single crystal of large-scale (3 cm in diameter and 10 cm in length) was revealed by the NDT-observation. It was discovered that the specimen crystal was made up from the layer-substructures parallel to (001) and to the [110] growth direction, and that each (001) layer-substructure mentioned above was further subdivided into the central thin sublayer parallel to (001) and thick plates of [100] and [010] directions, attached symmetrically to both sides of the central (001) sublayer with regular intervals. The model of the substructure described above was supported by the calculation of the diffraction intensities. The model of the layer-substructure described above, on the other hand, suggested a simple mechanism of crystal growth of the specimen. This document also reports the NDT-observation of the three-dimensional distribution of the lattice strains within a hot-pressed Ge single crystal, and the equal thickness fringes and the coherent boundaries of a twinned Si crystal. The powerfulness and the reliability of the NDT-technique were thus demonstrated. (author)

  11. The early development of neutron diffraction: science in the wings of the Manhattan Project.

    Science.gov (United States)

    Mason, T E; Gawne, T J; Nagler, S E; Nestor, M B; Carpenter, J M

    2013-01-01

    Although neutron diffraction was first observed using radioactive decay sources shortly after the discovery of the neutron, it was only with the availability of higher intensity neutron beams from the first nuclear reactors, constructed as part of the Manhattan Project, that systematic investigation of Bragg scattering became possible. Remarkably, at a time when the war effort was singularly focused on the development of the atomic bomb, groups working at Oak Ridge and Chicago carried out key measurements and recognized the future utility of neutron diffraction quite independent of its contributions to the measurement of nuclear cross sections. Ernest O. Wollan, Lyle B. Borst and Walter H. Zinn were all able to observe neutron diffraction in 1944 using the X-10 graphite reactor and the CP-3 heavy water reactor. Subsequent work by Wollan and Clifford G. Shull, who joined Wollan's group at Oak Ridge in 1946, laid the foundations for widespread application of neutron diffraction as an important research tool.

  12. On the neutron diffraction in a crystal in the field of a standing laser wave

    International Nuclear Information System (INIS)

    Grigoryan, K.K.; Hayrapetyan, A.G.; Petrosyan, R.G.

    2010-01-01

    The possibility of high-energy neutron diffraction in a crystal is shown by applying the solution of time-dependent Schroedinger equation for a neutron in the field of a standing laser wave. The scattering picture is examined within the framework of non-stationary S-matrix theory, where the neutron-laser field interaction is considered exactly and the neutron-crystal interaction is considered as a perturbation described by Fermi pseudopotential (Farri representation). The neutron-crystal interaction is elastic, and the neutron-laser field interaction has both inelastic and elastic behaviors which results in the observation of an analogous to the Kapitza-Dirac effect for neutrons. The neutron scattering probability is calculated and the analysis of the results are adduced. Both inelastic and elastic diffraction conditions are obtained and the formation of a 'sublattice' is illustrated in the process of neutron-photon-phonon elastic interaction.

  13. Application of a high-temperature neutron diffraction apparatus to the study of refractory oxides

    International Nuclear Information System (INIS)

    Aldebert, P.; Badie, J.-M.; Buevoz, J.-L.; Roult, G.

    1975-01-01

    A furnace allowing studies of refractory materials by neutron diffraction in situ up to 2500 deg C is described. It is fitted on to a new type of time of flight spectrometer the pulsed source of which is given by a correlation chopper. The advantages of this technique in comparison with fixed-wavelength goniometers are developped. The examination at high temperature of several refractory oxides has been carried out with this experimental device. The thermal expansion curve of α alumina has been established with accuracy up to near the melting point. Several high temperature cristalline forms, X form La 2 O 3 , the tetragonal and cubic ZrO 2 , tetragonal HfO 2 , have been studied. Concerning the latter two, the case of their solid solutions 2MO 2 -M' 2 O 3 (with M=Hf or Zr and M'=La or Y) has also been considered, at room temperature only [fr

  14. Deformation behaviors of aluminum alloys for automobile parts studied by neutron diffraction

    International Nuclear Information System (INIS)

    Katayanagi, Kazue; Morita, Kensuke; Tomota, Yo; Kamiyama, Takashi; Terakado, Katsuyoshi

    2008-01-01

    In situ time of flight neutron diffraction measurements during tension test were performed for three Al-Si alloys with different microstructures including hot-forged (AHS 2), T 6 heat-treated (AHS 2-T 6) and die-cast (ACD 12) specimens. Strength and work-hardening behaviors of these specimens are investigated by evaluating phase stresses, i.e., stress partitioning between Si and the Al matrix as well as intergranular stresses of [hkl] oriented family grains in the component phases. It is revealed that Si particles embedded in the Al matrix play a role of the hard second phase. The size and shape of the Si particles affect work hardening and fracture of the alloys. (author)

  15. Neutron diffraction study of the reduction of NiAl2O4

    International Nuclear Information System (INIS)

    Ustundag, E.; Clausen, B.; Bourke, M. A. M.

    2000-01-01

    The reduction of a solid NiAl 2 O 4 cylinder to a metal-ceramic composite consisting of Ni particles in an Al 2 O 3 matrix was monitored in situ at 1220 degree sign C with neutron powder diffraction. The reaction kinetics was determined with a time resolution of 30 min. The reduction is associated with a volume shrinkage. A comparison of finite element calculations and the changes in the measured lattice parameters suggests that creep has relaxed the residual strains that would otherwise result from the volume shrinkage. The data also indicate that structural evolution in unreduced NiAl 2 O 4 via a change in the cationic sublattice towards inverse spinel occurred and that led to a variation in lattice parameters. (c) 2000 American Institute of Physics

  16. Neutrons in studies of phospholipid bilayers and bilayer–drug interaction. I. Basic principles and neutron diffraction

    Directory of Open Access Journals (Sweden)

    Belička M.

    2014-12-01

    Full Text Available In our paper, we demonstrate several possibilities of using neutrons in pharmaceutical research with the help of examples of scientific results achieved at our University. In this first part, basic properties of neutrons and elementary principles of elastic scattering of thermal neutrons are described. Results of contrast variation neutron diffraction on oriented phospholipid bilayers with intercalated local anaesthetic or cholesterol demonstrate the potential of this method at determination of their position in bilayers. Diffraction experiments with alkan-1-ols located in the bilayers revealed their influence on bilayer thickness as a function of their alkyl chain length.

  17. In situ calibration of TFTR neutron detectors

    International Nuclear Information System (INIS)

    Hendel, H.W.; Palladino, R.W.; Barnes, C.W.; Diesso, M.; Felt, J.S.; Jassby, D.L.; Johnson, L.C.; Ku, L.; Liu, Q.P.; Motley, R.W.; Murphy, H.B.; Murphy, J.; Nieschmidt, E.B.; Roberts, J.A.; Saito, T.; Strachan, J.D.; Waszazak, R.J.; Young, K.M.

    1990-01-01

    We report results of the TFTR fission detector calibration performed in December 1988. A NBS-traceable, remotely controlled 252 Cf neutron source was moved toroidally through the TFTR vacuum vessel. Detection efficiencies for two 235 U detectors were measured for 930 locations of the neutron point source in toroidal scans at 16 different major radii and vertical heights. These scans effectively simulated the volume-distributed plasma neutron source and the volume-integrated detection efficiency was found to be insensitive to plasma position. The Campbell mode is useful due to its large overlap with the count rate mode and large dynamic range. The resulting absolute plasma neutron source calibration has an uncertainty of ±13%

  18. Needs of in-situ materials testing under neutron irradiation

    International Nuclear Information System (INIS)

    Noda, K.; Hishinuma, A.; Kiuchi, K.

    1989-01-01

    Under neutron irradiation, the component atoms of materials are displaced as primary knock-on atoms, and the energy of the primary knock-on atoms is consumed by electron excitation and nuclear collision. Elementary irradiation defects accumulate to form damage structure including voids and bubbles. In situ test under neutron irradiation is necessary for investigating into the effect of irradiation on creep behavior, the electric properties of ceramics, transport phenomena and so on. The in situ test is also important to investigate into the phenomena related to the chemical reaction with environment during irradiation. Accelerator type high energy neutron sources are preferable to fission reactors. In this paper, the needs and the research items of in situ test under neutron irradiation using a D-Li stripping type high energy neutron source on metallic and ceramic materials are described. Creep behavior is one of the most important mechanical properties, and depends strongly on irradiation environment, also it is closely related to microstructure. Irradiation affects the electric conductibity of ceramics and also their creep behavior. In this way, in situ test is necessary. (K.I.)

  19. Time-of-flight pulsed neutron diffraction of molten salts

    Energy Technology Data Exchange (ETDEWEB)

    Fukushima, Y; Misawa, M; Suzuki, K [Tohoku Univ., Sendai (Japan). Research Inst. for Iron, Steel and Other Metals

    1975-06-01

    In this work, the pulsed neutron diffraction of molten alkali metal nitrate and bismuth trihalide was measured by the time-of-flight method. An electron linear accelerator was used as the pulsed neutron source. All the measurements were carried out with the T-O-F neutron diffractometer installed on the 300 MeV electron lineac. Molten NaNO/sub 3/ and RbNO/sub 3/ were adopted as the samples for alkali metal nitrate. The measurement is in progress for KNO/sub 3/ and LiNO/sub 3/. As the first step of the study on bismuth-bismuth trihalide system, the temperature dependence of structure factors was observed for BiCl/sub 3/, BiBr/sub 3/ and BiI/sub 3/ in the liquid state. The structure factors Sm(Q) for molten NaNO/sub 3/ at 340/sup 0/C and RbNO/sub 3/ at 350/sup 0/C were obtained, and the form factor F/sub 1/(Q) for single NO/sub 3//sup -/ radical with equilateral triangle structure was calculated. In case of molten NaNO/sub 3/, the first peak of Sm(Q) is simply smooth and a small hump can be observed in the neighbourhood of the first minimum Q position. The first peak of Sm(Q) for molten RbNO/sub 3/ is divided into two peaks, whereas a hump at the first minimum becomes big, and shifts to the low Q side of the second peak. The size of the NO/sub 3//sup -/ radical in molten NaNO/sub 3/ is a little smaller than that in molten RbNO/sub 3/. The values of the bond length in the NO/sub 3//sup -/ radical are summarized for crystal state and liquid state. The temperature dependence of the structure factor S(Q) was observed for BiCl/sub 3/, BiBr/sub 3/ and BiI/sub 3/, and shown in a figure.

  20. Six-axis multi-anvil press for high-pressure, high-temperature neutron diffraction experiments

    Energy Technology Data Exchange (ETDEWEB)

    Sano-Furukawa, A., E-mail: sano.asami@jaea.go.jp; Hattori, T. [Quantum Beam Science Center, Japan Atomic Energy Agency, Ibaraki 319-1195 (Japan); J-PARC Center, Japan Atomic Energy Agency, Ibaraki 319-1195 (Japan); Arima, H. [Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Yamada, A. [The University of Shiga Prefecture, Shiga 522-8533 (Japan); Tabata, S.; Kondo, M.; Nakamura, A. [Sumitomo Heavy Industries Co., Ltd., Ehime 792-0001 (Japan); Kagi, H.; Yagi, T. [Geochemical Research Center, Graduate School of Science, The University of Tokyo, Tokyo 113-0033 (Japan)

    2014-11-15

    We developed a six-axis multi-anvil press, ATSUHIME, for high-pressure and high-temperature in situ time-of-flight neutron powder diffraction experiments. The press has six orthogonally oriented hydraulic rams that operate individually to compress a cubic sample assembly. Experiments indicate that the press can generate pressures up to 9.3 GPa and temperatures up to 2000 K using a 6-6-type cell assembly, with available sample volume of about 50 mm{sup 3}. Using a 6-8-type cell assembly, the available conditions expand to 16 GPa and 1273 K. Because the six-axis press has no guide blocks, there is sufficient space around the sample to use the aperture for diffraction and place an incident slit, radial collimators, and a neutron imaging camera close to the sample. Combination of the six-axis press and the collimation devices realized high-quality diffraction pattern with no contamination from the heater or the sample container surrounding the sample. This press constitutes a new tool for using neutron diffraction to study the structures of crystals and liquids under high pressures and temperatures.

  1. Time-of-flight diffraction at pulsed neutron sources: An introduction to the symposium

    International Nuclear Information System (INIS)

    Jorgensen, J.D.

    1994-01-01

    In the 25 years since the first low-power demonstration experiments, pulsed neutron sources have become as productive as reactor sources for many types of diffraction experiments. The pulsed neutron sources presently operating in the United States, England, and Japan offer state of the art instruments for powder and single crystal diffraction, small angle scattering, and such specialized techniques as grazing-incidence neutron reflection, as well as quasielastic and inelastic scattering. In this symposium, speakers review the latest advances in diffraction instrumentation for pulsed neutron sources and give examples of some of the important science presently being done. In this introduction to the symposium, I briefly define the basic principles of pulsed neutron sources, review their development, comment in general terms on the development of time-of-flight diffraction instrumentation for these sources, and project how this field will develop in the next ten years

  2. In-Situ Spectrometry of Neutrons

    Science.gov (United States)

    Maurer, Richard H.

    1999-01-01

    High energy charged particles of extra-galactic, galactic and solar origin collide with spacecraft structures in Earth orbit outside the atmosphere and in interplanetary travel beyond the Earth's magnetosphere. These primaries create a number of secondary particles inside the structures that can produce a significant ionizing radiation environment. This radiation is a threat to long term inhabitants or travelers for space missions and produces an increased risk of cancer and DNA damage. The primary high energy cosmic rays and trapped protons collide with common spacecraft materials such as aluminum and silicon and create secondary particles inside structures that are mostly protons and neutrons. Charged protons are readily detected and instruments are already in existence for this task. Neutrons are electrically neutral and therefore much more difficult to measure and detect. These neutrons are reported to contribute 30-60% of the dose inside space structures and cannot be ignored. Currently there is no compact, portable and real time neutron detector instrumentation available for use inside spacecraft or on planetary surfaces where astronauts will live and work. We propose to design and build a portable, low power and robust neutron spectrometer that will measure the neutron spectrum from 10 KeV to 500 MeV with at least 10% energy resolution in the various energy intervals. This instrument will monitor the existing neutron environment both inside spacecraft structures and on planetary surfaces to determine the safest living areas, warn of high fluxes associated with solar storms and assist the NSBRI Radiation Effects Team in making an accurate assessment of increased cancer risk and DNA damage to astronauts. The instrument uses a highly efficient proportional counter Helium 3 tube at the lowest energy intervals where .equivalent damage factors for tissue are the highest (10 KeV-2 MeV). The Helium 3 tube may be shielded with a cadmium absorber to eliminate the much

  3. X-ray and Neutron Diffraction in the Study of Organic Crystalline Hydrates

    Directory of Open Access Journals (Sweden)

    Katharina Fucke

    2010-07-01

    Full Text Available A review. Diffraction methods are a powerful tool to investigate the crystal structure of organic compounds in general and their hydrates in particular. The laboratory standard technique of single crystal X-ray diffraction gives information about the molecular conformation, packing and hydrogen bonding in the crystal structure, while powder X-ray diffraction on bulk material can trace hydration/dehydration processes and phase transitions under non-ambient conditions. Neutron diffraction is a valuable complementary technique to X-ray diffraction and gives highly accurate hydrogen atom positions due to the interaction of the radiation with the atomic nuclei. Although not yet often applied to organic hydrates, neutron single crystal and neutron powder diffraction give precise structural data on hydrogen bonding networks which will help explain why hydrates form in the first place.

  4. Dynamical theory of neutron diffraction. [One-body Schroedinger equation, review

    Energy Technology Data Exchange (ETDEWEB)

    Sears, V F [Atomic Energy of Canada Ltd., Chalk River, Ontario. Chalk River Nuclear Labs.

    1978-10-01

    We present a review of the dynamical theory of neutron diffraction by macroscopic bodies which provides the theoretical basis for the study of neutron optics. We consider both the theory of dispersion, in which it is shown that the coherent wave in the medium satisfies a macroscopic one-body Schroedinger equation, and the theory of reflection, refraction, and diffraction in which the above equation is solved for a number of special cases of interest. The theory is illustrated with the help of experimental results obtained over the past 10 years by a number of new techniques such as neutron gravity refractometry. Pendelloesung interference, and neutron interferometry.

  5. Study on Destructuring effect of trehalose on water by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Branca, C.; Maisano, G.; Migliardo, F. [Dipartimento di Fisica and INFM, Universita' di Messina, PO Box 55, 98166 Messina (Italy); Magazu' , V. [Facolta di Ingeeneria, Universita' di Messina, 98166 Messina (Italy); Soper, A.K. [ISIS Facility, Rutherford Appleton Laboratory, Chilton, Didcot, Oxon OX11 0QX (United Kingdom)

    2002-07-01

    In this work results on trehalose/water solutions by neutron diffraction are reported. The study of the partial structure factors and spatial distribution functions gives evidence of a decreasing tetrahedrality degree of water and justifies its cryoprotectant effectiveness. (orig.)

  6. Neutron scattering and diffraction instrument for structural study on biology in Japan

    Energy Technology Data Exchange (ETDEWEB)

    Niimura, Nobuo [Japan Atomic Energy Research Inst., Ibaraki-ken (Japan)

    1994-12-31

    Neutron scattering and diffraction instruments in Japan which can be used for structural studies in biology are briefly introduced. Main specifications and general layouts of the instruments are shown.

  7. Study on Destructuring effect of trehalose on water by neutron diffraction

    CERN Document Server

    Branca, C; Migliardo, F; Magazù, V; Soper, A K

    2002-01-01

    In this work results on trehalose/water solutions by neutron diffraction are reported. The study of the partial structure factors and spatial distribution functions gives evidence of a decreasing tetrahedrality degree of water and justifies its cryoprotectant effectiveness. (orig.)

  8. Structure analysis of liquids and disordered materials using pulsed neutron diffraction and total scattering

    International Nuclear Information System (INIS)

    Suzuya, Kentaro

    2011-01-01

    Neutron diffraction·total scattering at pulsed neutron source is a powerful method to analyze the complex structure of disordered materials: liquids, glasses, amorphous materials and disordered crystals. The basic idea of the structure of disordered materials, the fundamental diffraction theory for disordered materials, and structure analysis of disordered materials using pulsed neutron diffraction·total scattering technique (TOF method) are described in detail. In addition, the precise information of the world highest class J-PARC MLF spallation neutron source and typical J-PARC neutron total scattering instrument NOVA are also given. Recent structural modelling methods of disordered materials such like reverse Monte Carlo (RMC) simulation method is briefly described using an example of the analysis of a typical disordered material silica glass. (author)

  9. Comparative study of structural properties of trehalose water solutions by neutron diffraction, synchrotron radiation and simulation

    Energy Technology Data Exchange (ETDEWEB)

    Cesaro, A.; Magazu, V.; Migliardo, F.; Sussich, F.; Vadala, M

    2004-07-15

    Neutron diffraction measurements combined with H/D substitution have been performed on trehalose aqueous solutions as a function of temperature and concentration by using the SANDALS diffractometer at ISIS Facility (UK). The findings point out a high capability of trehalose to strongly affect the tetrahedral hydrogen bond network of water. The neutron diffraction results are also compared with simulation and experimental data obtained by synchrotron radiation on the phospholipid bilayer membranes (DPPC)/trehalose/H{sub 2}O ternary system.

  10. High-resolution neutron diffraction studies of biological and industrial fibres

    Energy Technology Data Exchange (ETDEWEB)

    Langan, P; Mason, S A [Institut Max von Laue - Paul Langevin (ILL), 38 - Grenoble (France); Fuller, W; Forsyth, V T; Mahendrasingam, A; Shotton, M; Simpson, L [Keele Univ. (United Kingdom); Grimm, H [FZ, Juelich (Germany); Leberman, R [EMBL, (Country Unknown)

    1997-04-01

    Neutron diffraction is becoming an important tool for studying fibres due to its complementarity to X-ray diffraction. Unlike X-rays, scattering of neutrons by polymer atoms is not a function of their atomic number. In high-resolution studies (1.5-3 A) on D19 deuteration (replacing H by D) is being used to change the relative scattering power of chosen groups making them easier to locate. Recent studies on DNA and cellulose are described. (author). 6 refs.

  11. X-ray and neutron diffraction studies of crystallinity in hydroxyapatite coatings.

    Science.gov (United States)

    Girardin, E; Millet, P; Lodini, A

    2000-02-01

    To standardize industrial implant production and make comparisons between different experimental results, we have to be able to quantify the crystallinity of hydroxyapatite. Methods of measuring crystallinity ratio were developed for various HA samples before and after plasma spraying. The first series of methods uses X-ray diffraction. The advantage of these methods is that X-ray diffraction equipment is used widely in science and industry. In the second series, a neutron diffraction method is developed and the results recorded are similar to those obtained by the modified X-ray diffraction methods. The advantage of neutron diffraction is the ability to obtain measurements deep inside a component. It is a nondestructive method, owing to the very low absorption of neutrons in most materials. Copyright 2000 John Wiley & Sons, Inc.

  12. The early development of neutron diffraction: science in the wings of the Manhattan Project

    Energy Technology Data Exchange (ETDEWEB)

    Mason, T. E., E-mail: masont@ornl.gov; Gawne, T. J.; Nagler, S. E.; Nestor, M. B. [Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Carpenter, J. M. [Argonne National Laboratory, Argonne, IL 60439 (United States); Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States)

    2013-01-01

    Early neutron diffraction experiments performed in 1944 using the first nuclear reactors are described. Although neutron diffraction was first observed using radioactive decay sources shortly after the discovery of the neutron, it was only with the availability of higher intensity neutron beams from the first nuclear reactors, constructed as part of the Manhattan Project, that systematic investigation of Bragg scattering became possible. Remarkably, at a time when the war effort was singularly focused on the development of the atomic bomb, groups working at Oak Ridge and Chicago carried out key measurements and recognized the future utility of neutron diffraction quite independent of its contributions to the measurement of nuclear cross sections. Ernest O. Wollan, Lyle B. Borst and Walter H. Zinn were all able to observe neutron diffraction in 1944 using the X-10 graphite reactor and the CP-3 heavy water reactor. Subsequent work by Wollan and Clifford G. Shull, who joined Wollan’s group at Oak Ridge in 1946, laid the foundations for widespread application of neutron diffraction as an important research tool.

  13. The early development of neutron diffraction: science in the wings of the Manhattan Project

    International Nuclear Information System (INIS)

    Mason, T. E.; Gawne, T. J.; Nagler, S. E.; Nestor, M. B.; Carpenter, J. M.

    2013-01-01

    Early neutron diffraction experiments performed in 1944 using the first nuclear reactors are described. Although neutron diffraction was first observed using radioactive decay sources shortly after the discovery of the neutron, it was only with the availability of higher intensity neutron beams from the first nuclear reactors, constructed as part of the Manhattan Project, that systematic investigation of Bragg scattering became possible. Remarkably, at a time when the war effort was singularly focused on the development of the atomic bomb, groups working at Oak Ridge and Chicago carried out key measurements and recognized the future utility of neutron diffraction quite independent of its contributions to the measurement of nuclear cross sections. Ernest O. Wollan, Lyle B. Borst and Walter H. Zinn were all able to observe neutron diffraction in 1944 using the X-10 graphite reactor and the CP-3 heavy water reactor. Subsequent work by Wollan and Clifford G. Shull, who joined Wollan’s group at Oak Ridge in 1946, laid the foundations for widespread application of neutron diffraction as an important research tool

  14. Incident spectrum determination for time-of-flight neutron powder diffraction data analysis

    International Nuclear Information System (INIS)

    Hodges, J. P.

    1998-01-01

    Accurate characterization of the incident neutron spectrum is an important requirement for precise Rietveld analysis of time-of-flight powder neutron diffraction data. Without an accurate incident spectrum the calculated model for the measured relative intensities of individual Bragg reflections will possess systematic errors. We describe a method for obtaining an accurate numerical incident spectrum using data from a transmitted beam monitor

  15. Proceedings of the 1986 workshop on advanced time-of-flight neutron powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Lawson, A.C.; Smith, K. (comps.)

    1986-09-01

    This report contains abstracts of talks and summaries of discussions from a small workshop held to discuss the future of time-of-flight neutron powder diffraction and its implementation at the Los Alamos Neutron Scattering Center. 47 refs., 3 figs.

  16. Application of 2-dimensional coordinate system conversion in stress measurements with neutron diffraction

    International Nuclear Information System (INIS)

    Wang, D.-Q.; Hubbard, C.R.; Spooner, S.

    2000-01-01

    This paper will present a method and program to precisely calculate the coordinates in a positioner coordinate system from given sample position coordinates with a minimum number of neutron surface scans for three possible circumstances in stress and texture measurement using neutron diffraction

  17. Proceedings of the 1986 workshop on advanced time-of-flight neutron powder diffraction

    International Nuclear Information System (INIS)

    Lawson, A.C.; Smith, K.

    1986-09-01

    This report contains abstracts of talks and summaries of discussions from a small workshop held to discuss the future of time-of-flight neutron powder diffraction and its implementation at the Los Alamos Neutron Scattering Center. 47 refs., 3 figs

  18. Influence of multiple small-angle neutron scattering on diffraction peak broadening in ferritic steel

    Czech Academy of Sciences Publication Activity Database

    Woo, W.; Em, V.; Shin, E.; Mikula, Pavol; Ryukhtin, Vasyl

    2015-01-01

    Roč. 48, APR (2015), s. 350-356 ISSN 0021-8898 R&D Projects: GA ČR GB14-36566G; GA MŠk(CZ) LM2011019 Institutional support: RVO:61389005 Keywords : peak broadening * small-angle neutron scattering * neutron diffraction * magnetic domain Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.720, year: 2014

  19. Stress measurement by neutron diffraction method. Standard method using angular dispersion method and trial of using neutron IP

    International Nuclear Information System (INIS)

    Sasaki, Toshihiko; Takago, Shigeki

    2016-01-01

    This paper outlined a stress measurement method using neutrons, and introduced the application examples to stress measurement for metal-based composite materials. In the angular dispersion type measurement using a steady-state reactor type neutron source, the white beams taken out from a nuclear reactor are monochromatized (wavelength λ is a constant value) with a single crystal monochromator and utilized. As an example of measurement, there was the case as follows: the stress of a sintered material which has been put to practical use as valve seat part for automobiles was measured by the neutron method, and the deformation behavior during load was studied. This study performed neutron diffraction measurement using a residual stress analyzer (RESA: Diffractometer for Residual Stress Analysis) installed at JAEA's experimental reactor JRR-3. As a result, it was found that the stress state of the sintered composite material of Fe-Cr and TiN can be predicted with a micromechanics model. A neutron diffraction ring can be obtained using a neutron image plate (IP), where fine powder of gadolinium (Gd) was incorporated into IP for X-rays, and it can be used as an IP reader in the same way as the case of X-rays. A report has been introduced on the examination results of the highly accurate stress measurement by applying the cos α method devised for X-ray stress measurement to neutron diffraction ring. (A.O.)

  20. Neutron irradiated uranium silicides studied by neutron diffraction and Rietveld analysis

    International Nuclear Information System (INIS)

    Birtcher, R.C.; Mueller, M.H.; Richardson, J.W. Jr.; Faber, J. Jr.

    1989-11-01

    Uranium silicides have been considered for use as reactor fuels in both high power and low enrichment applications. However, U 3 Si was found to become amorphous under irradiation and to become mechanically unstable to rapid growth by plastic flow. U 2 Si 2 appears to be stable against amorphization at low displacement rates, but the extent of this stability is uncertain. Although the mechanisms responsible for plastic flow in U 3 Si and other amorphous systems are unknown, as is the importance of crystal structure for amorphization, it may not be surprising that these materials amorphize, in light of the fact that many radioactive nuclide - containing minerals are known to metaminctize (lose crystallinity) under irradiation. The present experiment follows the detailed changes in the crystal structures of U 3 Si and U 3 Si 2 introduced by neutron bombardment and subsequent uranium fission at room temperature. U-Si seems the ideal system for a neutron diffraction investigation since the crystallographic and amorphous forms can be studied simultaneously by combining conventional Rietveld refinement of the crystallographic phases with Fourier-filtering of the non-crystalline scattering component

  1. Polarized neutron powder diffraction studies of antiferromagnetic order in bulk and nanoparticle NiO

    DEFF Research Database (Denmark)

    Brok, Erik; Lefmann, Kim; Deen, Pascale P.

    2015-01-01

    surface contribution to the magnetic anisotropy. Here we explore the potential use of polarized neutron diffraction to reveal the magnetic structure in NiO bulk and nanoparticle powders by applying the XYZ-polarization analysis method. Our investigations address in particular the spin orientation in bulk....... The results show that polarization analyzed neutron powder diffraction is a viable method to investigate magnetic order in powders of antiferromagnetic nanoparticles.......In many materials it remains a challenge to reveal the nature of magnetic correlations, including antiferromagnetism and spin disorder. Revealing the spin structure in magnetic nanoparticles is further complicated by the large incoherent neutron scattering cross section from water adsorbed...

  2. Setup for in situ X-ray diffraction studies of thin film growth by magnetron sputtering

    CERN Document Server

    Ellmer, K; Weiss, V; Rossner, H

    2001-01-01

    A novel method is described for the in situ-investigation of nucleation and growth of thin films during magnetron sputtering. Energy dispersive X-ray diffraction with synchrotron light is used for the structural analysis during film growth. An in situ-magnetron sputtering chamber was constructed and installed at a synchrotron radiation beam line with a bending magnet. The white synchrotron light (1-70 keV) passes the sputtering chamber through Kapton windows and hits one of the substrates on a four-fold sample holder. The diffracted beam, observed under a fixed diffraction angle between 3 deg. and 10 deg., is energy analyzed by a high purity Ge-detector. The in situ-EDXRD setup is demonstrated for the growth of tin-doped indium oxide (ITO) films prepared by reactive magnetron sputtering from a metallic target.

  3. Ultra-low-temperature neutron diffraction. Final report, July 1, 1983-June 30, 1985. Final report

    International Nuclear Information System (INIS)

    Halperin, W.P.; Ketterson, J.B.

    1985-07-01

    An ultra-low-temperature neutron diffraction facility has been constructed at Argonne National Laboratory. The initial and primary purpose of this facility is to study nuclear magnetic ordering phenomenon. Magnetic structure information is commonly recognized as being fundamental to the progress in theoretical and experimental efforts in the field of magnetism. We have initiated study of the nuclear spin in solid 3 He and in metals. In 3 He the nuclear spins order at 1.1 mK. Structure information for neutron diffraction would contribute significantly to this problem of nuclear magnetism. Despite substantial experimental difficulties, careful evaluation suggests that examination of the nuclear structure in this unique quantum crystal is indeed feasible by neutron diffraction. Substantial progress has been made in growing single crystals of 3 He and establishing its temperature in the presence of a neutron flux. We have also initiated investigation of nuclear ordering in copper and PrCu 6

  4. Alternative technique to neutron probe calibration in situ

    International Nuclear Information System (INIS)

    Encarnacao, F.; Carneiro, C.; Dall'Olio, A.

    1990-01-01

    An alternative technique of neutron probe calibration in situ was applied for Podzolic soil. Under field condition, the neutron probe calibration was performed using a special arrangement that prevented the lateral movement of water around the access tube of the neutron probe. During the experiments, successive amounts of water were uniformly infiltrated through the soil profile. Two plots were set to study the effect of the plot dimension on the slope of the calibration curve. The results obtained shown that the amounts of water transferred to the soil profile were significantly correlated to the integrals of count ratio along the soil profile on both plots. In consequence, the slope of calibration curve in field condition was determined. (author)

  5. Investigation of solid solution of hydrogen in α-manganese by neutron diffraction and inelastic neutron scattering

    International Nuclear Information System (INIS)

    Fedotov, V.K.; Antonov, V.E.; Kolesnikov, A.I.; Kornell, K.; Vipf, G.; Grosse, G.; Vagner, F.Eh.; Sikolenko, V.V.; Sumin, V.V.; )

    1997-01-01

    The FCC-lattice of the solid solution α-MnH 0.073 with the mass of 8.45 g is investigated by the neutron diffraction method and the inelastic neutron scattering technique. The neutron diffraction measurements are made by the diffractometer D1B with pyrographite monochromator and the high-resolution Fourier diffractometer HRFD at 300 K. The study of the inelastic incoherent neutron scattering is carried out by means of the inverse geometry spectrometer KDSOG-M at 90 K. The comparative analysis of α-MnH 0.073 and α-Mn spectra is fulfilled for the more correct separation of effects of hydrogen introduction. It is found out that the structure of the solid solution α-MnH 0.073 belongs to the same spatial group I-43m as the structure of α-Mn [ru

  6. Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials.

    Science.gov (United States)

    Kulriya, P K; Singh, F; Tripathi, A; Ahuja, R; Kothari, A; Dutt, R N; Mishra, Y K; Kumar, Amit; Avasthi, D K

    2007-11-01

    An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

  7. Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials

    Science.gov (United States)

    Kulriya, P. K.; Singh, F.; Tripathi, A.; Ahuja, R.; Kothari, A.; Dutt, R. N.; Mishra, Y. K.; Kumar, Amit; Avasthi, D. K.

    2007-11-01

    An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T =255K.

  8. 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.

  9. Texture investigation in aluminium and iron - silicon samples by neutron diffraction technique

    International Nuclear Information System (INIS)

    Pugliese, R.; Yamasaki, J.M.

    1988-09-01

    By means of the neutron diffraction technique the texture of 5% and 98% rolled-aluminium and of iron-silicon steel used in the core of electric transformers, have been determined. The measurements were performed by using a neutron diffractometer installed at the IEA-R1 Nuclear Research Reactor, in the Beam-Hole n 0 . 6. To avoid corrections such as neutron absorption and sample luminosity the geometric form of the samples were approximated to spheric or octagonal prism, and its dimensions do not exceed that of the neutron beam. The texture of the samples were analysed with the help of a computer programme that analyses the intensity of the diffracted neutron beam and plot the pole figures. (author) [pt

  10. The internal stress measurement the neutron diffraction bring happiness to your country

    Energy Technology Data Exchange (ETDEWEB)

    Minakawa, Nobuaki [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment

    2003-03-01

    The neutron was discovered by Chadwick in 1932. The first reactor was constructed by the USA in 1942. After that, the research and development of reactors advanced. Numbers of reactors were constructed in Europe and in the US. The researches, which use the neutron, were performed actively and excellent results were obtained in wide fields. The penetrating power of the neutron and the neutron diffraction method began to attract attention for the application to the internal stress measurement, too. In Japan, the neutron diffractometer for the residual stress measurement exclusive was installed in the JRR-3M research reactor of JAERI in 1992, and the research was started. At present, we are using it for the stress measurements of the parts of aircrafts, railways, automobiles, buildings, machines, home electronics products and so on including nuclear reactors. Reliable science must be introduced in order to support safety and long life operation and to supply them at reasonable cost. Among the various scientific probes to find faults in materials, diffraction technique is used to measure the strain distribution in materials by observing the local changes of the distance between crystallographic planes and the stress distribution is computed to improve manufacturing processes. It is only neutron diffraction that can be used to measure the strain inside the materials. Here, I present an overview of the utilization of neutron scattering research for the industrial uses and the history of the neutron scattering research in JAERI briefly. (J.P.N.)

  11. The internal stress measurement the neutron diffraction will bring happiness to your country

    International Nuclear Information System (INIS)

    Minakawa, Nobuaki

    2003-01-01

    The neutron was discovered by Chadwick in 1932. The first reactor was constructed by the USA in 1942. After that, the research and development of reactors advanced. Numbers of reactors were constructed in Europe and in the US. The researches, which use the neutron, were performed actively and excellent results were obtained in wide fields. The penetrating power of the neutron and the neutron diffraction method began to attract attention for the application to the internal stress measurement, too. In Japan, the neutron diffractometer for the residual stress measurement exclusive was installed in the JRR-3M research reactor of JAERI in 1992, and the research was started. At present, we are using it for the stress measurements of the parts of air crafts, railways, automobiles, buildings, machines, home electronics products and so on including nuclear reactors. Reliable science must be introduced in order to support safety and long life operation and to supply them at reasonable cost. Among the various scientific probes to find faults in materials, diffraction technique is used to measure the strain distribution in materials by observing the local changes of the distance between crystallographic planes and the stress distribution is computed to improve manufacturing processes. It is only neutron diffraction that can be used to measure the strain inside the materials. Here, I present an overview of the utilization of neutron scattering research for the industrial uses and the history of the neutron scattering research in JAERI briefly. (J.P.N.)

  12. Residual stress distribution in carbon steel pipe welded joint measured by neutron diffraction

    International Nuclear Information System (INIS)

    Hayashi, Makoto; Ishiwata, Masayuki; Morii, Yukio; Minakawa, Nobuaki

    2000-01-01

    In order to estimate crack growth behavior of fatigue and stress corrosion cracking in pipes, the residual stress distribution near the pipe weld region has to be measured through the wall thickness. Since the penetration depth of neutron is deep enough to pass through the thick pipe wall, the neutron diffraction technique for the residual stress measurement is effective for this purpose. At the first step the residual stress distribution near the weld region in a butt-welded carbon steel pipe was measured by the neutron diffraction. Significant stresses extended only to a distance of 30 mm from the center of the weld. The major tensile stresses occurred in the hoop direction in the fusion and heat affected zones of the weldment, and they attained a level greater than 200 MPa through the thickness. While the axial residual stress at the inside surface was 50 MPa, the stress at the outside surface was -100 MPa. The comparison of residual stress distributions measured by the neutron diffraction, the X-ray diffraction and the strain gauge method reveals that the neutron diffraction is the most effective for measuring the residual stress inside the structural components. (author)

  13. Neutron and X-ray diffraction from modulated structures

    International Nuclear Information System (INIS)

    Harris, P.

    1994-07-01

    This thesis describes X-ray and neutron scattering experiments performed on two examples of modulated structures. After an introduction to the subject of modulated structures, the thesis is divided in three parts. A single crystal elastic neutron scattering experiment between 4.2 and 115 Κ has been performed and four-circle X-ray data have been collected at 8 Κ for the monoclinic low-temperature phase of the layered perovskite PAMC. The results from the neutron scattering experiment indicate that magnetoelastic effects influence the ordering of the crystal. The X-ray experiments have made it possible to determine the crystal structure in the low-temperature phase. The superspace group is P2 1 /b(β-30)Os, with β = 1/3. A small-angle neutron scattering experiment has been performed on the magnetic structure of manganese silicide. When a magnetic field is applied, the modulation vectors turn towards the field direction, showing domain growth and diverging peak widths as they approach the field direction. Phase 'A' is established to have the modulation vectors directed perpendicular to the field direction. Cooling in zero field shows increasing peak widths at low temperatures, indicating a lock-in transition below the lowest reached temperature. To be able to analyse the data of the magnetic order in MnSi, and analytical calculation of the three dimensional resolution function for a small-angle neutron scattering spectrometer has been performed. The calculation is done by application of a combination of phase space analysis and Gaussian approximations for the neutron distribution as well as for the transmission functions of the different apertures. A finite mosaic spread of the crystal and finite correlation widths of the Bragg reflections have been included in the cross section. (au) (3 tabs., 48 ills., 100 refs.)

  14. A preliminary neutron diffraction study of rasburicase, a recombinant urate oxidase enzyme, complexed with 8-azaxanthin

    Energy Technology Data Exchange (ETDEWEB)

    Budayova-Spano, Monika, E-mail: spano@embl-grenoble.fr [European Molecular Biology Laboratory Grenoble Outstation, 6 Rue Jules Horowitz, 38042 Grenoble (France); Institut Laue-Langevin, 6 Rue Jules Horowitz, BP 156, 38042 Grenoble (France); Bonneté, Françoise; Ferté, Natalie [Centre de Recherche en Matière Condensée et Nanosciences, Campus de Luminy, Case 913, 13288 Marseille (France); El Hajji, Mohamed [Sanofi-Aventis, 371 Rue du Professeur Blayac, 34184 Montpellier (France); Meilleur, Flora [Institut Laue-Langevin, 6 Rue Jules Horowitz, BP 156, 38042 Grenoble (France); Blakeley, Matthew Paul [European Molecular Biology Laboratory Grenoble Outstation, 6 Rue Jules Horowitz, 38042 Grenoble (France); Castro, Bertrand [Sanofi-Aventis, 371 Rue du Professeur Blayac, 34184 Montpellier (France); European Molecular Biology Laboratory Grenoble Outstation, 6 Rue Jules Horowitz, 38042 Grenoble (France)

    2006-03-01

    Neutron diffraction data of hydrogenated recombinant urate oxidase enzyme (Rasburicase), complexed with a purine-type inhibitor 8-azaxanthin, was collected to 2.1 Å resolution from a crystal grown in D{sub 2}O by careful control and optimization of crystallization conditions via knowledge of the phase diagram. Deuterium atoms were clearly seen in the neutron-scattering density map. Crystallization and preliminary neutron diffraction measurements of rasburicase, a recombinant urate oxidase enzyme expressed by a genetically modified Saccharomyces cerevisiae strain, complexed with a purine-type inhibitor (8-azaxanthin) are reported. Neutron Laue diffraction data were collected to 2.1 Å resolution using the LADI instrument from a crystal (grown in D{sub 2}O) with volume 1.8 mm{sup 3}. The aim of this neutron diffraction study is to determine the protonation states of the inhibitor and residues within the active site. This will lead to improved comprehension of the enzymatic mechanism of this important enzyme, which is used as a protein drug to reduce toxic uric acid accumulation during chemotherapy. This paper illustrates the high quality of the neutron diffraction data collected, which are suitable for high-resolution structural analysis. In comparison with other neutron protein crystallography studies to date in which a hydrogenated protein has been used, the volume of the crystal was relatively small and yet the data still extend to high resolution. Furthermore, urate oxidase has one of the largest primitive unit-cell volumes (space group I222, unit-cell parameters a = 80, b = 96, c = 106 Å) and molecular weights (135 kDa for the homotetramer) so far successfully studied with neutrons.

  15. Martensite phase stress and the strengthening mechanism in TRIP steel by neutron diffraction.

    Science.gov (United States)

    Harjo, Stefanus; Tsuchida, Noriyuki; Abe, Jun; Gong, Wu

    2017-11-09

    Two TRIP-aided multiphase steels with different carbon contents (0.2 and 0.4 mass%) were analyzed in situ during tensile deformation by time-of-flight neutron diffraction to clarify the deformation induced martensitic transformation behavior and its role on the strengthening mechanism. The difference in the carbon content affected mainly the difference in the phase fractions before deformation, where the higher carbon content increased the phase fraction of retained austenite (γ). However, the changes in the relative fraction of martensitic transformation with respect to the applied strain were found to be similar in both steels since the carbon concentrations in γ were similar regardless of different carbon contents. The phase stress of martensite was found much larger than that of γ or bainitic ferrite since the martensite was generated at the beginning of plastic deformation. Stress contributions to the flow stress were evaluated by multiplying the phase stresses and their phase fractions. The stress contribution from martensite was observed increasing during plastic deformation while that from bainitic ferrite hardly changing and that from γ decreasing.

  16. Neutron diffraction study of the deformation mechanisms of the uranium-7 wt.% niobium shape memory alloy

    Energy Technology Data Exchange (ETDEWEB)

    Brown, D.W. [Los Alamos National Lab, Los Alamos, NM 87545 (United States)]. E-mail: dbrown@lanl.gov; Bourke, M.A.M. [Los Alamos National Lab, Los Alamos, NM 87545 (United States); Field, R.D. [Los Alamos National Lab, Los Alamos, NM 87545 (United States); Hults, W.L. [Los Alamos National Lab, Los Alamos, NM 87545 (United States); Teter, D.F. [Los Alamos National Lab, Los Alamos, NM 87545 (United States); Thoma, D.J. [Los Alamos National Lab, Los Alamos, NM 87545 (United States); Vogel, S.C. [Los Alamos National Lab, Los Alamos, NM 87545 (United States)

    2006-04-15

    The shape memory effect (SME) has been reported in the uranium-niobium alloy system in the region of the phase diagram surrounding U-6.5 wt.% Nb. In this regime, the material may have either an {alpha}'' monoclinic (U-6 wt.% Nb), or {gamma}{sup 0} tetragonal structure (U-7 wt.% Nb) and is two phase near 6.5 wt.% niobium. In situ neutron diffraction studies during uniaxial compressive loading of U-7 wt.% Nb indicate that strain in the recoverable region is accommodated by both motion of existing twin boundaries within {gamma}{sup 0}-phase and stress-induced phase transformation from the {gamma}{sup 0} to the {alpha}'' structure. The volume fraction of the {gamma}{sup 0}-phase decreases from 100% initially to {approx}26% after 4% total strain and some reversion is observed on release. The initial stress state of the stress-induced {alpha}'' grains will be discussed as well as the load sharing between the two phases.

  17. Modelamiento del proceso de carbonatación del hormigón (UR-CORE, con datos de conversión fraccional obtenidos a través de experimentos de difracción de neutrones monitoreados in-situ Modelling of the carbonation of concrete (UR-CORE from fractionafconversion data obtained through in situ monitored neutrón diffraction experiments

    Directory of Open Access Journals (Sweden)

    Marta Castellote

    2009-12-01

    Full Text Available Una de las principales causas de despasivación de las armaduras embebidas en hormigón es la denominada carbonatación, que consiste en la neutralización de la matriz de cemento como consecuencia de su interacción con el C0(2 atmosférico. En este trabajo, se presenta un resumen del desarrollo de un modelo de carbonatación de las matrices de base cemento (UR-CORE. En primer lugar se ha llevado a cabo la carbonatación acelerada (al 100% de C0(2 sobre probetas de pasta de cemento con distintas matrices cementantes tomando espectros de Difracción de Neutrones a lo largo del tiempo de experimento. La evolución de la intensidad de los picos correspondientes a cada una de las fases involucradas ha proporcionado datos de conversión fraccional en tiempo real, lo que ha posibilitado una aproximación cinética al fenómeno de la carbonatación y el desarrollo del modelo UR-CORE, basado en los principios de los sistemas de "núcleo sin reaccionar", típicos de los procesos en ingeniería química.One of the most important depassivation mechanisms of steel reinforcement in concrete is that caused by the neutralisation of the cement matrix. In this work, a summary of the development of a model for the carbonation of cementitious matrixes (UR-CORE is presented. On one hand, in-situ monitoring of the changes that take place in the phase composition of cement pastes during accelerated carbonation (100% C02 for different binders, is reported, by taking Neutrón Diffraction patterns in parallel with the carbonation experiments. The variation of the intensity of chosen reflections for each phase along the experiment supplied data, in real time, for fractional conversión of different phases. On the second hand, fitting of these results allowed to make a quantitative approach to the kinetics of the carbonation of the different phases, and develop the UR-CORE model that is based on the principies of the "unreacted-core" systems, typical of chemical

  18. In Situ X-ray Diffraction Studies of (De)lithiation Mechanism in Silicon Nanowire Anodes

    KAUST Repository

    Misra, Sumohan; Liu, Nian; Nelson, Johanna; Hong, Seung Sae; Cui, Yi; Toney, Michael F.

    2012-01-01

    -Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li 15Si 4 phase forms

  19. Study of FeC1{sub 2} by neutron diffraction; Etude de Fe C1{sub 2} par diffraction de neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Herpin, A; Meriel, P [Commissariat a l' Energie Atomique, Saclay (France)

    1959-07-01

    Magnetic measurements have shown that anhydrous ferrous chloride behaves as a metamagnetic at temperatures below 24 deg. K, in other words as an antiferromagnetic sensitive to the action of an external field of moderate strength. The aim of the neutron diffraction study is to determine precisely the arrangement of the magnetic moments, and to follow its evolution as a function of the applied field. (author) [French] Des mesures magnetiques ont montre que le chlorure ferreux anhydre se comporte comme un metamagnetique a une temperature inferieure a 24 deg. K, c'est a dire comme un antiferromagnetique sensible a l'action d'un champ exterieur modere. L'etude par diffraction de neutrons a pour buts de preciser la disposition des moments magnetiques et de suivre son evolution en fonction du champ applique. (auteur)

  20. Study of FeC1{sub 2} by neutron diffraction; Etude de Fe C1{sub 2} par diffraction de neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Herpin, A.; Meriel, P. [Commissariat a l' Energie Atomique, Saclay (France)

    1959-07-01

    Magnetic measurements have shown that anhydrous ferrous chloride behaves as a metamagnetic at temperatures below 24 deg. K, in other words as an antiferromagnetic sensitive to the action of an external field of moderate strength. The aim of the neutron diffraction study is to determine precisely the arrangement of the magnetic moments, and to follow its evolution as a function of the applied field. (author) [French] Des mesures magnetiques ont montre que le chlorure ferreux anhydre se comporte comme un metamagnetique a une temperature inferieure a 24 deg. K, c'est a dire comme un antiferromagnetique sensible a l'action d'un champ exterieur modere. L'etude par diffraction de neutrons a pour buts de preciser la disposition des moments magnetiques et de suivre son evolution en fonction du champ applique. (auteur)

  1. Refractive and diffractive neutron optics with reduced chromatic aberration

    DEFF Research Database (Denmark)

    Poulsen, Stefan Othmar; Poulsen, Henning Friis; Bentley, P.M.

    2014-01-01

    by the use of optics for focusing and imaging. Refractive and diffractive optical elements, e.g. compound refractive lenses and Fresnel zone plates, are attractive due to their low cost, and simple alignment. These optical elements, however, suffer from chromatic aberration, which limit their effectiveness...

  2. Electrochemical cell for in situ x-ray diffraction under ultrapure conditions

    DEFF Research Database (Denmark)

    Koop, T.; Schindler, W.; Kazimirov, A.

    1998-01-01

    within a few seconds. The oxygen level in the electrolyte is reduced by continuous N(2) flow to less than 0.2% compared to that of a fresh electrolyte. This can be done while rotating the cell by 360 degrees about the surface normal. The electrode potential is accurately measured at the position......An electrochemical cell has been developed for in situ x-ray diffraction from a working electrode under clean conditions equivalent to ultrahigh vacuum conditions of 5 x 10(-10) mbar. The substrate crystals can be prepared ex situ and transferred into the cell under protection of ultrapure water...... of the crystal using a Luggin capillary and a standard reference electrode. We demonstrate the performance of our cell by in situ synchrotron x-ray diffraction measurements on ultrathin Co layers electrodeposited on Cu(001) in an aqueous H(2)SO(4)/CoSO(4) solution. (C) 1998 American Institute of Physics....

  3. Analysis of neutron diffraction peak broadening caused by internal stresses in composite materials

    International Nuclear Information System (INIS)

    Todd, R.I.; Borsa, C.; Derby, B.

    1994-01-01

    Neutron diffraction is an essential tool in the study of internal stresses in composite materials. In most work only the peak shifts caused by the related elastic strains are considered, but other valuable information exists in the form of peak shape changes. The conditions under which the pure diffraction profile of the composite (i.e. the profile when all sources of broadening not caused by the residual stresses are removed) represents the probability distribution of the peak shifts corresponding to the strains are examined. It is shown that in these conditions, the pure diffraction profile has no attributes of particle size broadening (and vice versa), thereby providing a test for the validity of results interpreted in this way. The experimental derivation of measured strain distributions in Al 2 O 3 /SiCp composites using neutron diffraction is described. No apparent particle size broadening was detected, demonstrating the validity of the results, which also satisfied other tests for consistency

  4. Performance of novel moderator for pulsed neutron diffraction

    International Nuclear Information System (INIS)

    Mayer, R.E.; Granada, J.R.; Dawidowski, J.; Gillette, V.H.

    1991-01-01

    Measurements of neutron pulse time-width and intensity have been carried out on grids of small moderators placed side by side and decoupled by cadmium strips. This moderator concept had been introduced at ICANS-10. The present measurements explore greater moderator thicknesses than those previously attained, yielding information on thickness optimization, while confirming the previous results on resolution which make this moderator a favourable choice in front of the conventional sandwich set-up. (author)

  5. Through-thickness Residual Stress Measurement by Neutron Diffraction in Cu+W Plasma Spray Coatings

    Czech Academy of Sciences Publication Activity Database

    Luzin, V.; Matějíček, Jiří; Gnäupel-Herold, T.

    2010-01-01

    Roč. 652, č. 652 (2010), s. 50-56 ISSN 1662-9752. [International Conference on Mechanical Stress Evaluation by Neutrons and Synchrotron Radiation/5th./. Mito, 10.11.2009-12.11.2009] R&D Projects: GA MŠk ME 901 Institutional research plan: CEZ:AV0Z20430508 Keywords : fusion materials * plasma sprayed coatings * residual stress * neutron diffraction Subject RIV: JG - Metallurgy http://www.scientific.net/MSF.652.50

  6. The use of pulsed neutron diffraction to measure strain in composites

    International Nuclear Information System (INIS)

    Bourke, M.A.M.; Goldstone, J.A.; Shi, N.; Gray, G.T. III; James, M.R.

    1994-01-01

    Neutron diffraction is a technique for measuring strain in crystalline materials. It is non destructive, phase discriminatory and more penetrating than X rays. Pulsed neutron sources (in contrast with steady state reactor sources) are particularly appropriate for examining heterogeneous materials or for recording the polycrystalline response of all lattice reflections. Several different aspects of composite behavior can be characterized and examples are given of residual strain measurements, strain relaxation during heating, applied loading, and determination of the strain distribution function

  7. Time-of-Flight Three Dimensional Neutron Diffraction in Transmission Mode for Mapping Crystal Grain Structures

    DEFF Research Database (Denmark)

    Cereser, Alberto; Strobl, Markus; Hall, Stephen A.

    2017-01-01

    constituting the material. This article presents a new non-destructive 3D technique to study centimeter-sized bulk samples with a spatial resolution of hundred micrometers: time-of-flight three-dimensional neutron diffraction (ToF 3DND). Compared to existing analogous X-ray diffraction techniques, ToF 3DND......-of-flight neutron beamline. The technique was developed and tested with data collected at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Complex (J-PARC) for an iron sample. We successfully reconstructed the shape of 108 grains and developed an indexing procedure...

  8. Locations of oxygen, nitrogen and carbon atoms in vanadium determined by neutron diffraction

    International Nuclear Information System (INIS)

    Hiraga, K.; Onozuka, T.; Hirabayashi, M.

    1977-01-01

    The occupation sites of oxygen, nitrogen, and carbon atoms dissolved interstitially in vanadium have been determined by means of neutron diffraction with use of single crystals of VOsub(0.032), VNsub(0.013) and VCsub(0.006). It is revealed that the interstitial atoms occupy, randomly, the octahedral sites in the b.c.c. host lattice of the three crystals. Neutron diffraction is advantageous for the present purpose, since the coherent scattering amplitudes of the solute atoms are much larger than that of the vanadium atom. (Auth.)

  9. Molecular structure and correlations in liquid D-2-propanol through neutron diffraction

    International Nuclear Information System (INIS)

    Sahoo, A.; Sarkar, S.; Joarder, R.N.; Krishna, P.S.R.

    2003-01-01

    Like t-butanol, 2-propanol molecules are quite big with substantial amount of asymmetry in the structure and so the analysis of the neutron diffraction data is tricky. A modified method of analysis, similar to one for liquid t-butanol, enables extraction of the detailed molecular conformation and intermolecular correlations through neutron diffraction. The pre-peak in the structure function, a signature of chain molecular association together with partially identified inter-molecular correlations yield some information about the nature of possible H-bonded molecular clusters in the liquid state. (author)

  10. ATALANTA: a multicomponent pulsed neutron diffraction analysis code

    International Nuclear Information System (INIS)

    Benham, M.J.; Ross, D.K.

    1986-01-01

    The analysis of powder diffraction patterns from metal hydrogen systems present certain problems which have been addressed in a restructured profile analysis program. The heart of this program, ATALANTA, is a routine which locates and processes small sections of the data field to which a minimal number of Bragg peaks contribute intensity. The analysis of a three component test data set is presented in order to demonstrate the method. (author)

  11. 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.

  12. Neutron Diffraction Studies of Nuclear Magnetic Ordering in Copper

    DEFF Research Database (Denmark)

    Jyrkkiö, T.A.; Huiku, M.T.; Siemensmeyer, K.

    1989-01-01

    for measurements in the ordered state; both our calculations and the experiments yield 1 nW beam heating. Polarized neutron experiments show that the scattered intensities from the strong fcc reflections are severely reduced by extinction. This makes the sample not very suitable for further studies with polarized...... to depend strongly on the external magnetic field between zero and the critical fieldB c=0.25 mT, indicating the existence of at least two antiferromagnetic phases. The results are compared to previous measurements of the magnetic susceptibility. Theoretical calculations do not provide a full explanation...

  13. Condensed matter and materials research using neutron diffraction and spectroscopy: reactor and pulsed neutron sources

    International Nuclear Information System (INIS)

    Bisanti, Paola; Lovesey, S.W.

    1987-05-01

    The paper provides a short, and partial view of the neutron scattering technique applied to condensed matter and materials research. Reactor and accelerator-based neutron spectrometers are discussed, together with examples of research projects that illustrate the puissance and modern applications of neutron scattering. Some examples are chosen to show the range of facilities available at the medium flux reactor operated by Casaccia ENEA, Roma and the advanced, pulsed spallation neutron source at the Rutherford Appleton Laboratory, Oxfordshire. (author)

  14. Crystallite Size and Microstrain Measurement of Cathode Material after Mechanical Milling using Neutron Diffraction Technique

    Directory of Open Access Journals (Sweden)

    A. Fajar

    2010-12-01

    Full Text Available The measurements of neutron diffraction patterns of commercially product and 10 hour mechanically milled cathode material lithium cobaltites (LiCoO2 have been performed. Rietveld analysis using FullProf does not show the change of crystal structure due to milling process, but the diffraction pattern has a lower intensity and the diffraction-line was broadening. The results of line-broadening study on milled sample using Rietveld methods detected that the microstrain was occurred in the sample with value 0.127080(35 % and the average crystallite size was 424.78(20 Å.

  15. Diffraction plane dependency of elastic constants in ferritic steel in neutron stress measurement

    International Nuclear Information System (INIS)

    Hayashi, M.; Ishiwata, M.; Minakawa, N.; Funahashi, S.

    1993-01-01

    Neutron diffraction measurements have been made to investigate the elastic properties of the ferritic steel obtained from socket weld. The Kroner elastic model is found to account for the [hkl]-dependence of Young's modulus and Poisson's ratio in the material. Maps of residual stress are later to be made by measuring lattice strain from shifts in the (112) diffraction peak, for which the diffraction elastic constants the herein found to be E=243±5GPa and ν=0.28±0.01. (author)

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

    International Nuclear Information System (INIS)

    Eveno, Myriam; Duran, Adrian; Castaing, Jacques

    2010-01-01

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

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

    Science.gov (United States)

    Eveno, Myriam; Duran, Adrian; Castaing, Jacques

    2010-09-01

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

  18. In situ diffraction profile analysis during tensile deformation motivated by molecular dynamics

    International Nuclear Information System (INIS)

    Van Swygenhoven, H.; Budrovic, Z.; Derlet, P.M.; Froseth, A.G.; Van Petegem, S.

    2005-01-01

    Molecular dynamics simulations can provide insight into the slip mechanism at the atomic scale and suggest that in nanocrystalline metals dislocations are nucleated and absorbed by the grain boundaries. However, this technique is limited by very short simulation times. Using suggestions from molecular dynamics, we have developed a new in situ X-ray diffraction technique wherein the profile analysis of several Bragg diffraction peaks during tensile deformation is possible. Combining experiment and careful structural analysis the results confirm the suggestions from atomistic simulations

  19. Single-crystal neutron diffraction studies of hydrogen-bonded systems: Two recent examples from IPNS

    Energy Technology Data Exchange (ETDEWEB)

    Koetzle, Thomas F. [IPNS Division, Argonne National Laboratory, Argonne, IL 60439 (United States)], E-mail: tkoetzle@anl.gov; Piccoli, Paula M.B.; Schultz, Arthur J. [IPNS Division, Argonne National Laboratory, Argonne, IL 60439 (United States)

    2009-02-21

    Beginning with work in the 1950s at the first generation of research reactors, studies of hydrogen-bonded systems have been a prime application for single-crystal neutron diffraction. The range of systems studied was extended in the 1960s and 1970s, with the advent of high flux reactor sources, and beginning around 1980 studies at pulsed neutron sources have made increasingly important contributions. Recently at the Argonne Intense Pulsed Neutron Source (IPNS), working with collaborators, we completed two studies of hydrogen-bonded systems that will serve to illustrate topics of current interest. In the first study, on andrographolide, an active diterpenoid natural product, our neutron diffraction results definitively characterize the hydrogen-bonding interactions. The second IPNS study is on tetraacetylethane (TAE), a {beta}-diketone enol system with a very short, strong intramolecular O-H...O hydrogen bond. At IPNS, we have determined the neutron crystal structure of TAE at five temperatures between 20 and 298 K to investigate changes in the structure with temperature and to probe for disorder. Despite the successes illustrated by the two examples presented here and by many other studies, at present applications of single-crystal neutron diffraction continue to be extremely flux limited and constrained by the requirement for mm-size crystals for many problems. These limitations are being addressed through the realization of powerful instruments at a new generation of pulsed neutron sources, including in the USA the TOPAZ and MaNDi single-crystal diffractometers that are under development at the Spallation Neutron Source (SNS)

  20. Single-crystal neutron diffraction studies of hydrogen-bonded systems: Two recent examples from IPNS

    Science.gov (United States)

    Koetzle, Thomas F.; Piccoli, Paula M. B.; Schultz, Arthur J.

    2009-02-01

    Beginning with work in the 1950s at the first generation of research reactors, studies of hydrogen-bonded systems have been a prime application for single-crystal neutron diffraction. The range of systems studied was extended in the 1960s and 1970s, with the advent of high flux reactor sources, and beginning around 1980 studies at pulsed neutron sources have made increasingly important contributions. Recently at the Argonne Intense Pulsed Neutron Source (IPNS), working with collaborators, we completed two studies of hydrogen-bonded systems that will serve to illustrate topics of current interest. In the first study, on andrographolide, an active diterpenoid natural product, our neutron diffraction results definitively characterize the hydrogen-bonding interactions. The second IPNS study is on tetraacetylethane (TAE), a β-diketone enol system with a very short, strong intramolecular O-H⋯O hydrogen bond. At IPNS, we have determined the neutron crystal structure of TAE at five temperatures between 20 and 298 K to investigate changes in the structure with temperature and to probe for disorder. Despite the successes illustrated by the two examples presented here and by many other studies, at present applications of single-crystal neutron diffraction continue to be extremely flux limited and constrained by the requirement for mm-size crystals for many problems. These limitations are being addressed through the realization of powerful instruments at a new generation of pulsed neutron sources, including in the USA the TOPAZ and MaNDi single-crystal diffractometers that are under development at the Spallation Neutron Source (SNS).

  1. Single-crystal neutron diffraction studies of hydrogen-bonded systems: Two recent examples from IPNS

    International Nuclear Information System (INIS)

    Koetzle, Thomas F.; Piccoli, Paula M.B.; Schultz, Arthur J.

    2009-01-01

    Beginning with work in the 1950s at the first generation of research reactors, studies of hydrogen-bonded systems have been a prime application for single-crystal neutron diffraction. The range of systems studied was extended in the 1960s and 1970s, with the advent of high flux reactor sources, and beginning around 1980 studies at pulsed neutron sources have made increasingly important contributions. Recently at the Argonne Intense Pulsed Neutron Source (IPNS), working with collaborators, we completed two studies of hydrogen-bonded systems that will serve to illustrate topics of current interest. In the first study, on andrographolide, an active diterpenoid natural product, our neutron diffraction results definitively characterize the hydrogen-bonding interactions. The second IPNS study is on tetraacetylethane (TAE), a β-diketone enol system with a very short, strong intramolecular O-H...O hydrogen bond. At IPNS, we have determined the neutron crystal structure of TAE at five temperatures between 20 and 298 K to investigate changes in the structure with temperature and to probe for disorder. Despite the successes illustrated by the two examples presented here and by many other studies, at present applications of single-crystal neutron diffraction continue to be extremely flux limited and constrained by the requirement for mm-size crystals for many problems. These limitations are being addressed through the realization of powerful instruments at a new generation of pulsed neutron sources, including in the USA the TOPAZ and MaNDi single-crystal diffractometers that are under development at the Spallation Neutron Source (SNS).

  2. In situ x-ray diffraction studies of three-dimensional C60 polymers

    International Nuclear Information System (INIS)

    Wood, R A; Lewis, M H; Bennington, S M; Cain, M G; Kitamura, N; Fukumi, A K

    2002-01-01

    In situ investigations into the P/T field of C 60 fullerene were performed using energy-dispersive x-ray diffraction techniques. Isobars were obtained at 11 and 9 GPa accompanied by isotherms at 750 and 800 K with pressure reaching 13 GPa. The P/T history and pressure isotropy were investigated with the aim of optimizing conditions for 3D polymer formation. Confirmation of the formation of 3D polymers was performed in situ; however, the reclaimed sample did not exhibit the expected high hardness value, due to depolymerization on pressure release. Isotropy in the pressure field promoted formation and retention of the face-centred-cubic structure

  3. Textures of iron oxide ores by neutron diffraction and topotactical relation

    International Nuclear Information System (INIS)

    Wagner, F.; Esling, C.; Baro, R.; Englander, M.

    1977-01-01

    Two samples are cut from a polycrystalline haematite block. The first one is directly submitted to texture analysis by neutron diffraction, whereas the second one is first reduced into magnetite. The comparison of both textures is in agreement with a topotactical relationship previously reported for monocrystals. (orig.) [de

  4. Neutron diffraction measurements of residual stress in a powder metallurgy component

    International Nuclear Information System (INIS)

    Schneider, L.C.R.; Hainsworth, S.V.; Cocks, A.C.F.; Fitzpatrick, M.E.

    2005-01-01

    Residual stresses in a typical industrial green component were determined using neutron diffraction. The measured residual stresses were found to correlate with cross-sectional variations. Residual stress at the edge of the compact in contact with the die wall during compaction reached up to +80 MPa (tension) and -100 MPa (compression)

  5. Neutron diffraction from the vortex lattice in the heavy-fermion superconductor UPt3

    DEFF Research Database (Denmark)

    Kleiman, R.N.; Broholm, C.; Aeppli, G.

    1992-01-01

    We have used neutron diffraction to observe the vortex lattice of UPt3. This is the first such measurement in a heavy-fermion system, a superconductor below 1 K, or in a system with such a long magnetic penetration depth (6000 +/- 75 angstrom). It also provides the first value for the pair...

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Parrot, I. M. [Institut Laue-Langevin (ILL); Urban, Volker S [ORNL; Gardner, K. H. [DuPont Experimental Station; Forsyth, V. T. [Institut Laue Langevin and Keele University

    2005-04-01

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

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

    Science.gov (United States)

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

    2005-08-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Parrot, I.M. [Institut Laue Langevin, 6 Rue Jules Horowitz, 38042 Grenoble Cedex 9 (France); Institute of Science and Technology in Medicine, Keele University Medical School, Staffordshire ST4 7QB (United Kingdom); Urban, V. [Oak Ridge National Laboratory, P.O. Box 2008, Oak Ridge, TN 37831-6100 (United States); Gardner, K.H. [Department of Materials Science and Engineering University of Delaware, Newark, DE 19719 (United States); Forsyth, V.T. [Institut Laue Langevin, 6 Rue Jules Horowitz, 38042 Grenoble Cedex 9 (France) and Institute of Science and Technology in Medicine, Keele University Medical School, Staffordshire ST4 7QB (United Kingdom)]. E-mail: tforsyth@ill.fr

    2005-08-15

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

  10. Neutron diffraction study on the medium and short-range order of ternary chalcogenide glasses

    Czech Academy of Sciences Publication Activity Database

    Neov, S.; Gerasimova, I.; Skordeva, E.; Arsova, D.; Pamukchieva, V.; Mikula, Pavol; Lukáš, Petr; Sonntag, R.

    1999-01-01

    Roč. 34, - (1999), s. 3669-3676 ISSN 0022-2461 R&D Projects: GA ČR GV202/97/K038 Keywords : neutron diffraction * short-range order * chalcogenide glasses Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.786, year: 1999

  11. Neutron diffraction studies of Ho1-xYxNi2B2C compounds

    DEFF Research Database (Denmark)

    Chang, L.J.; Tomy, C.V.; Paul, D.M.K.

    1996-01-01

    Neutron diffraction measurements have been carried out to investigate the nature of magnetic ordering in Ho(1-x)Y(x)Ni(2)B(2)C (x = 0, 0.1 and 0.2) compounds. HoNi(2)B(2)C shows a complex type of magnetic ordering below the superconducting transition, with a commensurate antiferromagnetic ordering...

  12. Measurement of the velocity of sound in crystals by pulsed neutron diffraction

    International Nuclear Information System (INIS)

    Willis, B.T.M.; Carlile, C.J.; Ward, R.C.; David, W.I.F.; Johnson, M.W.

    1986-03-01

    The diffraction method of observing elementary excitations in crystals has been applied to the study of one-phonon thermal diffuse scattering from pyrolytic graphite on a high resolution pulsed neutron diffractometer. The variation of the phase velocity of sound as a function of direction in the crystal and efficient method of determining sound velocities in crystals under extreme conditions. (author)

  13. Analytical model for neutron diffraction peak shifts due to the surface effect

    Czech Academy of Sciences Publication Activity Database

    Šaroun, Jan; Kornmeier, J. R.; Hofmann, M.; Mikula, Pavol; Vrána, Miroslav

    2013-01-01

    Roč. 46, č. 6 (2013), s. 628-638 ISSN 0021-8898 R&D Projects: GA ČR GAP204/10/0654 Institutional support: RVO:61389005 Keywords : residual-stress * neutron diffraction * Monte Carlo simulation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.950, year: 2013

  14. Residual stresses in cold-coiled helical compression springs for automotive suspensions measured by neutron diffraction

    Czech Academy of Sciences Publication Activity Database

    Matějíček, Jiří; Brand, P. C.; Drews, A. R.; Krause, A.; Lowe-Ma, C.

    2004-01-01

    Roč. 367, 1-2 (2004), s. 306-311 ISSN 0921-5093 Institutional research plan: CEZ:AV0Z2043910 Keywords : residual stress, automotive springs, neutron diffraction Subject RIV: JB - Sensors, Measurment, Regulation Impact factor: 1.445, year: 2004

  15. Experimental evaluation of a polycrystal deformation modeling scheme using neutron diffraction measurements

    DEFF Research Database (Denmark)

    Clausen, Bjørn; Lorentzen, Torben

    1997-01-01

    The uniaxial behavior of aluminum polycrystals is simulated using a rate-independent incremental self-consistent elastic-plastic polycrystal deformation model, and the results are evaluated by neutron diffraction measurements. The elastic strains deduced from the model show good agreement...

  16. Neutron Diffraction from the Second Layer of 4He on Graphite

    DEFF Research Database (Denmark)

    da Costa Carneiro, Kim; Passell, L.; Thomlinson, W.

    1981-01-01

    Neutron diffraction has been used to study the second atomic layer of **4He adsorbed on graphite. As the **4He-coverage exceeds the first layer, the second initially forms a fluid phase. But when there is enough **4He in the third layer to compress the second, this layer solidifies. The structure...

  17. Neutron diffraction study of a nitrogen martensitic steel 0Kh16N4AB under load

    Czech Academy of Sciences Publication Activity Database

    Sumin, V. V.; Papushkin, I.V.; Bannykh, O.A.; Blinov, V.M.; Lukáš, Petr

    2008-01-01

    Roč. 105, č. 1 (2008), s. 88-91 ISSN 0031-918X Institutional research plan: CEZ:AV0Z10480505 Keywords : steel 0Kh16N4AB * neutron diffraction * FSD Subject RIV: BG - Nuclear, Atomic and Molecular Physics , Colliders Impact factor: 0.412, year: 2008

  18. Anomalous spin distribution in the superconducting ferromagnet UCoGe studied by polarized neutron diffraction

    NARCIS (Netherlands)

    Prokeš, K.; de Visser, A.; Huang, Y.K.; Fåk, B.; Ressouche, E.

    2010-01-01

    We report a polarized neutron-diffraction study conducted to reveal the nature of the weak ferromagnetic moment in the superconducting ferromagnet UCoGe. We find that the ordered moment in the normal phase in low magnetic fields (B∥c) is predominantly located at the U atom and has a magnitude of

  19. Residual stresses determination by neutron diffraction in a 100Cr6 chromium steel bearing ring

    Czech Academy of Sciences Publication Activity Database

    Rogante, M.; Martinat, G.; Mikula, Pavol; Vrána, Miroslav

    2013-01-01

    Roč. 51, č. 5 (2013), s. 275-281 ISSN 0023-432X R&D Projects: GA MŠk(XE) LM2011019 Institutional support: RVO:61389005 Keywords : 100Cr6 steel * rings * martensitic hardening * tempering * residual stress es * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.546, year: 2013

  20. The application of X-ray, γ-ray and neutron diffraction to the characterization of single crystal perfection

    International Nuclear Information System (INIS)

    Freund, A.; Schneider, J.R.

    1976-01-01

    The work is divided into the following three chapters: 1) diffraction by perfect and imperfect crystals, 2) experimental apparatus (describing gamma ray, X-ray and neutron diffractometers), 3) application of diffraction methods to the development of neutron monochromators. (WBU) [de

  1. Crystal structure solution of hydrides containing natEu from neutron powder diffraction data

    International Nuclear Information System (INIS)

    Kohlmann, H.

    1999-01-01

    Complete text of publication follows. The location of hydrogen in crystal structures of metal hydrides usually requires neutron diffraction data. Some elements, however, show excessively high absorption cross sections, σ a , for neutrons, thus making this technique seemingly impractical. Therefore no complete, refined crystal structure data of europium hydrides (σ a ( nat Eu) = .4530 barns at λ = 179.8 pm [1]) have been reported so far. It is shown that the absorption can be reduced to a value reasonable for neutron diffraction experiments by taking advantage of the wavelength dependence of σ a combined with the use of annular samples at advanced diffractometers. Neutron powder diffraction data on several nat Eu containing deuterides suitable for the ab initio crystal structure solution and refinement have been taken at D20 and D4 (ILL, Grenoble). The crystal chemistry of these europium hydrides, among them the two new compounds EuMg 2 H 6 and EuMgH 4 [2], is discussed. (author) [1] V.F. Sears, Neutron News 1992, 3, 26-37.; [2] H. Kohlmann, F. Gingl, T. Hansen, K. Yvon, Angew. Chem. Int. Ed. Eng. 1999, 38, accepted

  2. High-resolution neutron powder-diffraction in CMR manganates

    Energy Technology Data Exchange (ETDEWEB)

    Suard, E; Radaelli, P G [Institut Max von Laue - Paul Langevin (ILL), 38 - Grenoble (France)

    1997-04-01

    Manganese-oxide materials have recently been the subject of renewed attention, due to the `colossal` magnetoresistance (CMR) displayed near the spin-ordering temperature T{sub c} by some of these compounds. CMR has been evidenced in at least three families of manganese oxides. In most cases, the CMR compounds behave as paramagnetic semiconductors at high temperatures, and as ferromagnetic metals below T{sub c}. The study of this metallization process has lead some theorists to challenge its traditional interpretation in terms of the so-called double-exchange mechanism, and to propose alternative scenarios in which the coupling of the charge carriers with the lattice plays a paramount role. Powder diffraction method, being at the forefront of CMR research is presented. (author). 4 refs.

  3. Neutron diffraction measurements of microstress and macrostress in composites

    International Nuclear Information System (INIS)

    Tanaka, Keisuke; Akiniwa, Yoshiaki

    2001-01-01

    For accurate stress measurements, precise values of the diffraction elastic constant (DEC) is required. The theoretical prediction of DEC of engineering materials on the basis of the self-consistent model agreed well with the experimental results of sintered alumina with various porosities. From the experimental results of DEC of sintered silicon nitride, the elastic anisotropy of single crystals of β-silicon nitride was estimated with the simplex method. The phase stress measured in the matrix and SiC particles of composite subjected to the applied stress agreed well with the theoretical prediction. The macrostress calculated from the phase stress by using the rule of mixture was equal to the applied stress. The measured values of the thermal residual stress in ceramic composites of alumina mixed with various volume fractions of zirconia agreed well with the theoretical prediction based on Eshelby's inclusion model. (author)

  4. Measurement of residual stress in textured Al alloy by neutron diffraction method

    International Nuclear Information System (INIS)

    Okido, S.; Hayashi, M.; Tanaka, K.; Akiniwa, Y.; Minakawa, N.; Morii, Y.

    1999-01-01

    Residual stress generated in a shrunken aluminum alloy specimen, which was prepared for the round robin test conducted by VAMAS (Versailles Project on Advanced Materials and Standards) TWA-20 organized for the purpose of standardizing residual stress measurement methods, was evaluated by a neutron diffraction method. The main purpose of the round robin test was to assess the reproducibility of data obtained with the measurement facilities of the participants. The general standard of the Residual Stress Analyzer (RESA) constructed in the Japan Atomic Energy Research Institute was verified from the measured residual strains, which were equivalent to the values calculated by FEM and values measured by the research facilities in North America. Residual stress was calculated from residual strain in three perpendicular directions. The diffraction intensities were dependent on measurement directions since the prepared specimen possessed texture. Diffraction profiles in directions having a weak diffraction intensity caused an inaccurate evaluation of the residual stress. To solve this problem, a new method for evaluating residual stress with respect to diffraction plane dependency of the elastic constant was applied. The diffraction plane giving the highest intensity among 110, 200, and 220 diffraction was used to evaluate the residual strain in each of three directions. The residual strain obtained on the used diffraction plane was converted to the equivalent strain for the defined diffraction plane using the ratio of elastic constants of these two planes. The developed evaluation method achieved highly accurate measurement and remarkable efficiency in the measurement process. (author)

  5. New developments of TOF neutron diffraction at the IBR-2 pulsed reactor

    International Nuclear Information System (INIS)

    Balagurov, Anatoli M.

    2001-01-01

    Development of high-resolution RTOF Fourier technique for powder neutron diffraction studies is being continued at the IBR-2 pulsed reactor in Dubna. Besides some technical improvements in the operating HRFD instrument, a new dedicated instrument, Fourier Strain Diffractometer (FSD), for investigation of residual stresses in bulk materials has been constructed at IBR-2 in 1999. With a new HRFD Fourier chopper smaller than 10 μs TOF contribution in a resolution function was obtained in the experiment with perfect Si single crystal. A series of diffraction experiments with the beams from a new methane cold neutron moderator installed at the IBR-2 in 1999 is discussed. A comparison with the results obtained with the conventional water comb-like moderator shows that for various types of experiments, which are performed at HRFD and DN-2 diffractometers, the methane cold neutron source provides better conditions. (author)

  6. Rietveld refinement with time-of-flight powder diffraction data from pulsed neutron sources

    International Nuclear Information System (INIS)

    David, W.I.F.; Jorgensen, J.D.

    1990-10-01

    The recent development of accelerator-based pulsed neutron sources has led to the widespread use of the time-of-flight technique for neutron powder diffraction. The properties of the pulsed source make possible unusually high resolution over a wide range of d spacings, high count rates, and the ability to collect complete data at fixed scattering angles. The peak shape and other instrument characteristics can be accurately modelled, which make Rietveld refinement possible for complex structures. In this paper we briefly review the development of the Rietveld method for time-of-flight diffraction data from pulsed neutron sources and discuss the latest developments in high resolution instrumentation and advanced Rietveld analysis methods. 50 refs., 12 figs., 14 tabs

  7. Residual stress measurement of the jacket material for ITER coil by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Tsuchiya, Yoshinori [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment

    1998-03-01

    Nickel-Iron based super alloy INCOLOY 908 is used for the jacket of a central solenoid coil (CS coil) of the International Thermonuclear Experimental Reactor (ITER). INCOLOY 908, however, has a possibility of fracture due to Stress Accelerated Grain Boundary Oxidation (SAGBO) under a tensile residual stress beyond 200MPa. Therefore it is necessary to measure the residual stress of the jacket to avoid SAGBO. We performed residual stress measurement of the jacket by neutron diffraction using the neutron diffractometer for residual stress analysis (RESA) installed at JRR-3M in JAERI. A sample depth dependence of internal strain was obtained from the (111) plane spacing. A residual stress distribution was calculated from the strain using Young`s modulus and Poisson`s ratio that were evaluated by a tensile test with neutron diffraction. The result shows that the tensile residual stress exceeds 200MPa of the SAGBO condition in some regions inside the jacket. (author)

  8. Applications of image plates in neutron radiography and neutron diffraction at BARC, Trombay

    International Nuclear Information System (INIS)

    Shaikh, A.M.

    2013-01-01

    Neutron radiography techniques based on Gd, Dy and In metallic foils and X-ray film have been used at this centre since early seventies for various NDT and R and D work in nuclear, defence and aerospace industries. In recent years use of photostimulated luminescence based phosphor imaging plate has been introduced in our work. This has enabled to achieve higher sensitivities and dynamic ranges of recording radiographs with acceptable spatial resolution. It also provides digital image information which is more convenient for quantitative evaluations. Neutron image plates have been used in variety of radiography techniques such as conventional neutron radiography (NR), neutron induced beta radiography (NIBR), hydrogen sensitive epithermal neutron radiography (HYSEN) and for neutron powder diffractometry using Apsara, CIRUS and Dhruva reactors as neutron sources. Recently the image plates have also been used for characterization of thermalized neutron beam from a plasma focus neutron source and recording neutron radiographs. Prior to the utilization image plates have been characterised for their performance. Details of the measurements and applications will be presented. (author)

  9. In-situ oxidation study of Pd(100) by surface x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Kilic, Volkan; Franz, Dirk; Stierle, Andreas [AG Grenzflaechen, Universitaet Siegen (Germany); Martin, Natalia; Lundgren, Edvin [Department of Synchrotron Radiation Research, Lund University (Sweden); Mantilla, Miguel [MPI fuer Metallforschung, Stuttgart (Germany)

    2011-07-01

    The oxidation of the Pd(100) surface at oxygen pressures in the 10{sup -6} mbar to 10{sup 3} mbar range and temperatures up to 1000 K has been studied in-situ by surface x-ray diffraction (SXRD). The SXRD experiments were performed at the MPI beamline at the Angstrom Quelle Karlsruhe (ANKA). We present the surface and crystal truncation rod (CTR) data from the ({radical}(5) x {radical}(5)) surface layer. We show that the transformation from the surface oxide to PdO bulk oxide can be observed in-situ under specific pressure and temperature conditions. We compare our results with previously proposed structure models based on low energy electron diffraction (LEED) I(V) curves and density functional theory calculations. Finally, we elucidate the question of commensurability of the surface oxide layer with respect to the Pd(100) substrate.

  10. In situ electron backscattered diffraction of individual GaAs nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Prikhodko, S.V. [Department of Materials Science and Engineering, University of California Los Angeles, Los Angeles, CA 90095 (United States)], E-mail: sergey@seas.ucla.edu; Sitzman, S. [Oxford Instruments America, Concord, MA 01742 (United States); Gambin, V. [Northrop Grumman Space Technology, Redondo Beach, CA 90278 (United States); Kodambaka, S. [Department of Materials Science and Engineering, University of California Los Angeles, Los Angeles, CA 90095 (United States)

    2008-12-15

    We suggest and demonstrate that electron backscattered diffraction, a scanning electron microscope-based technique, can be used for non-destructive structural and morphological characterization of statistically significant number of nanowires in situ on their growth substrate. We obtain morphological, crystal phase, and crystal orientation information of individual GaAs nanowires in situ on the growth substrate GaAs(1 1 1) B. Our results, verified using transmission electron microscopy and selected area electron diffraction analyses of the same set of wires, indicate that most wires possess a wurtzite structure with a high density of thin structural defects aligned normal to the wire growth axis, while others grow defect-free with a zincblende structure. The demonstrated approach is general, applicable to other material systems, and is expected to provide important insights into the role of substrate structure on nanowire structure on nanowire crystallinity and growth orientation.

  11. Characterization of a polychromatic neutron beam diffracted by pyrolytic graphite crystals

    CERN Document Server

    Byun, S H; Choi, H D

    2002-01-01

    The beam spectrum for polychromatic neutrons diffracted by pyrolytic graphite crystals was characterized. The theoretical beam spectrum was obtained using the diffraction model for a mosaic crystal. The lattice vibration effects were included in the calculation using the reported vibration amplitude of the crystal and the measured time-of-flight spectra in the thermal region. The calculated beam spectrum was compared with the results obtained in the absence of thermal motion. The lattice vibration effects became more important for the higher diffraction orders and a large decrease in the neutron flux induced by the vibrations was identified in the epithermal region. The validity of the beam spectrum was estimated by comparing with the effective quantities determined from prompt gamma-ray measurements and Cd-ratios measured both for 1/nu and non-1/nu nuclides.

  12. Study of the ferrimagnetic and paramagnetic phases of magnetite measured by multiple neutron diffraction

    International Nuclear Information System (INIS)

    Mazzocchi, V.L.

    1992-01-01

    Structural parameters of the ferrimagnetic and paramagnetic phases of magnetite have been refined from neutron multiple diffraction data. Experimental multiple diffraction patterns used in the refinement, were obtained by measuring the 111 primary reflection of a natural single crystal of this compound, at room temperature for the ferrimagnetic phase and 703 0 C for the paramagnetic phase. Corresponding theoretical patterns for both phases have been calculated by the program MULTI which uses the iterative method for the intensity calculations in neutron multiple diffraction. In this method intensities are calculated as Taylor series expansions summed up to a order sufficient for a good approximation. A step by step process has been used in the refinements according to the parameter-shift method. Both isotropic and anisotropic thermal parameters were used in the calculation of the temperature factor. (author)

  13. Neutron diffraction measurements of residual stress in additively manufactured stainless steel

    International Nuclear Information System (INIS)

    Brown, D.W.; Bernardin, J.D.; Carpenter, J.S.; Clausen, B.; Spernjak, D.; Thompson, J.M.

    2016-01-01

    Charpy test specimens were additively manufactured (AM) on a single stainless steel plate from a 17–4 class stainless steel using a powder-bed, laser melting technique on an EOS M280 direct metal laser sintering (DMLS) machine. Cross-hatched mesh support structures for the Charpy test specimens were varied in strut width and density to parametrically study their influence on the build stability and accuracy as the DMLS process has been known to generate parts with large amounts of residual stress. Neutron diffraction was used to profile the residual stresses in several of the AM samples before and after the samples were removed from the support structure for the purpose of determining residual stresses. The residual stresses were found to depend very little on the properties of the support structure over the limited range studied here. The largest stress component was in the long direction of each of the samples studied and was roughly 2/3 of the yield stress of the material. The stress field was altered considerably when the specimen was removed from the support structure. It was noted in this study that a single Charpy specimen developed a significant tear between the growth plate and support structure. The presence of the tear in the support structure strongly affected the observed stress field: the asymmetric tear resulted in a significantly asymmetric stress field that propagated through removal of the sample from the base plate. The altered final residual stress state of the sample as well as its observed final shape indicates that the tear initiated during the build and developed without disrupting the fabrication process, suggesting a need for in-situ monitoring.

  14. Neutron diffraction measurements of residual stress in additively manufactured stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Brown, D.W.; Bernardin, J.D.; Carpenter, J.S.; Clausen, B.; Spernjak, D.; Thompson, J.M.

    2016-12-15

    Charpy test specimens were additively manufactured (AM) on a single stainless steel plate from a 17–4 class stainless steel using a powder-bed, laser melting technique on an EOS M280 direct metal laser sintering (DMLS) machine. Cross-hatched mesh support structures for the Charpy test specimens were varied in strut width and density to parametrically study their influence on the build stability and accuracy as the DMLS process has been known to generate parts with large amounts of residual stress. Neutron diffraction was used to profile the residual stresses in several of the AM samples before and after the samples were removed from the support structure for the purpose of determining residual stresses. The residual stresses were found to depend very little on the properties of the support structure over the limited range studied here. The largest stress component was in the long direction of each of the samples studied and was roughly 2/3 of the yield stress of the material. The stress field was altered considerably when the specimen was removed from the support structure. It was noted in this study that a single Charpy specimen developed a significant tear between the growth plate and support structure. The presence of the tear in the support structure strongly affected the observed stress field: the asymmetric tear resulted in a significantly asymmetric stress field that propagated through removal of the sample from the base plate. The altered final residual stress state of the sample as well as its observed final shape indicates that the tear initiated during the build and developed without disrupting the fabrication process, suggesting a need for in-situ monitoring.

  15. Capillary based Li-air batteries for in situ synchrotron X-ray powder diffraction studies

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune E.; Younesi, Reza

    2015-01-01

    For Li-air batteries to reach their full potential as energy storage system, a complete understanding of the conditions and reactions in the battery during operation is needed. To follow the reactions in situ a capillary-based Li-O2 battery has been developed for synchrotron-based in situ X......-ray powder diffraction (XRPD). In this article, we present the results for the analysis of 1st and 2nd deep discharge and charge for a cathode being cycled between 2 and 4.6 V. The crystalline precipitation of Li2O2 only is observed in the capillary battery. However, there are indications of side reactions...... of constant exposure of X-ray radiation to the electrolyte and cathode during charge of the battery was also investigated. X-ray exposure during charge leads to changes in the development of the intensity and the FWHM of the Li2O2 diffraction peaks. The X-ray diffraction results are supported by ex situ X...

  16. Neutron diffraction determination of mean-square atomic displacements

    International Nuclear Information System (INIS)

    Tibballs, J.E.; Feteris, S.M.; Barnea, Z.

    1981-01-01

    Integrated intensities for Bragg reflection of neutrons from single crystals of the III-V compounds, InAs and GaSb, have been measured at room temperature. The data were collected at two wavelengths, 0.947 A and 1.241 A, in order to establish the adequacy of a correction for moderate to severe anisotropic extinction. Data were also obtained for InAs at four temperatures from 408 K to 933 K. Corrections for thermal diffuse scattering were applied. The results were analysed in the one-particle potential approximation with terms to fourth-order in the atomic displacements u = (u 1 , u 2 , u 3 ). At 296 K, the mean-square components were determined for In, 0.0116(2)A 2 and As, 0.0102 (1)A 2 ; for Ga, 0.0120(3)A 2 and Sb, 0.0107(3)A 2 . The third-order coefficients for InAs are comparable with those for Si and Ge, those for GaSb with those for zinc chalcogenides. Non-harmonic behaviour in InAs is observed below 400 K

  17. Visualization of time-of-flight neutron diffraction data

    International Nuclear Information System (INIS)

    Mikkelson, D.J.; Price, D.L.; Worlton, T.G.

    1995-01-01

    The glass, liquids and amorphous materials diffractometer (GLAD) is a new instrument at the intense pulsed neutron source (IPNS) at Argonne National Laboratory. The GLAD currently has 218 linear position sensitive detectors arranged in five banks. Raw data collected from the instrument are typically split into 1000-1500 angular groups each of which contains approximately 2000 time channels. In order to obtain a meaningful overview of such a large amount of data, an interactive system to view the data has been designed. The system was implemented in C using the graphical kernel system (GKS) for portability.The system treats data from each bank of detectors as a three-dimensional data set with detector number, position along detector and time of flight as the three coordinate axes. The software then slices the data parallel to any of the coordinate planes and displays the slices as images. This approach has helped with the detailed analysis of detector electronics, verification of instrument calibration and resolution determination. In addition, it has helped to identify low-level background signals and provided insight into the overall operation of the instrument. ((orig.))

  18. In situ neutron scattering study of nanostructured PbTe-PbS bulk thermoelectric material

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Fei [Temple University; Schmidt, Robert D [ORNL; Case, Eldon D [Michigan State University, East Lansing; An, Ke [ORNL

    2016-01-01

    Nanostructures play an important role in thermoelectric materials. Their thermal stability, such as phase change and evolution at elevated temperatures, is thus of great interest to the thermoelectric community. In this study, in situ neutron diffraction was used to examine the phase evolution of nanostructured bulk PbTe-PbS materials fabricated using hot pressing and pulsed electrical current sintering (PECS). The PbS second phase was observed in all samples in the as-pressed condition. The temperature dependent lattice parameter and phase composition data show an initial formation of PbS precipitates followed by a redissolution during heating. The redissolution process started around 570 600 K, and completed at approximately 780 K. During cooling, the PECS sample followed a reversible curve while the heating/cooling behavior of the hot pressed sample was irreversible.

  19. Stress-induced martensitic transformations in NiTi and NiTi-TiC composites investigated by neutron diffraction

    International Nuclear Information System (INIS)

    Vaidyanathan, R.; Dunand, D.C.

    1999-01-01

    Superelastic NiTi (51.0 at.% Ni) specimens reinforced with 0, 10 and 20 vol.% TiC particles were deformed under uniaxial compression while neutron diffraction spectra were collected. The experiments yielded in-situ measurements of the thermoelastic stress-induced transformation. The evolution of austenite/martensite phase fractions and of elastic strains in the reinforcing TiC particles and the austenite matrix were obtained by Rietveld refinement during the loading cycle as the austenite transforms to martensite (and its subsequent back transformation during unloading). Phase fractions and strains are discussed in terms of load transfer in composites where the matrix undergoes a stress-induced phase transformation. (orig.)

  20. Neutron diffraction studies on ordered and disordered materials

    International Nuclear Information System (INIS)

    Krishna, P.S.R

    2016-01-01

    Knowledge of the symmetry and distribution of atoms in the unit cell and the bonding between atoms is the key point for understanding, designing and manipulating chemical behavior or physical properties of novel materials for technological applications. This could be achieved using diffraction techniques. At the Dhruva national facility, BARC, Mumbai, a Powder diffractometer (PD2) and a High-Q diffractometer (HQD) are in operation for more than 2 decades. PD2 and HQD are equipped with banks of 5 and 10 position sensitive detectors (PSD) respectively, to cover the Q-ranges 9.4 Å -1 and 15 Å -1 respectively. The resolutions (Δd/d) of these instruments are 0.8% (λ = 1.24 Å) and 2.5% (λ = 0.78 Å). We report about the studies of changes in the long range order in crystalline materials as a function of temperature and/or composition as well as short and intermediate range orders studied in amorphous materials on these diffractometers in recent years. PD2 has been extensively used in the structural/phase transition studies of ferroics, multiferroics, nanoferrites along with magnetic structure determinations. On the other hand, HQD has been extensively used to understand the short and intermediate range order in network glasses like chalcogenides, H-bonded alcohols, Telluride glasses etc. We will be discussing the recent structural results obtained on many of these crystalline systems, glasses and molecular fluids on both of these diffractometers. (author)

  1. In Situ High Resolution Synchrotron X-Ray Powder Diffraction Studies of Lithium Batteries

    DEFF Research Database (Denmark)

    Amri, Mahrez; Fitch, Andy; Norby, Poul

    2015-01-01

    allowing diffraction information to be obtained from only the active material during battery operation [2]. High resolution synchrotron x-ray powder diffraction technique has been undertaken to obtain detailed structural and compositional information during lithiation/delithiation of commercial LiFePO4...... materials [3]. We report results from the first in situ time resolved high resolution powder diffraction experiments at beamline ID22/31 at the European Synchrotron Radiation Facility, ESRF. We follow the structural changes during charge of commercial LiFePO4 based battery materials using the Rietveld...... method. Conscientious Rietveld analysis shows slight but continuous deviation of lattice parameters from those of the fully stoichiometric end members LiFePO4 and FePO4 indicating a subsequent variation of stoichiometry during cathode delithiation. The application of an intermittent current pulses during...

  2. Fundamentals and applications of neutron diffraction. Applications 7. Crystal structure analysis of fuel cell materials by means of neutron diffractometry

    International Nuclear Information System (INIS)

    Itoh, Takanori

    2010-01-01

    Perovskite oxides, which have 'A' atoms of an alkaline earth metal and/or a rare earth metal and 'B' atoms of a transition metal, have considerable potential for use in electrochemical devices such as cathodes of solid oxide fuel cells (SOFC), oxygen pumps, oxygen sensors, catalysts, and other devices such as oxygen separation membranes. The oxygen ion behavior is studied with relation performance of electrochemical devices. I have analyzed the crystal structure of SOFC materials by neutron diffraction. Using the Rietveld refinement technique, I showed that the O1(4c) and O2(8d) sites in a perovskite oxide of SOFC cathode material has different oxygen site occupancies. Furthermore, oxygen diffusion behavior is associated with temperature dependence of oxygen anisotropic atomic displacement parameters. The maximum entropy method (MEM) analysis of neutron diffraction measurements revealed nuclear scattering length distribution at high temperature by three-dimensional images in detail, therefore 1 found oxygen diffusion pass and new proton site in SOFC materials. From these results, neutron diffraction is confirmed to be very useful tool for the study of light element behavior in fuel cell materials. (author)

  3. Desorption of hydrogen from magnesium hydride: in-situ electron diffraction study

    International Nuclear Information System (INIS)

    Paik, B.; Jones, I.P.; Walton, A.; Mann, V.; Book, D.; Harris, I.R.

    2009-01-01

    The dynamics of a phase change has been studied where electron beam in Transmission Electron Microscope (TEM) has been used to transform MgH 2 into magnesium. A combination of in-situ Electron Diffraction (ED) and an in-situ Electron Energy Loss Spectroscopy (EELS) study under ED mode describes the phase transformation in terms of, respectively, change in the crystal structure and Plasmon energy shift. The orientation relation [001] MgH2 //[-2110] Mg and (-110) MgH2 //(0001) Mg , obtained from the ED study, has been used to propose a model for the movements of magnesium atoms in the structural change to describe the dynamics of the process. The in-situ EELS study has been compared with the existing H-desorption model. The study aims to describe the sorption dynamics of hydrogen in MgH 2 which is a base material for a number of promising hydrogen storage systems. (author)

  4. Non-destructive bulk analysis of the Buggenum sword by neutron resonance capture analysis and neutron diffraction

    International Nuclear Information System (INIS)

    Postma, H.; Clarijs, M.; Borella, A.; Schillebeeckx, P.; Kamermans, H.

    2010-01-01

    Two neutron based techniques, neutron resonance capture analysis (NRCA) and time-of-flight neutron-diffraction (TOF-ND) have been used to determine the elemental composition and structure of a precious and very well preserved all-metal sword from the Bronze Age. This Buggenum sword was on loan from the National Museum of Antiquities (NMA) in Leiden (NL). NRCA and TOF-ND experiments have been carried out at a number of more or less identical positions of the sword. The tin-bronze ratio and the relative amounts of some minor elements (Sb, As, Ag, In) have been determined. The results of neutron diffraction measurements showed considerable tin-segregation, and clear indications of hardening on the edges of the blade. In addition, radiographs using Bremsstrahlung revealed the construction of the hilt-blade connection. The work was carried out at the EC Joint Research Centre IRMM in Geel (B) and at the ISIS facility of the Rutherford Appleton Laboratory (UK). (author)

  5. Study of quartz-glass using Roentgen- and neutron-diffraction

    International Nuclear Information System (INIS)

    Sikkenk, P.J.

    1988-08-01

    An X-ray diffraction measurement, with wavelength 0.0711 nm, is made of a vitreous silica to kappa of 200nm -1 . (faculty of materials science) A second X-ray diffraction measurement has been executed (National Laboratory Oak Ridge). For this research we also used neutron diffraction measurement (IRI), with wavelength 0.085 nm of a vitreous silica to kappa of 132 nm -1 . The intermolecular scattering functions derived from the X-ray measurements and neutron measurements by omitting the intramolecular scattering contribution. A theoretical model for the structure of vitreous silica is used, derived from a mixture of Si en SiO-4 units. The partial scattering functions i-S-i---S-i is determined with help of the model and the intermolecular X-ray scattering functions and intermolecular neutron scattering functions and intermolecular neutron scatteirng functions. The fouriertransform of the partial scattering function i-S-i---S-i leads to the partial radial correlation function. When this partial radial correlation function is compared to a correlation function directly obtained by the intermolecular scattering function, a considerable increase of the resolution is observed in the partial correlation function if r > 0.29 nm and r < 0.45 nm. (author). 16 refs.; 30 figs.; 9 tabs

  6. Neutron diffraction analysis of the structure of rod photoreceptor membranes in intact retinas

    Energy Technology Data Exchange (ETDEWEB)

    Yaeger, M; Schoenborn, B; Engelman, D; Moore, P; Stryer, L

    1980-01-01

    Neutron diffraction data have been collected from samples containing ten dark-adapted Rana catesbiana bullfrog retinas in 100, 80, 60, 40, and 30% D/sub 2/O Ringer's solution using a step-scanning Soller slit diffractometer. Diffraction was also recorded from retinas equilibrated in D/sub 2/O solutions with varying osmolarity. Rocking curve experiments demonstrated that the rods are disoriented in a cylindrically symmetrical fashion. Structure factor amplitudes were obtained using semi-automated curve-fitting procedures, and phases were obtained by interpreting the D/sub 2/O-H/sub 2/O and osmotic Patterson maps. In D/sub 2/O Ringer's solution the first four structure factors are -353 +- 25, 246 +- 19, 434 +- 13 and 383 +- 19. Neutron scattering density profiles were calculated to 75 A resolution using these structure factors. These neutron diffraction data are consistent with the view that the lipid bilayer is a major structural motif of the rod outer segment disc membrane. Neutron Fourier syntheses in different mixtures of D/sub 2/O and H/sub 2/O indicate that the intradisc and extradisc spaces are predominantly aqueous, consistent with the increase in the intradisc and extradisc volumes as the Ringer's solution is made more hypotomic. In isotonic Ringer's solution, the thicknesses of the intradisc and extradisc spaces are about 36 A and 160 A, respectively, and the center-to-center separation between the 50 A thick lipid bilayer is 88 A.

  7. Crystallization of porcine pancreatic elastase and a preliminary neutron diffraction experiment

    Energy Technology Data Exchange (ETDEWEB)

    Kinoshita, Takayoshi [Department of Biological Science, Graduate School of Science, Osaka Prefecture University, 1-1 Gakuen-cho, Naka-ku, Sakai, Osaka 599-8531 (Japan); Tamada, Taro [Molecular Structural Biology Group, Quantum Beam Science Directorate, Japan Atomic Energy Agency, 2-4 Shirakata-Shirane, Tokai, Ibaraki 319-1195 (Japan); Imai, Keisuke [Lead Discovery Research Laboratories, Astellas Pharma Inc., 21 Miyukigaoka, Tsukuba-shi, Ibaraki 305-8585 (Japan); Kurihara, Kazuo; Ohhara, Takashi [Molecular Structural Biology Group, Quantum Beam Science Directorate, Japan Atomic Energy Agency, 2-4 Shirakata-Shirane, Tokai, Ibaraki 319-1195 (Japan); Tada, Toshiji [Department of Biological Science, Graduate School of Science, Osaka Prefecture University, 1-1 Gakuen-cho, Naka-ku, Sakai, Osaka 599-8531 (Japan); Kuroki, Ryota, E-mail: kuroki.ryota@jaea.go.jp [Molecular Structural Biology Group, Quantum Beam Science Directorate, Japan Atomic Energy Agency, 2-4 Shirakata-Shirane, Tokai, Ibaraki 319-1195 (Japan); Department of Biological Science, Graduate School of Science, Osaka Prefecture University, 1-1 Gakuen-cho, Naka-ku, Sakai, Osaka 599-8531 (Japan)

    2007-04-01

    To investigate the structural characteristics of a covalent inhibitor bound to porcine pancreatic elastase (PPE), including H atoms and hydration by water, a crystal of porcine pancreatic elastase with its inhibitor was grown to a size of 1.6 mm{sup 3} for neutron diffraction study. The crystal diffracted to 2.3 Å resolution with sufficient quality for further structure determination owing to the similar atomic scattering properties of deuterium and carbon. Porcine pancreatic elastase (PPE) resembles the attractive drug target leukocyte elastase, which has been implicated in a number of inflammatory disorders. In order to investigate the structural characteristics of a covalent inhibitor bound to PPE, including H atoms and the hydration by water, a single crystal of PPE for neutron diffraction study was grown in D{sub 2}O containing 0.2 M sodium sulfate (pD 5.0) using the sitting-drop vapour-diffusion method. The crystal was grown to a size of 1.6 mm{sup 3} by repeated macroseeding. Neutron diffraction data were collected at room temperature using a BIX-3 diffractometer at the JRR-3 research reactor of the Japan Atomic Energy Agency (JAEA). The data set was integrated and scaled to 2.3 Å resolution in space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 51.2, b = 57.8, c = 75.6 Å.

  8. The magnetic structure of GdNi2B2C investigated by neutron powder diffraction

    International Nuclear Information System (INIS)

    Barcza, A.; Rotter, M.; Doerr, M.; Beuneu, B.

    2005-01-01

    Full text: The group of ReT 2 B 2 C (Re=rare earth, T=transition metal) shows a very interesting interplay between magnetism and superconductivity due to the rare earth metals. In this work the magnetism of GdNi 2 B 2 C was studied with neutron diffraction. Previous investigations with x-ray diffraction methods have determined the crystal structure as a body centered tetragonal structure (I 4/mmm). Hot neutrons were used for the diffraction experiment, because the absorption cross section of Gd is significantly smaller for short wavelengths. The investigated compound orders magnetically at TN=19.5 K, and so the experiment was carried out at two temperatures, namely 30 K and 2.2 K. The results show a incommensurate spin structure with a propagation vector of (0.55 0 0). To confirm this results additional simulations of the spin structure were done based on the Standard Model of rare earth magnetism. A neutron diffraction pattern was calculated using the McPhase program package and is compared to the experimental data. (author)

  9. In situ neutron moisture meter calibration in lateritic soils

    International Nuclear Information System (INIS)

    Ruprecht, J.K.; Schofield, N.J.

    1990-01-01

    An in situ calibration procedure for complex lateritic soils of the jarrah forest of Western Australia is described. The calibration is based on non-destructive sampling of each access tube and on a regression of change in water content on change in neutron count ratio at 'wet' and 'dry' times of the year. Calibration equations with adequate precision were produced. However, there were high residual errors in the calibration equations which were due to a number of factors including soil water variability, the presence of a duricrust layer, soil sampling of gravelly soils and the variability of the cement slurry annulus surrounding each access tube. The calibration equations derived did not compare well with those from other studies in south-west Western Australia, but there was reasonable agreement with the general equations obtained by the Institute of Hydrology, U.K. 15 refs., 6 figs., 2 tabs

  10. Nanocrystallite characterization of milled simulated dry process fuel powders by neutron diffraction

    International Nuclear Information System (INIS)

    Ryu, Ho Jin; Kang, Kwon Ho; Moon, Je Sun; Song, Kee Chan; Choi, Yong Nam

    2003-01-01

    The nano-scale crystallite sizes of simulated spent fuel powders were measured by the neutron diffraction line broadening method in order to analyze the sintering behavior of the dry process fuel. The mixed U0 2 and fission product oxide powders were dry-milled in an attritor for 30, 60, and 120 min. The diffraction patterns of the powders were obtained by using the high resolution powder diffractometer in the HANARO research reactor. Diffraction line broadening due to crystallite size was measured using various techniques such as the Stokes' deconvolution, profile fitting methods using Cauchy function, Gaussian function, and Voigt function, and the Warren-Averbach method. The r.m.s. strain, stacking fault, twin and dislocation density were measured using the information from the diffraction pattern. The realistic crystallite size can be obtained after separation of the contribution from the non-uniform strain, stacking fault and twin

  11. Kinetics of methane-ethane gas replacement in clathrate-hydrates studied by time-resolved neutron diffraction and Raman spectroscopy.

    Science.gov (United States)

    Murshed, M Mangir; Schmidt, Burkhard C; Kuhs, Werner F

    2010-01-14

    The kinetics of CH(4)-C(2)H(6) replacement in gas hydrates has been studied by in situ neutron diffraction and Raman spectroscopy. Deuterated ethane structure type I (C(2)H(6) sI) hydrates were transformed in a closed volume into methane-ethane mixed structure type II (CH(4)-C(2)H(6) sII) hydrates at 5 MPa and various temperatures in the vicinity of 0 degrees C while followed by time-resolved neutron powder diffraction on D20 at ILL, Grenoble. The role of available surface area of the sI starting material on the formation kinetics of sII hydrates was studied. Ex situ Raman spectroscopic investigations were carried out to crosscheck the gas composition and the distribution of the gas species over the cages as a function of structure type and compared to the in situ neutron results. Raman micromapping on single hydrate grains showed compositional and structural gradients between the surface and core of the transformed hydrates. Moreover, the observed methane-ethane ratio is very far from the one expected for a formation from a constantly equilibrated gas phase. The results also prove that gas replacement in CH(4)-C(2)H(6) hydrates is a regrowth process involving the nucleation of new crystallites commencing at the surface of the parent C(2)H(6) sI hydrate with a progressively shrinking core of unreacted material. The time-resolved neutron diffraction results clearly indicate an increasing diffusion limitation of the exchange process. This diffusion limitation leads to a progressive slowing down of the exchange reaction and is likely to be responsible for the incomplete exchange of the gases.

  12. Cyclic olefin homopolymer-based microfluidics for protein crystallization and in situ X-ray diffraction

    International Nuclear Information System (INIS)

    Emamzadah, Soheila; Petty, Tom J.; De Almeida, Victor; Nishimura, Taisuke; Joly, Jacques; Ferrer, Jean-Luc; Halazonetis, Thanos D.

    2009-01-01

    A cyclic olefin homopolymer-based microfluidics system has been established for protein crystallization and in situ X-ray diffraction. Microfluidics is a promising technology for the rapid identification of protein crystallization conditions. However, most of the existing systems utilize silicone elastomers as the chip material which, despite its many benefits, is highly permeable to water vapour. This limits the time available for protein crystallization to less than a week. Here, the use of a cyclic olefin homopolymer-based microfluidics system for protein crystallization and in situ X-ray diffraction is described. Liquid handling in this system is performed in 2 mm thin transparent cards which contain 500 chambers, each with a volume of 320 nl. Microbatch, vapour-diffusion and free-interface diffusion protocols for protein crystallization were implemented and crystals were obtained of a number of proteins, including chicken lysozyme, bovine trypsin, a human p53 protein containing both the DNA-binding and oligomerization domains bound to DNA and a functionally important domain of Arabidopsis Morpheus’ molecule 1 (MOM1). The latter two polypeptides have not been crystallized previously. For X-ray diffraction analysis, either the cards were opened to allow mounting of the crystals on loops or the crystals were exposed to X-rays in situ. For lysozyme, an entire X-ray diffraction data set at 1.5 Å resolution was collected without removing the crystal from the card. Thus, cyclic olefin homopolymer-based microfluidics systems have the potential to further automate protein crystallization and structural genomics efforts

  13. Neutron diffraction tomography: a unique, 3D inspection technique for crystals using an intensifier TV system

    International Nuclear Information System (INIS)

    Davidson, J.B.; Case, A.L.

    1978-01-01

    The application of phosphor-intensifier-TV techniques to neutron topography and tomography of crystals is described. The older, analogous x-ray topography using wavelengths approximately 1.5A is widely used for surface inspection. However, the crystal must actually be cut in order to see diffraction anomalies beneath the surface. Because 1.5-A thermal neutrons are highly penetrating, much larger and thicker specimens can be used. Also, since neutrons have magnetic moments, they are diffracted by magnetic structures within crystals. In neutron volume topography, the entire crystal or a large part of it is irradiated, and the images obtained are superimposed reflections from the total volume. In neutron tomography (or section topography), a collimated beam irradiates a slice (0.5 to 10 mm) of the crystal. The diffracted image is a tomogram from this part only. A series of tomograms covering the crystal can be taken as the specimen is translated in steps across the narrow beam. Grains, voids, twinning, and other defects from regions down to 1 mm in size can be observed and isolated. Although at present poorer in resolution than the original neutron and film methods, the TV techniques are much faster and, in some cases, permit real-time viewing. Two camera systems are described: a counting camera having a 150 mm 6 Li-ZnS screen for low-intensity reflections which are integrated in a digital memory, and a 300-mm system using analog image storage. Topographs and tomograms of several crystals ranging in size from 4 mm to 80 mm are shown

  14. ''In situ'' electronic testing method of a neutron detector performance

    International Nuclear Information System (INIS)

    Gonzalez, J.M.; Levai, F.

    1987-01-01

    The method allows detection of any important change in the electrical characteristics of a neutron sensor channel. It checks the response signal produced by an electronic detector circuit when a pulse generator is connected as input signal in the high voltage supply. The electronic circuit compares the detector capacitance value, previously measured, against a reference value, which is adjusted in a window type comparator electronic circuit to detect any important degrading condition of the capacitance value in a detector-cable system. The ''in-situ'' electronic testing method of neutron detector performance has been verified in a laboratory atmosphere to be a potential method to detect any significant change in the capacitance value of a nuclear sensor and its connecting cable, also checking: detector disconnections, cable disconnections, length changes of the connecting cable, electric short-opened circuits in the sensor channel, and any electrical trouble in the detector-connector-cable system. The experimental practices were carried out by simulation of several electric changes in a nuclear sensor-cable system from a linear D.C. channel which measures reactor power during nuclear reactor operation. It was made at the Training Reactor Electronic Laboratory. The results and conclusions obtained at the Laboratory were proved, satisfactorily, in the Electronic Instrumentation of Budapest Technical University Training Reactor, Hungary

  15. The measurement of internal stress fields in weldments and around cracks using high resolution neutron diffraction

    International Nuclear Information System (INIS)

    Allen, A.J.; Hutchings, M.T.; Windsor, C.G.

    1987-01-01

    The paper describes and illustrates the capability of neutron diffraction to measure the complete internal lattice macrostrain field, and hence the stress field, within steel components and weldments arising from their fabrication. A brief outline is given of the theory of the neutron method. The experimental considerations are discussed. The method is illustrated by its application to the measurement of the stress distribution in a:- uniaxially stressed mild steel rod, a double - V test weld, a tube-plate weld, and a cracked fatigue test specimen. (U.K.)

  16. Use of neutron diffraction in determining strains in high-temperaure superconducting composites

    International Nuclear Information System (INIS)

    Hitterman, R.L.; Faber, J. Jr.; Kupperman, D.S.; Singh, J.P.; Majumdar, S.

    1990-01-01

    The Argonne Intense Pulsed Neutron Source and General Purpose Powder Diffractometer have been used to study high T c metal oxide composites composed of yttrium barium copper oxide and silver. Neutron diffraction techniques were applied to composites with 15, 20 and 30% silver content by volume. The authors have observed that after hot pressing, the 30% Ag specimens contained both orthorhombic high T c and tetragonal, non-superconducting phases near the center of the specimens but only tetragonal near the surface. The relationship of shifts in Bragg peaks to strains of the constituents is discussed

  17. Real Structure and Resudal Stresses in Advanced Welds Determined by X-ray and Neutron Diffraction

    Czech Academy of Sciences Publication Activity Database

    Trojan, K.; Hervoches, Charles; Ganev, N.; Mikula, Pavol; Čapek, J.

    2017-01-01

    Roč. 9, SEP (2017), s. 32-38 E-ISSN 2336-5382 R&D Projects: GA MŠk LM2015056; GA ČR GB14-36566G Institutional support: RVO:61389005 Keywords : laser and MAG welding * residual stresses * X-ray diffraction * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) https://ojs.cvut.cz/ojs/index.php/APP/article/view/4401/4298

  18. Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source

    Energy Technology Data Exchange (ETDEWEB)

    Mauro, N. A., E-mail: namauro@noctrl.edu [Department of Physics, North Central College, Naperville, Illinois 60540 (United States); Vogt, A. J. [Instrument and Source Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States); Derendorf, K. S. [Mechanical Engineering and Materials Science, Washington University, St. Louis, Missouri 63130 (United States); Johnson, M. L.; Kelton, K. F. [Department of Physics and Institute of Materials Science and Engineering, Washington University, 1 Brookings Drive, St. Louis, Missouri 63130 (United States); Rustan, G. E.; Quirinale, D. G.; Goldman, A. I. [Department of Physics and Astronomy, Iowa State University, Ames, Iowa 50011 (United States); Kreyssig, A. [Department of Physics and Astronomy, Iowa State University, Ames, Iowa 50011 (United States); Division of Materials Sciences and Engineering, Ames Laboratory, Ames, Iowa 50011 (United States); Lokshin, K. A. [Department of Materials Science and Engineering, University of Tennessee, Knoxville, Tennessee 37996 (United States); Quantum Condensed Matter Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States); Neuefeind, J. C.; An, Ke [Chemical and Engineering Materials Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States); Wang, Xun-Li [Department of Physics and Materials Science, City University of Hong Kong, 83 Tat Chee Ave., Kowloon (Hong Kong); Egami, T. [Department of Materials Science and Engineering, University of Tennessee, Knoxville, Tennessee 37996 (United States); Department of Physics and Astronomy, Joint Institute for Neutron Sciences, University of Tennessee, Knoxville, Tennessee 37996 (United States)

    2016-01-15

    Neutron diffraction studies of metallic liquids provide valuable information about inherent topological and chemical ordering on multiple length scales as well as insight into dynamical processes at the level of a few atoms. However, there exist very few facilities in the world that allow such studies to be made of reactive metallic liquids in a containerless environment, and these are designed for use at reactor-based neutron sources. We present an electrostatic levitation facility, NESL (for Neutron ElectroStatic Levitator), which takes advantage of the enhanced capabilities and increased neutron flux available at spallation neutron sources (SNSs). NESL enables high quality elastic and inelastic neutron scattering experiments to be made of reactive metallic and other liquids in the equilibrium and supercooled temperature regime. The apparatus is comprised of a high vacuum chamber, external and internal neutron collimation optics, and a sample exchange mechanism that allows up to 30 samples to be processed between chamber openings. Two heating lasers allow excellent sample temperature homogeneity, even for samples approaching 500 mg, and an automated temperature control system allows isothermal measurements to be conducted for times approaching 2 h in the liquid state, with variations in the average sample temperature of less than 0.5%. To demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr{sub 64}Ni{sub 36} measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample (∼100 mg)

  19. Methodology for studying strain inhomogeneities in polycrystalline thin films during in situ thermal loading using coherent x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Vaxelaire, N; Labat, S; Thomas, O [Aix-Marseille University, IM2NP, FST avenue Escadrille Normandie Niemen, F-13397 Marseille Cedex (France); Proudhon, H; Forest, S [MINES ParisTech, Centre des materiaux, CNRS UMR 7633, BP 87, 91003 Evry Cedex (France); Kirchlechner, C; Keckes, J [Erich Schmid Institute for Material Science, Austrian Academy of Science and Institute of Metal Physics, University of Leoben, Jahnstrasse 12, 8700 Leoben (Austria); Jacques, V; Ravy, S [Synchrotron SOLEIL, L' Orme des merisiers, Saint-Aubin BP 48, 91192 Gif-sur-Yvette Cedex (France)], E-mail: nicolas.vaxelaire@univ-cezanne.fr

    2010-03-15

    Coherent x-ray diffraction is used to investigate the mechanical properties of a single grain within a polycrystalline thin film in situ during a thermal cycle. Both the experimental approach and finite element simulation are described. Coherent diffraction from a single grain has been monitored in situ at different temperatures. This experiment offers unique perspectives for the study of the mechanical properties of nano-objects.

  20. Methodology for studying strain inhomogeneities in polycrystalline thin films during in situ thermal loading using coherent x-ray diffraction

    International Nuclear Information System (INIS)

    Vaxelaire, N; Labat, S; Thomas, O; Proudhon, H; Forest, S; Kirchlechner, C; Keckes, J; Jacques, V; Ravy, S

    2010-01-01

    Coherent x-ray diffraction is used to investigate the mechanical properties of a single grain within a polycrystalline thin film in situ during a thermal cycle. Both the experimental approach and finite element simulation are described. Coherent diffraction from a single grain has been monitored in situ at different temperatures. This experiment offers unique perspectives for the study of the mechanical properties of nano-objects.

  1. Neutron powder diffraction and theory-aided structure refinement of rubidium and cesium ureate

    Energy Technology Data Exchange (ETDEWEB)

    Sterri, Kjersti B.; Deringer, Volker L.; Houben, Andreas; Jacobs, Philipp [RWTH Aachen Univ. (Germany). Inst. of Inorganic Chemistry; Kumar, Chogondahalli M.N. [Forschungszentrum Juelich GmbH, Juelich Centre for Neutron Science (JCNS), Outstation at SNS, Oak Ridge National Laboratory, Oak Ridge, TN (United States); Oak Ridge National Laboratory, TN (United States). Chemical and Engineering Materials Div.; Dronskowski, Richard [RWTH Aachen Univ. (Germany). Inst. of Inorganic Chemistry; RWTH Aachen Univ. (Germany). Juelich-Aachen Research Alliance (JARA-HPC)

    2016-08-01

    Urea (CN{sub 2}H{sub 4}O) is a fundamental biomolecule whose derivatives are abundant throughout chemistry. Among the latter, rubidium ureate (RbCN{sub 2}H{sub 3}O) and its cesium analog (CsCN{sub 2}H{sub 3}O) have been described only very recently and form the first structurally characterized salts of deprotonated urea. Here, we report on a neutron diffraction study on the aforementioned alkaline-metal ureates, which affords the positions for all hydrogen atoms (including full anisotropic displacement tensors) and thus allows us to gain fundamental insights into the hydrogen-bonding networks in the title compounds. The structure refinements of the experimental neutron data proceeded successfully using starting parameters from ab initio simulations of atomic positions and anisotropic displacement parameters. Such joint experimental-theoretical refinement procedures promise significant practical potential in cases where complex solids (organic, organometallic, framework materials) are studied by powder diffraction.

  2. Kinetic neutron diffraction and SANS studies of phase formation in bioactive machinable glass ceramics

    International Nuclear Information System (INIS)

    Bentley, P M; Kilcoyne, S H; Bubb, N L; Ritter, C; Dewhurst, C D; Wood, D J

    2007-01-01

    Bioactive fluormica-fluorapatite glass-ceramic materials offer a very encouraging solution to the problem of efficient restoration and reconstruction of hard tissues. To produce material with the desired crystalline phases, a five-stage heat treatment must be performed. This thermal processing has a large impact on the microstructure and ultimately the final mechanical properties of the materials. We have examined the thermal processing of one of our most promising machinable biomaterials, using time-resolved small angle neutron scattering and neutron diffraction to study the nucleation and growth of crystallites. The processing route had already been optimized by studying the properties of quenched samples using x-ray diffraction, mechanical measurements and differential thermal analysis. However these results show that the heat treatment can be further optimized in terms of crystal nucleation, and we show that these techniques are the only methods by which a truly optimized thermal processing route may be obtained

  3. A time-of-flight spectrometer for neutron diffraction under high pressure or at high temperature

    International Nuclear Information System (INIS)

    Roult, G.; Buevoz, J.L.

    1975-01-01

    For high pressure neutron diffraction studies (40 kilobars) the sample is placed in a very thick cell. In order to allow the neutron beam to go through the cell loosing as little intensity as possible, the inner part is kept solid while the external part has some windows facing the incident and reflected beam. The window dimensions are small (a few millimeters wide and a few centimeters long). There are two alternatives: to have the window either in a perpendicular plane or in a plane parallel to the axis. In the first case a fixed wavelength spectrometer can be used but the sample is small and the contribution of the cell to the diffraction pattern is relatively great. In the second case samples can be something like ten times greater and the cell contribution can be eliminated but a fixed wavelength spectrometer cannot be used. Thus the time-of-flight method is very convenient. The second alternative was chosen

  4. Neutron-diffraction measurement of residual stresses in Al-Cu cold-cut welding

    CERN Document Server

    Fiori, F

    2002-01-01

    Usually, when it is necessary to join different materials with a large difference in their melting points, welding should be avoided. To overcome this problem we designed and built a device to obtain cold-cut welding, which is able to strongly decrease oxidation problems of the surfaces to be welded. Thanks to this device it is possible to achieve good joining between different pairs of materials (Al-Ti, Cu-Al, Cu-Al alloys) without reaching the material melting point. The mechanical and microstructural characterisation of the joining and the validation of its quality were obtained using several experimental methods. In particular, in this work neutron-diffraction experiments for the evaluation of residual stresses in Cu-Al junctions are described, carried out at the G5.2 diffractometer of LLB, Saclay. Neutron-diffraction results are presented and related to other experimental tests such as microstructural characterisation (through optical and scanning electron microscopy) and mechanical characterisation (ten...

  5. Neutron diffraction study of carbontetrachloride, siliciumtetrachloride, titaniumtetrachloride, and tintetrachloride in the liquid state at 295 K

    International Nuclear Information System (INIS)

    Tricht, J.B. van

    1977-01-01

    Neutron diffraction data on the molecular liquids CCl 4 , SiCl 4 , TiCl 4 , and sSnCl 4 have been collected in an interval of the scattering parameter, kappa = 4πsintheta/lambda, extending from 0.4 A -1 to 13.3 A -1 . The neutron wavelength was 0.878 A. The statistical accuracy of the data was better than 0.25 percent, and for titanium and tin tetrachloride a factor of two better. The intermolecular contributions to the diffracted intensity is dealt with in two ways: first a comparison in kappa- and in r-space between the experimental scattering and the corresponding distribution calculated from a model of randomly oriented molecules consisting of hard spheres. Furthermore, the regions in kappa- and in r-space can be identified where positional and where orientational correlations are predominent

  6. Dehydration reactions of gypsum: A neutron and X-ray diffraction study

    Science.gov (United States)

    Abriel, W.; Reisdorf, K.; Pannetier, J.

    1990-03-01

    The kinetics of the dehydration of gypsum was investigated by powder diffraction methods. Using the incoherent scattering effect of H with the neutron beam, the background intensity as a measure of the water content was checked in the temperature range 295-623 K. The superposed Bragg peaks yielded four major phases: Gypsum, subhydratesCaSO 4(H 2O) x (1 > x > 0),AIII-CaSO 4, AII-CaSO 4. For the subhydrates a maximum water content of x > = 0.74was determined. A different kinetic was found using Guinier X-ray technique with the heated sample prepared on a thin foil. Only with high local H 2O steam pressure, produced in the comparable larger sample container of the neutron diffraction experiment, could this high H 2O occupation of the subhydrate tunnel structure be found. A topotactic mechanism can describe the phase transitions for this reaction.

  7. X – ray and neutron diffraction of TiAl alloys

    International Nuclear Information System (INIS)

    Valkov, Stefan; Petrov, Peter; Neov, Dimitar; Beskrovny, Anatoly; Kozlenko, Denis

    2015-01-01

    TiAl alloys were prepared by electron beam hybrid method. Composite Ti-Al film, from composite target, was deposited on Ti substrate by electron beam evaporation, followed by electron beam treatment with scanning electron beam. Experiments were made using Leybold Heraus (EWS 300/ 15 - 60) with the following technological parameters : accelerating voltage U = 60kV; beam current I=40 mA, speed of movement of specimens V=5 cm/s, current of the focusing lens If =512mA, specimen distance D0 = 38cm. X- ray and neutron diffraction methods were used to determine the phase composition on the surface and at the volume, respectively. Time of flight neutron diffraction study of TiAl specimens was performed on DN-2 diffractometer at fast pulsed IBR-2 reactor in FLNP JINR (Dubna, Russia).We found that intermetallic TiAl phases were successfully obtained on the surface, as well as in the volume.

  8. Neutron diffraction study of the β1-β2 transformation in Ta2D

    International Nuclear Information System (INIS)

    Kaneko, H.; Kajitani, T.; Hirabayashi, M.

    1984-01-01

    The β 1 -β 2 phase transformation in Ta 2 D was studied by neutron diffraction using the pulsed source at the Tohoku Linac and the Intense Pulsed Neutron Source, Argonne National Laboratory. It was found that the hhO reflections almost disappear in the β 2 phase, whereas the 00l reflections are the same as those in the β 1 phase. The diffraction data show that the β 2 phase has an orthorhombic unit cell which is identical with that of the β 1 phase and contains four tantalum and two deuterium atoms in a volume which is approximately 2sup(1/2) X 1 X 2sup(1/2) that of the b.c.c. host lattice. The deuterium atoms fractionally occupy the tetrahedral sites in alternate (002)sub(orth) planes. (Auth.)

  9. Determination of the hexagonal network parameters of the quartz β using neutron multiple diffraction

    International Nuclear Information System (INIS)

    Campos, L.C.; Parente, C.B.R.; Mazzocchi, V.L.; Helene, O.

    2000-01-01

    In this work, neutron multiple diffraction is employed for the determination of the parameters a and c of the β-quartz hexagonal cell. This crystalline phase of silica (SiO 2 ) occurs in temperatures between ca. 846 and 1143 K. A β-quartz neutron multiple diffraction pattern has been used in the determinations. This pattern was obtained with a natural quartz single crystal heated to 1003 K. During the indexing of the pattern it was verified that most of the pairs of secondary reflections, which are responsible for the formation of peaks, could be classified as 'good for the determination of a' or 'good for the determination of c'. With this classification, it became possible to employ an iterative method for the determination of both parameters. After 8 cycles of iteration the values found for the parameters were a = 4.9964 +- 0.0018 and c = 5.46268 +- 0.00052 A. (author)

  10. 40-Tesla pulsed-field cryomagnet for single crystal neutron diffraction

    Science.gov (United States)

    Duc, F.; Tonon, X.; Billette, J.; Rollet, B.; Knafo, W.; Bourdarot, F.; Béard, J.; Mantegazza, F.; Longuet, B.; Lorenzo, J. E.; Lelièvre-Berna, E.; Frings, P.; Regnault, L.-P.

    2018-05-01

    We present the first long-duration and high duty cycle 40-T pulsed-field cryomagnet addressed to single crystal neutron diffraction experiments at temperatures down to 2 K. The magnet produces a horizontal field in a bi-conical geometry, ±15° and ±30° upstream and downstream of the sample, respectively. Using a 1.15 MJ mobile generator, magnetic field pulses of 100 ms length are generated in the magnet, with a rise time of 23 ms and a repetition rate of 6-7 pulses per hour at 40 T. The setup was validated for neutron diffraction on the CEA-CRG three-axis spectrometer IN22 at the Institut Laue Langevin.

  11. Secondary extinction in cylindrical and spherical crystals for X-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Hu Huachen; Li Zhaohuan; Yang Bin; Shen Caiwan

    2001-01-01

    The distribution of the reflection power ratio for a neutron or x-ray diffracted from a cylindrical crystal immersed in an homogenous incident beam is obtained by the numerical solution of the transfer equations for the first time. The profile well reflects all the physical properties of the absorption and extinction behaviour in the crystals. A systematic investigation of the secondary extinction for cylindrical and spherical crystals was carried out based on these results

  12. Stresses in plasma-sprayed Cr2O3 coatings measured by neutron diffraction

    Czech Academy of Sciences Publication Activity Database

    Dubský, Jiří; Prask, H. J.; Matějíček, Jiří; Gnäupel-Herold, T.

    2002-01-01

    Roč. 75, - (2002), s. 1-3 ISSN 0947-8396. [International Conference on Neutron Scattreing. Munich, 09.08.2001-13.08.2002] R&D Projects: GA ČR GA106/01/0094 Institutional research plan: CEZ:AV0Z2043910 Keywords : plasma sprayed, diffraction Subject RIV: JK - Corrosion ; Surface Treatment of Materials Impact factor: 2.231, year: 2002

  13. Neutron diffraction studies on cobalt substituted BiFeO3

    Science.gov (United States)

    Ray, J.; Biswal, A. K.; Acharya, S.; Babu, P. D.; Siruguri, V.; Vishwakarma, P. N.

    2013-02-01

    A dilute concentration of single phase Cobalt substituted Bismuth ferrite, BiFe1-XCoXO3; (x=0, 0.02) is prepared by sol-gel auto combustion method. Room temperature neutron diffraction patterns show no change in the crystal and magnetic structure upon cobalt doping. The calculation of magnetic moments shows 3.848 μB for Fe+ and 2.85 μB for Co3+. The cobalt is found to be in intermediate spin state.

  14. The neutron diffraction of molten TlCl, TlBr, and TlI

    International Nuclear Information System (INIS)

    Satow, T.; Uemura, O.; Hoshino, K.; Watanabe, T.

    1984-01-01

    Structure factors S(K) for liquid TlCl, TlBr, and TlI are determined by neutron diffraction measurements. Atomic radial distribution functions (RDF) derived from S(K) are presented. All RDF values are slightly smaller than those of their solid state counter parts. Results show that TlX has a tendency not to retain cesium-chloride type local order, but to take sodium-chloride type order when melting

  15. Neutron diffraction on CeMnAlD{sub x} (0{<=}x{<=}2.5)

    Energy Technology Data Exchange (ETDEWEB)

    Spatz, P.; Gross, K.; Schlapbach, L. [Fribourg Univ. (Switzerland); Fischer, P.; Fauth, F. [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-09-01

    CeMnAl was found to absorb considerable amounts of hydrogen. Part of the totally stored hydrogen is absorbed at low pressures (< 10 mbar). Additional hydrogen can be absorbed and desorbed reversible in a wide pressure range (10 mbar to 10 bar) at room temperature. In order to a better understanding of this new metal-hydride system, we performed neutron diffraction on deuterated CeMnAl samples with different D-concentrations. (author) 1 fig., 2 refs.

  16. Residual Stress Analysis for Engineering Applications by Means of Neutron Diffraction

    International Nuclear Information System (INIS)

    Gndupel-Herold, Thomas; Brand, Paul C.; Prask, Henry J.

    1999-01-01

    The economic and scientific importance of neutron diffraction residual stress analysis has led to an increasing number of suitable instruments worldwide. Recently, a dedicated state-of-the-art diffractometer has been installed at the National Institute of Standards and Technology reactor. It has been used for a variety of measurements on basic and engineering stress problems. Among the most prominent examples that have been investigated are residual stresses in rails, weldments, and plasma-sprayed coatings

  17. Neutron powder diffraction studies of Hydrogen and Denterium in Palladium Phosphides

    International Nuclear Information System (INIS)

    Andersson, Y.

    1986-01-01

    The use of the Rietveld-type profile refinements on neutron powder diffraction intensity data for determining crystallographic positions of hydrogen and deuterium in metal hydrides is illustrated by results obtained on some hydrogenated and deuterated palladium phosphides. The structural features of the solid solutions of hydrogen and deuterium in Pd/sb15/P/sb2/ Pd/sb6/P and Pd/sb3/P/sb1-u/ (0< u<0.28) are briefly presented and discussed

  18. Complex investigation of deformation twinning in gamma-TiAl by TEM and neutron diffraction

    Czech Academy of Sciences Publication Activity Database

    Beran, Přemysl; Heczko, Milan; Kruml, Tomáš; Panzner, T.; van Petegem, S.

    2016-01-01

    Roč. 95, OCT (2016), s. 647-662 ISSN 0022-5096 R&D Projects: GA ČR(CZ) GAP107/11/0704; GA MŠk(CZ) ED1.1.00/02.0068 Institutional support: RVO:68081723 ; RVO:61389005 Keywords : dislocations * twinning * polycrystalline material * neutron diffraction * electron microscopy Subject RIV: BM - Solid Matter Physics ; Magnetism; JL - Materials Fatigue, Friction Mechanics (UFM-A) Impact factor: 4.255, year: 2016

  19. Development of a sample environment for neutron diffraction at low temperature

    International Nuclear Information System (INIS)

    Lee, Jeong Soo; Lee, Chang Hee; Choi, Yong Nam

    2000-06-01

    This report contains the development of low temperature sample environment for the neutron diffraction and its utilization techniques. With this research, a low temperature experimental facility of T=10-300 K was developed. We measured magnetic peak of La 1 .4Sr 1 .6Mn 2 O 7 due to low temperature phase transition successfully by this unit installed at the sample table of HRPD. Therefore, the research capability for various materials under the low temperature was expanded

  20. Crystal structure of barium hydride, determined by neutron diffraction experiments on BaD2

    International Nuclear Information System (INIS)

    Bronger, W.; Scha Chi-Chien; Mueller, P.

    1987-01-01

    A reinvestigation of the structure of BaH 2 and BaD 2 was performed on powdered samples by X-ray- and neutron diffraction experiments. It is shown, that the hydrogen positions correspond with those found in calcium deuteride and not with those proposed in the literature. The classification of barium hydride in the PbCl 2 structure type is discussed. (author)

  1. Deformation behavior of Mg-alloy-based composites at different temperatures studied by neutron diffraction

    Czech Academy of Sciences Publication Activity Database

    Farkas, Gergely; Máthis, K.; Pilch, Jan; Minárik, P.; Lukáš, Petr; Vinogradov, A.

    2017-01-01

    Roč. 685, FEB (2017), s. 284-293 ISSN 0921-5093 R&D Projects: GA ČR GB14-36566G; GA MŠk LM2015056 Institutional support: RVO:61389005 Keywords : magnesium alloy matrix composite s * neutron diffraction * deformation * twinning Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 3.094, year: 2016

  2. A high-resolution neutron powder diffraction study of neodymium doping in barium cerate

    DEFF Research Database (Denmark)

    Knight, K.S.; Bonanos, N.

    1995-01-01

    High-resolution neutron powder diffraction data have been collected on 6 perovskites of composition BaCe1-xNdxO3-x/(2), with 0 less than or equal to x less than or equal to 0.2, in which structural phase transitions Pmcn-->P4/mbm at x=0.05, and P4/mbm-->Pm3m at x=0.1, were inferred from a recent ...

  3. Structural characterisation of 1- and 2-dimensional transition metal polymers using powder neutron diffraction

    International Nuclear Information System (INIS)

    James, M.

    1999-01-01

    Powder neutron diffraction provides an alternate technique for the structural study of transition metal polymers and finds utility over standard X-ray methods in two significant ways. Firstly, due to a different instrument geometry, preferred orientation effects are removed from the system. The second advantage gained by utilising neutrons is that H atoms in the sample contribute much more to the nuclear scattering of the diffraction profile - allowing their atomic position to be accurately determined. In X-ray diffraction studies, where H atoms typically account for only ∼3-5% of the scattering from the sample, it is essentially impossible to refine their position in the molecular structure. The structures of several transition metal polymers have been determined using neutrons from the HIFAR reactor at ANSTO and the Powder Diffractometers HRPD and MRPD, along with Rietveld refinement methods. The 1-dimensional polymer dibromobis(thiazole)nickel(II) illustrated in the paper is characteristic of these types of systems which are comprised of transition metal centres bridged by halogen atoms with pendant amine side groups

  4. In-situ Indentation and Correlated Precession Electron Diffraction Analysis of a Polycrystalline Cu Thin Film

    Science.gov (United States)

    Guo, Qianying; Thompson, Gregory B.

    2018-04-01

    In-situ TEM nanoindentation of a polycrystalline Cu film was cross-correlated with precession electron diffraction (PED) to quantify the microstructural evolution. The use of PED is shown to clearly reveal features, such as grain size, that are easily masked by diffraction contrast created by the deformation. Using PED, the accompanying grain refinement and change in texture as well as the preservation of specific grain boundary structures, including a ∑3 boundary, under the indent impression were quantified. The nucleation of dislocations, evident in low-angle grain boundary formations, was also observed under the indent. PED quantification of texture gradients created by the indentation process linked well to bend contours observed in the bright-field images. Finally, PED enabled generating a local orientation spread map that gave an approximate estimation of the spatial distribution of strain created by the indentation impression.

  5. In situ laser heating and radial synchrotron X-ray diffraction ina diamond anvil cell

    Energy Technology Data Exchange (ETDEWEB)

    Kunz, Martin; Caldwell, Wendel A.; Miyagi, Lowell; Wenk,Hans-Rudolf

    2007-06-29

    We report a first combination of diamond anvil cell radialx-ray diffraction with in situ laser heating. The laser-heating setup ofALS beamline 12.2.2 was modified to allow one-sided heating of a samplein a diamond anvil cell with an 80 W yttrium lithium fluoride laser whileprobing the sample with radial x-ray diffraction. The diamond anvil cellis placed with its compressional axis vertical, and perpendicular to thebeam. The laser beam is focused onto the sample from the top while thesample is probed with hard x-rays through an x-ray transparentboron-epoxy gasket. The temperature response of preferred orientation of(Fe,Mg)O is probed as a test experiment. Recrystallization was observedabove 1500 K, accompanied by a decrease in stress.

  6. Investigation of TbMn2O5 by polarized neutron diffraction.

    Science.gov (United States)

    Zobkalo, I A; Gavrilov, S V; Sazonov, A; Hutanu, V

    2018-05-23

    In order to make a new approach to the elucidation of the microscopic mechanisms of multiferroicity in the RMn 2 O 5 family, experiments with different methods of polarized neutrons scattering were performed on a TbMn 2 O 5 single crystal. We employed three different techniques of polarized neutron diffraction without the analysis after scattering, the XYZ-polarization analysis, and technique of spherical neutron polarimetry (SNP). Measurements with SNP were undertaken both with and without external electric field. A characteristic difference in the population of 'right' and 'left' helix domains in all magnetically ordered phases of TbMn 2 O 5 , was observed. This difference can be controlled by an external electric field in the field-cooled mode. The analysis of the results gives an evidence that antisymmetric Dzyaloshinsky-Moria exchange is effective in all the magnetic phases in TbMn 2 O 5 .

  7. Polarized neutron diffraction - a tool for testing extinction models: application to yttrium iron garnet

    International Nuclear Information System (INIS)

    Bonnet, M.; Delapalme, A.; Becker, P.

    1976-01-01

    This paper shows that polarized neutron experiments, which do not depend on any scale factor, are very dependent on extinction and provide original tests for extinction models. Moon, Koehler, Cable and Child (1972) have formulated the problem and proposed a first-order solution applicable only when the extinction is small. In the first part, some analytical derivations of secondary extinction corrections are discussed, using the formalism of Becker and Coppens (1974). In the second part, the main principles governing polarized neutron diffraction are briefly reviewed, with a special discussion of extinction problems. The method is then applied to the case of yttrium iron garnet (YIG). This experiment shows the technique of polarized neutrons to be very powerful for testing extinction models and for deciding whether the crystal behaves dynamically or kinematically (following Kato's criterion). (Auth.)

  8. Investigation of TbMn2O5 by polarized neutron diffraction

    Science.gov (United States)

    Zobkalo, I. A.; Gavrilov, S. V.; Sazonov, A.; Hutanu, V.

    2018-05-01

    In order to make a new approach to the elucidation of the microscopic mechanisms of multiferroicity in the RMn2O5 family, experiments with different methods of polarized neutrons scattering were performed on a TbMn2O5 single crystal. We employed three different techniques of polarized neutron diffraction without the analysis after scattering, the XYZ-polarization analysis, and technique of spherical neutron polarimetry (SNP). Measurements with SNP were undertaken both with and without external electric field. A characteristic difference in the population of ‘right’ and ‘left’ helix domains in all magnetically ordered phases of TbMn2O5, was observed. This difference can be controlled by an external electric field in the field-cooled mode. The analysis of the results gives an evidence that antisymmetric Dzyaloshinsky-Moria exchange is effective in all the magnetic phases in TbMn2O5.

  9. High pressure sample container for thermal neutron spectroscopy and diffraction on strongly scattering fluids

    International Nuclear Information System (INIS)

    Verkerk, P.; Pruisken, A.M.M.

    1979-01-01

    A description is presented of the construction and performance of a container for thermal neutron scattering on a fluid sample with about 1.5 cm -1 macroscopic cross section (neglecting absorption). The maximum pressure is about 900 bar. The container is made of 5052 aluminium capillary with inner diameter 0.75 mm and wall thickness 0.25 mm; it covers a neutron beam with a cross section of 9 X 2.5 cm 2 . The container has been successfully used in neutron diffraction and time-of-flight experiments on argon-36 at 120 K and several pressures up to 850 bar. It is shown that during these measurements the temperature gradient over the sample as well as the error in the absolute temperature were both less than 0.05 K. Subtraction of the Bragg peaks due to container scattering in diffraction experiments may be dfficult, but seems feasible because of the small amount of aluminium in the neutron beam. Correction for container scattering and multiple scattering in time-of-flight experiments may be difficult only in the case of coherently scattering samples and small scattering angles. (Auth.)

  10. Structural Investigation of Sodium Layered Oxides Via in Situ Synchrotron X-Ray Diffraction

    DEFF Research Database (Denmark)

    Jung, Young Hwa; Christiansen, Ane Sælland; Johnsen, Rune

    2015-01-01

    electrochemical reaction is generally considered to be a pivotal feature for understanding the relationship between layered structures and electrochemical properties. Here the structure, phase stability, and electrochemical properties of two kinds of layered oxides, P2 and O3, are investigated through in......-situ synchrotron XRD experiments. A capillary Na-based cell is designed to minimize interference in other substances such as a separator or external battery parts. This approach could give us to obtain clear diffraction patterns with high intensity during electrochemical reaction in a short period of time without...... further relaxation step. We carefully scrutinized reversible structural phase transformations during electrochemical reaction of P2 and O3-layered compounds based on in situ analysis, and detailed results will be discussed....

  11. Application of in situ x-ray diffraction techniques in heterogenous catalytic systems

    International Nuclear Information System (INIS)

    Sharifah Bee Abd Hamid

    2002-01-01

    A broad range of techniques is available today for the characterisation of catalysts and the investigation of catalyst reaction mechanisms. However, only a limited number of those are suitable for in situ studies, i.e experiments performed in conditions mimicking or close as possible to real operating conditions. Various commercially and in-house developed in situ X-Ray diffraction (XRD) cells have been used to obtain information on the phase and structure of materials at the initial formation stage, activation methodology, calcination, reduction and carburization. A major advantage of the in situ X-ray cells is that it allows direct observations on the decomposition of precursors leading to various phases in a controlled environment, i.e. controlled temperature and pressure under specified gases. The cells can be operated both at high temperatures and high pressures, equipped with Position Sensitive Detector (PSD), feature which was used to study phase transformation occurring during the activation of various solids. In MoO 3 , XRD results provide detailed information on the hydrogen insertion into its lattice, followed by carburization providing good understanding on the mechanism in the solid transformation leading to the metastable MoC 1 -x phase. For the Bi-SnO x systems, the environmental cell coupled with XRD and PSD allow the design of activation procedure to obtain the active Bi 2 Sn 2 O 7 . The in situ XRD technique reveals crucial information on the initial stage of oxides formations prior to condensation reaction shown in MCM-41 and titania systems. In this presentation, discussions on general achievements and problems relating to the use of in situ XRD techniques as well as of specific examples selected to illustrate the use and potential of in situ XRD are made. It is not intended to be a review of the art but a highlight of the challenges which the catalytic and material scientists face when entering the avenue. (Author)

  12. Hydrogen Absorption in Metal Thin Films and Heterostructures Investigated in Situ with Neutron and X-ray Scattering

    Directory of Open Access Journals (Sweden)

    Sara J. Callori

    2016-05-01

    Full Text Available Due to hydrogen possessing a relatively large neutron scattering length, hydrogen absorption and desorption behaviors in metal thin films can straightforwardly be investigated by neutron reflectometry. However, to further elucidate the chemical structure of the hydrogen absorbing materials, complementary techniques such as high resolution X-ray reflectometry and diffraction remain important too. Examples of work on such systems include Nb- and Pd-based multilayers, where Nb and Pd both have strong affinity to hydrogen. W/Nb and Fe/Nb multilayers were measured in situ with unpolarized and polarized neutron reflectometry under hydrogen gas charging conditions. The gas-pressure/hydrogen-concentration dependence, the hydrogen-induced macroscopic film swelling as well as the increase in crystal lattice plane distances of the films were determined. Ferromagnetic-Co/Pd multilayers were studied with polarized neutron reflectometry and in situ ferromagnetic resonance measurements to understand the effect of hydrogen absorption on the magnetic properties of the system. This electronic effect enables a novel approach for hydrogen sensing using a magnetic readout scheme.

  13. In situ electron backscatter diffraction (EBSD) during the compression of micropillars

    International Nuclear Information System (INIS)

    Niederberger, C.; Mook, W.M.; Maeder, X.; Michler, J.

    2010-01-01

    For the first time, in situ electron backscatter diffraction (EBSD) measurements during compression experiments by a modified nanoindenter on micron-sized single crystal pillars are demonstrated here. The experimental setup and the requirements concerning the compression sample are described in detail. EBSD mappings have been acquired before loading, under load and after unloading for consecutive compression cycles on a focused ion beam (FIB) milled GaAs micropillar. In situ EBSD allows for the determination of crystallographic orientation with sub-100 nm spatial resolution. Thereby, it provides highly localized information pertaining to the deformation phenomena such as elastic bending of the micropillar or the formation of deformation twins and plastic orientation gradients due to geometrically necessary dislocations. The most striking features revealed by in situ EBSD are the non-negligible amount of reversible (elastic) bending of the micropillar and the fact that deformation twinning and dislocation glide initiate where the bending is strongest. Due to this high spatial and orientation resolution, in situ EBSD measurements during micromechanical testing are demonstrated to be a promising technique for the investigation of deformation phenomena at the nano- to micro-scale.

  14. Neutron powder diffraction at a pulsed neutron source: a study of resolution effects

    International Nuclear Information System (INIS)

    Faber, J. Jr.; Hitterman, R.L.

    1985-11-01

    The General Purpose Powder Diffractometer (GPPD), a high resolution (Δd/d = 0.002) time-of-flight instrument, exhibits a resolution function that is almost independent of d-spacing. Some of the special properties of time-of-flight scattering data obtained at a pulsed neutron source will be discussed. A method is described that transforms wavelength dependent data, obtained at a pulsed neutron source, so that standard structural least-squares analyses can be applied. Several criteria are given to show when these techniques are useful in time-of-flight data analysis. 14 refs., 6 figs., 1 tab

  15. Sample positioning in neutron diffraction experiments using a multi-material fiducial marker

    Energy Technology Data Exchange (ETDEWEB)

    Marais, D., E-mail: Deon.Marais@necsa.co.za [Research and Development Division, South African Nuclear Energy Corporation (Necsa) SOC Limited, PO Box 582, Pretoria 0001 (South Africa); School of Mechanical and Nuclear Engineering, North-West University, Potchefstroom 2520 (South Africa); Venter, A.M., E-mail: Andrew.Venter@necsa.co.za [Research and Development Division, South African Nuclear Energy Corporation (Necsa) SOC Limited, PO Box 582, Pretoria 0001 (South Africa); Faculty of Agriculture Science and Technology, North-West University, Mahikeng 2790 (South Africa); Markgraaff, J., E-mail: Johan.Markgraaff@nwu.ac.za [School of Mechanical and Nuclear Engineering, North-West University, Potchefstroom 2520 (South Africa); James, J., E-mail: Jon.James@open.ac.uk [Faculty of Mathematics, Computing and Technology, The Open University, Milton Keynes, MK76AA England (United Kingdom)

    2017-01-01

    An alternative sample positioning method is reported for use in conjunction with sample positioning and experiment planning software systems deployed on some neutron diffraction strain scanners. In this approach, the spherical fiducial markers and location trackers used with optical metrology hardware are replaced with a specifically designed multi-material fiducial marker that requires one diffraction measurement. In a blind setting, the marker position can be determined within an accuracy of ±164 µm with respect to the instrument gauge volume. The scheme is based on a pre-determined relationship that links the diffracted peak intensity to the absolute positioning of the fiducial marker with respect to the instrument gauge volume. Two methods for establishing the linking relationship are presented, respectively based on fitting multi-dimensional quadratic functions and a cross-correlation artificial neural network.

  16. Neutron diffraction studies of water in meso- and micro-pores

    International Nuclear Information System (INIS)

    Steytler, D.C.; Dore, J.C.; Wright, C.J.

    1982-07-01

    Neutron diffraction studies have been made for D 2 O water in two high surface-area silica samples, Spherisorb and Gasil. The results show that the structural arrangement is similar to that of bulk water and that the modification due to the interface is restricted to a range of the order of 10 A or less. Measurements also indicate that the dispersed water undergoes significant structural changes with temperature variation but the behaviour is similar to that of the bulk liquid. The differences observed in the diffraction patterns can be partially described in terms of diffraction broadening due to the small volume of the dispersed water but there remains a significant variation which appears to be related to the hydrogen-bonding interactions. (author)

  17. Study of the α and β phases of quartz by neutron multiple diffraction

    International Nuclear Information System (INIS)

    Mazzocchi, V.L.

    1984-01-01

    Crystal structures of α and β phases of quartz are studied, employing neutron multiple diffraction as a method of analysis. Theoretical multiple diffraction patterns in a many-beam case were determined by a computer program which calculates intensities of beams as sums of Taylor's series expansions, retaining terms up to a order n. Experimental 'umweg' and transmitted beam patterns were obtained for the 00.1 primary reflection of α and β phases of quartz. To calculate α - quartz multiple diffraction intensities it was necessary to determine the Dauphine twinning fraction for the crystal after having passed by the β-phase. For the two models of β-quartz a better agreement between experimental and calculated integrated intensities was found for the disordered structure model based on split-half-oxigen positions. (Author) [pt

  18. Neutron- and X-ray diffraction investigations for the metallic glasses Ni81B19 and Co80P20

    International Nuclear Information System (INIS)

    Sperl, W.

    1982-01-01

    By means of isotope substitution for three chemically and technically identical amorphous Ni 81 B 19 samples neutron diffraction experiments are performed and the partial structure factors and the partial pair correlation functions are determined. (BHO)

  19. Neutron diffraction investigation of hysteresis reduction and increase in linearity in the stress-strain response of superelastic NiTi

    International Nuclear Information System (INIS)

    Rathod, C.R.; Clausen, B.; Bourke, M.A.M.; Vaidyanathan, R.

    2006-01-01

    In situ neutron diffraction measurements during loading have been performed on plastically deformed superelastic NiTi samples. The measurements observed retained B19 ' phase in the unloaded state as a result of the plastic deformation in otherwise completely B2 phase samples. A reversible stress-induced B2-B19 ' transformation on application and removal of stress occurred in the presence of this retained B19 ' phase. The amount and orientation of this retained B19 ' phase changed with cycling. Such direct atomic scale observations in the bulk are used here for the first time to qualitatively elucidate the macroscopic stress-strain response in plastically deformed superelastic NiTi

  20. Investigation of the neutron diffraction anomaly and electrical behaviour of α-LiIO3 single crystal under AC field

    International Nuclear Information System (INIS)

    Wang Guang; Yang Zhen

    1990-01-01

    A systematic study of the unique neutron diffraction and electric behaviour of α-LiIO 3 single crystal under AC field is reported. A frequency dependent rectification effect was observed and can be explained as the relaxation process in the ionic conduction. Theoretical treatment using Boltzmann equation gives satisfactory agreement with experimental results. The neutron diffraction anomaly can be attributed to the effect of the rectified DC current in the sample

  1. In situ X-ray diffraction studies on the piezoelectric response of PZT thin films

    Energy Technology Data Exchange (ETDEWEB)

    Davydok, A., E-mail: davydok@mpie.de [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Max-Planck-Institut für Eisenforschung, Department Structure and Nano-/Micromechanics of Materials, D-40237 Düsseldorf (Germany); Cornelius, T.W. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Mocuta, C. [SOLEIL Synchrotron, DiffAbs beamline, L' Orme des Merisiers, Saint-Aubin - BP 48, 91192 Gif-sur-Yvette Cedex (France); Lima, E.C. [Universidade Federal do Tocantins, 77500-000 Porto Nacional, TO (Brazil); Araujo, E.B. [Departamento de Fisica e Quimica, Universidade Estadual Paulista, Av. Brasil, 56 Centro, 15385-000 Ilha Solteira, SP (Brazil); Thomas, O. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France)

    2016-03-31

    Piezoelectric properties of randomly oriented self-polarized PbZr{sub 0.50}Ti{sub 0.50}O{sub 3} (PZT) thin films were investigated using in situ synchrotron X-ray diffraction. Possibilities for investigating the piezoelectric effect using micro-sized hard X-ray beams are demonstrated and perspectives for future dynamical measurements on PZT samples with variety of compositions and thicknesses are given. Studies performed on the crystalline [100, 110] directions evidenced piezoelectric anisotropy. The piezoelectric coefficient d{sub 33} was calculated in terms of the lab reference frame (d{sub perp}) and found to be two times larger along the [100] direction than along the [110] direction. The absolute values for the d{sub perp} amount to 120 and 230 pm/V being in good agreement with experimental and theoretical values found in literature for bulk PZT ceramics. - Highlights: • We performed in situ synchrotron X-ray diffraction studies on (PZT) thin films. • We discuss anisotropy of piezo effect in different crystallographic directions. • Perpendicular component Piezo coefficient of thin PZT layer is defined.

  2. Residual Stress Measurement of Coarse Crystal Grain in Aluminium Casting Alloy by Neutron Diffraction

    International Nuclear Information System (INIS)

    Nishida, Masayuki; Watanabe, Yoshitaka; Hanabusa, Takao

    2009-01-01

    Full text: Neutron stress measurement can detect strain and stress information in deep region because of large penetration ability of neutron beams. The present paper describes procedure and results in the residual stress measurement of aluminium casting alloy by neutron diffraction. Usually, the aluminium casting alloy includes the large crystal grains. The existence of large crystal grains makes it difficult to estimate the residual stresses in highly accuracy. In this study, the modified three axial method using Hook's equation was employed for neutron stress measurement. These stress measurements were performed under the two kinds of new techniques. One is a rocking curve method to calculate the principal strains in three directions. The peak profiles which appear discretely on rocking curves were translated to principle stresses by the Bragg law and the basic elastic theory. Another is the consideration of measurement positions and the edge effect in the neutron irradiated area (volume gage). The edge effect generates the errors of 2θ-peak position in the neutron stress measurement. In this study, the edge effect was investigated in detail by a small bit of copper single crystal. The copper bit was moved and scanned on three dimensionally within the gage volume. Furthermore, the average strains of symmetrical positions are measure by the sample turning at 180 degrees, because the error distributions of the 2θ-peak position followed to positions inside the gage volume. Form these results of this study, the residual stresses in aluminium casting alloy which includes the large crystal grains were possible to estimate by neutron stress measurement with the rocking curve method and the correction of the edge effect. (author)

  3. Preferred orientation of a naturally and experimentally deformed pyrrhotite ore by X-ray and neutron diffraction texture analysis

    International Nuclear Information System (INIS)

    Niederschlag, E.; Brokmeier, H.G.; Siemes, H.

    1994-01-01

    Two samples of polycrystalline naturally deformed hexagonal Pyrrhotite were deformed experimentally in axial compression tests with different temperatures and strain. The texture of the naturally deformed ore was investigated both by X-ray and neutron texture analyses. Texture measurements on the experimentally deformed ore were carried out by neutron diffraction. (orig.)

  4. Historical review of neutron spectrometry and diffraction in Brazil - 50 years

    International Nuclear Information System (INIS)

    Voi, Dante L.; Ferreira, Francisco J.O.; Stasiulevicius, Roberto; Rodrigues, Claudio; Parente, Carlos B.R.; Mazzocchi, Vera L.; Mestnik Filho, Jose; Pugliesi, Reinaldo

    2011-01-01

    Neutron Spectrometry and Diffraction techniques began to be studied in Brazil with the construction of the first research reactors in the years 50 and 60, and were developed with the participation of national and international scientists. In particular, we note the perseverance of the Brazilian pioneer of nuclear energy, Dr. Marcello Damy de Souza Santos, and from that time, with the involvement of some of the early pioneers, such as the physicist Roberto Stasiulevicius, who had the privilege of working in all three Brazilian nuclear research reactors. All these scientists shared half a century of acquired knowledge, helping in the training of a number of experts who are now working in national and international nuclear institutes. The present work reviews in chronological order, the testimony of the historical facts associated with the development and application of experimental techniques using neutrons as a tool for materials analysis and studies for many areas of the sciences and also with the training of personnel. IPEN, IEN and CDTN, all institutes of the CNEN-Brazil, are important in the national and international scene as a result of the research carried out there and the large number of publications produced in the field of neutron spectrometry and diffraction from experimental work carried out using the IEA (5MW), Argonauta (5kW) and more recently, the IPR (250kW) research reactors. An extensive bibliography is also presented and this can be disseminated to everyone interested. (author)

  5. Neutron diffraction studies on lattice strain evolution around a crack-tip during tensile loading and unloading cycles

    Energy Technology Data Exchange (ETDEWEB)

    Sun Yinan [Department of Materials Science and Engineering, University of Tennessee, Knoxville, TN 37996 (United States)]. E-mail: ysun1@utk.edu; Choo, Hahn [Department of Materials Science and Engineering, University of Tennessee, Knoxville, TN 37996 (United States); Metals and Ceramics Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Liaw, Peter K. [Department of Materials Science and Engineering, University of Tennessee, Knoxville, TN 37996 (United States); Lu Yulin [Department of Materials Science and Engineering, University of Tennessee, Knoxville, TN 37996 (United States); Yang Bing [Department of Materials Science and Engineering, University of Tennessee, Knoxville, TN 37996 (United States); Brown, Donald W. [Materials Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Bourke, Mark A.M. [Materials Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

    2005-10-15

    Elastic lattice-strain profiles ahead of a fatigue-crack-tip were measured during tensile loading and unloading cycles using neutron diffraction. The crack-closure phenomenon after an overload was observed. Furthermore, the plastic-zone size in front of the crack-tip was estimated from the diffraction-peak broadening, which showed good agreement with the calculated result.

  6. Quantitative phase analysis of alumina/calcium-hexaluminate composites using neutron diffraction data and the Rietveld method

    International Nuclear Information System (INIS)

    Asmi, D.; Low, I.M.; O'Connor, B.H.; Kennedy, S.J.

    2000-01-01

    Full text: The Al 2 O 3 -CaO system is the basis of an important class of high-temperature refractories in the steel industry. It contains a number of stable intermediate compounds which include C 3 A, C 12 A 7 , CA, CA 2 , and CA 6 . These calcium aluminates are also important constituents of high alumina cement and have been used to produce high-strength and high-toughness ceramic-polymer composite materials. More recently, alumina composites containing 30 wt% CA 6 platelets have been developed by An et al which show characteristics of self-reinforcement and enhanced toughening through crack-bridging. In this paper, we describe the use of high-temperature neutron diffraction to monitor the in-situ phase formation and abundances of calcium aluminates (CA, CA 2 , and CA 6 ) in alumina composites containing 5-50 wt % CA 6 .at temperatures in the range 1000 - 1600 deg C. These composites were produced using reaction sintering of alumina and calcium oxide. For comparison purposes, control samples of pure α-alumina and CA 6 were also produced. Determination of relative phase abundances in these materials has been performed using the standardless Rietveld refinement method. Results show that the relative phase abundance of calcium aluminates in the composites increased with temperature and in proportion with the amount of calcium oxide present. The formation temperatures of CA, CA 2 , and CA 6 have been observed to occur at 1000 deg , 1200 deg, and ∼1350 deg C respectively, which agree well with results obtained from x-ray diffraction, synchrotron radiation diffraction and differential thermal analysis

  7. Perdeuteration, purification, crystallization and preliminary neutron diffraction of an ocean pout type III antifreeze protein

    International Nuclear Information System (INIS)

    Petit-Haertlein, Isabelle; Blakeley, Matthew P.; Howard, Eduardo; Hazemann, Isabelle; Mitschler, Andre; Haertlein, Michael; Podjarny, Alberto

    2009-01-01

    Perdeuterated type III antifreeze protein has been expressed, purified and crystallized. Preliminary neutron data collection showed diffraction to 1.85 Å resolution from a 0.13 mm 3 crystal. The highly homologous type III antifreeze protein (AFP) subfamily share the capability to inhibit ice growth at subzero temperatures. Extensive studies by X-ray crystallography have been conducted, mostly on AFPs from polar fishes. Although interactions between a defined flat ice-binding surface and a particular lattice plane of an ice crystal have now been identified, the fine structural features underlying the antifreeze mechanism still remain unclear owing to the intrinsic difficulty in identifying H atoms using X-ray diffraction data alone. Here, successful perdeuteration (i.e. complete deuteration) for neutron crystallographic studies of the North Atlantic ocean pout (Macrozoarces americanus) AFP in Escherichia coli high-density cell cultures is reported. The perdeuterated protein (AFP D) was expressed in inclusion bodies, refolded in deuterated buffer and purified by cation-exchange chromatography. Well shaped perdeuterated AFP D crystals have been grown in D 2 O by the sitting-drop method. Preliminary neutron Laue diffraction at 293 K using LADI-III at ILL showed that with a few exposures of 24 h a very low background and clear small spots up to a resolution of 1.85 Å were obtained using a ‘radically small’ perdeuterated AFP D crystal of dimensions 0.70 × 0.55 × 0.35 mm, corresponding to a volume of 0.13 mm 3

  8. Preliminary neutron diffraction analysis of challenging human manganese superoxide dismutase crystals.

    Science.gov (United States)

    Azadmanesh, Jahaun; Trickel, Scott R; Weiss, Kevin L; Coates, Leighton; Borgstahl, Gloria E O

    2017-04-01

    Superoxide dismutases (SODs) are enzymes that protect against oxidative stress by dismutation of superoxide into oxygen and hydrogen peroxide through cyclic reduction and oxidation of the active-site metal. The complete enzymatic mechanisms of SODs are unknown since data on the positions of hydrogen are limited. Here, methods are presented for large crystal growth and neutron data collection of human manganese SOD (MnSOD) using perdeuteration and the MaNDi beamline at Oak Ridge National Laboratory. The crystal from which the human MnSOD data set was obtained is the crystal with the largest unit-cell edge (240 Å) from which data have been collected via neutron diffraction to sufficient resolution (2.30 Å) where hydrogen positions can be observed.

  9. Extra spots in the electron diffraction patterns of neutron irradiated zirconium and its alloys

    International Nuclear Information System (INIS)

    Madden, P.K.

    1977-01-01

    Specimens of neutron irradiated zirconium and its alloys were examined in the transmission electron microscope. Groups of extra spots, often exhibiting four-fold symmetry, were observed in thin foil electron diffraction patterns of these specimens. The 'extra-spot' structure, like the expected black-dot/small scale dislocation loop neutron irradiated damage, is approximately 100 A in size. Its nature is uncertain. It may be related to irradiation damage or to some artefact introduced during specimen preparation. If it is the latter, then published irradiation damage defect size distributions and determined irradiation growth strains of other investigators, may require modification. The present inconclusive results indicate that extra-spot structure is likely to consist of oxide particles, but may correspond to hydride precipitation or decoration effects, or even, to electron beam effects. (author)

  10. X-ray and neutron diffraction and molecular dynamics simulation of molten lithium and rubidium nitrates

    International Nuclear Information System (INIS)

    Yamaguchi, Toshio; Okada, Isao; Ohtaki, Hitoshi; Mikami, Masuhiro; Kawamura, Kazutaka

    1986-01-01

    Molecular dynamics simulations have been performed for lithium and rubidium nitrate melts at 550 and 600K, respectively, together with X-ray and neutron diffraction experiments. Simple Coulomb pair potentials with Born-type repulsions have been adopted in the simulations with a rigid body model for the nitrate ion. Structure functions derived from the X-ray and neutron experiments are well reproduced by the simulations, from which the three-dimensional cation distribution around the nitrate ion has been revealed. The self-diffusion coefficients, the velocity autocorrelation functions and the self-exchange velocities of lithium, rubidium and nitrate ions have been calculated. Anisotropic motion of nitrate ions has been found and is discussed on the basis of the structure of the melts. (author)

  11. Measurement of residual strain in composites by means of time-of- flight neutron diffraction

    International Nuclear Information System (INIS)

    Kupperman, D.S.; Majumdar, S.; Richardson, J.; Saigal, A.

    1993-01-01

    Neutron diffraction time-of-flight measurements using the Intense Pulsed Neutron Source at Argonne National Laboratory have been employed to study strain in various metal- and ceramic-matrix composites. For example, measurements carried out to 900 C on a composite composed of a titanium alloy matrix and silicon carbide fibers have been used to validate theoretical assumptions in the prediction of fabrication-induced residual stress. Sapphire reinforced nickel aluminide composites have also been studied. Studies of a high-temperature ceramic superconducting composite consisting of yttrium barium copper oxide and silver with various volume fractions of silver have also been carried out. The results of these studies have provided information on the effect of Ag content on interface bonding. In addition, ceramic-matrix composites with randomly dispersed ceramic whiskers with varying fiber content have been investigated

  12. Comparison of neutron and synchrotron diffraction measurements of residual stress in bead-on-plate weldments

    International Nuclear Information System (INIS)

    Paradowska, A.M.; Price, J.W.; Finlayson, T.R.; Lienert, U.; Ibrahim, R.

    2010-01-01

    This paper explores the use of neutron and synchrotron diffractions for the evaluation of residual stresses in welded components. It has been shown that it is possible to achieve very good agreement between the two independent diffraction techniques. This study shows the significance of the weld start and end sites on the residual strain/stress distribution. Quantitative evaluation of the residual stress development process for multibead weldments has been presented. Some measurements were also taken before and after postweld stress relieving to establish the reduction and redistribution of the residual stress. The detailed measurements of residual stress around the weld achieved in this work significantly improve the knowledge and understanding of residual stress in welded components.

  13. Integrated intensities and flipping ratios in neutron diffraction by perfect magnetic crystals

    International Nuclear Information System (INIS)

    Guigay, J.P.; Schlenker, M.

    1979-01-01

    A theoretical study of neutron diffraction by perfect magnetic crystals is presented which shows that when the magnetization is perpendicular to the diffraction vector (β- π/2), the dispersion surface is made up of two hyperbolic surfaces corresponding to simple polarization states and the results of the two-beam dynamical theory for non-magnetic crystals can be directly applied. The asymptotic properties of the dispersion surface are of the dispersion surface are also discussed in the more general case (β is not equal to π/2) and an analytical treatment of the kinematical limit is presented. Integrated intensities and flipping ratios outside this limit can only be calculated numerically. It is shown that the wave fields defined by the different points of the dispersion surface are polarized in the (g, B 0 ) plane; this is a generalization of the fact that they are (+-) states with respect to B 0 in the simple case (β=π/2). (UK)

  14. Thermal diffuse scattering in time-of-flight neutron diffraction studied on SBN single crystals

    International Nuclear Information System (INIS)

    Prokert, F.; Savenko, B.N.; Balagurov, A.M.

    1994-01-01

    At time-of-flight (TOF) diffractometer D N-2, installed at the pulsed reactor IBR-2 in Dubna, Sr x Ba 1-x Nb 2 O 6 mixed single crystals (SBN-x) of different compositions (0.50 < x< 0.75) were investigated between 15 and 773 K. The diffraction patterns were found to be strongly influenced by the thermal diffuse scattering (TDS). The appearance of the TDS from the long wavelength acoustic models of vibration in single crystals is characterized by the ratio of the velocity of sound to the velocity of neutron. Due to the nature of the TOF Laue diffraction technique used on D N-2, the TDS around Bragg peaks has rather a complex profile. An understanding of the TDS close to Bragg peaks is essential in allowing the extraction of the diffuse scattering occurring at the diffuse ferroelectric phase transition in SBN crystals. 11 refs.; 9 figs.; 1 tab. (author)

  15. Structure of molten TbCl sub 3 measured by neutron diffraction

    CERN Document Server

    Martin, R A; Barnes, A C; Cuello, G J

    2002-01-01

    The total structure factor of molten TbCl sub 3 at 617 deg. C was measured by using neutron diffraction. The data are in agreement with results from previous experimental work but the use of a diffractometer having an extended reciprocal-space measurement window leads to improved resolution in real space. Significant discrepancies with the results obtained from recent molecular dynamics simulations carried out using a polarizable ion model, in which the interaction potentials were optimized to enhance agreement with previous diffraction data, are thereby highlighted. It is hence shown that there is considerable scope for the development of this model for TbCl sub 3 and for other trivalent metal halide systems spanning a wide range of ion size ratios. (letter to the editor)

  16. Refinement of the ferri and paramagnetic phases of magnetite measured by neutron multiple diffraction

    International Nuclear Information System (INIS)

    Mazzochi, V.L.; Parente, C.B.R.

    1989-10-01

    Structural parameters of the ferri and paramagnetic phases of magnetite have been refined from neutron multiple diffraction data. Experimental patterns were obtained by measuring the III primary reflection of a natural single crystal of this compound, at room temperature for the ferrimagnetic phase and 703 0 C for the paramagnetic phase. Theoretical multiple diffraction patterns for both phases have been calculated by the program MULTI which uses the iterative method. In this method intensities are caluclated as Taylor series expansions summed up to a order sufficient for a good approximation. A step by step process has been used in the refinements similarly to the parameter-shift method. Final values for the discrepancy factor found for the ferri and paramagnetic phases were R = 3.96% and R = 3.46%, respectively. (author) [pt

  17. Discussion on accuracy of weld residual stress measurement by neutron diffraction. Influence of strain free reference

    International Nuclear Information System (INIS)

    Suzuki, Hiroshi; Akita, Koichi

    2012-01-01

    It is required to evaluate a strain-free reference, α 0 , to perform accurate stress measurement using neutron diffraction. In this study, accuracy of neutron stress measurement was quantitatively discussed from α 0 evaluations on a dissimilar metal butt-weld between a type 304 austenitic stainless steel and an A533B low alloy ferritic steel. A strain-free standard specimen and a sliced specimen with 10 mm thickness taken from the dissimilar metal butt-weld were utilized. In the lattice constant evaluation using the standard specimen, average lattice constant derived from multiple hkl reflections was evaluated as the stress-free reference with cancelling out an intergranular strain. Comparing lattice constant distributions in each reflection with average lattice constant distribution in the standard specimen, αFe211 and γFe311 reflections were judged as a suitable reflection for neutron strain measurement to reduce intergranular strain effects. Residual stress distribution in the sliced specimen evaluated using α 0 measured here exhibited higher accuracy than that measured using strain gauges. On the other hand, α 0 distributions were evaluated using the sliced specimen under the plane-stress condition. Existence of slight longitudinal residual stresses near the weld center decreased accuracy of the α 0 evaluations, which means that it is required to optimize the thickness of the sliced specimen for accurate α 0 evaluation under plane strain condition. As a conclusion of this study, it was confirmed that procedures of accurate α 0 evaluation, optimization of the measurement condition, and multiple evaluations on the results play an important role to improve accuracy of the residual stress measurement using neutron diffraction. (author)

  18. Residual Stress Distribution In Heat Affected Zone Of Welded Steel By Means Of Neutron Diffraction Method

    International Nuclear Information System (INIS)

    Fajar, Andika; Prasuad; Gunawan; Muslich, M. Rifai

    1996-01-01

    Three dimensional residual stress distribution in the heat affected zone of 10 mm thick welded steel by means of neutron diffraction technique has been measured. The results showed that the residual stress was distributed near the welded metal, namely within about 46,25 mm. The major tensile stresses occurred in the X-direction, and they attained a level greater than 2000 MPa through the position far away fram the weld. The tensile stresses in the Y and Z- directions lied between 500 and 1500 MPa, The results also suggest that the stress in the surface was greater than that in the middle of the sample

  19. Data analysis of a polycrystalline nickel sample obtained with neutron diffraction

    International Nuclear Information System (INIS)

    Parente, C.B.R.; Mazzochi, V.L.; Araujo Kaschny, J.R. de; Costa, M.S. da; Rizzo, P.; Campos, W.M.S.

    1990-01-01

    A simple analysis of the nickel structure was made. Neutron diffraction data were used, obtained with polycrystalline nickel placed in a cylindrical sample-holder with dimensions of 1,5cm of diameter and 5cm of height. The theoretical intensities were calculated of 3 forms: 1. without considering the temperature and obsorption effects, 2. considering only the temperature effect and 3. considering both the temperature and absorption effects. The disagreement factors found in this 3 cases were, respectively, R 1 = 13.4%, R 2 = 7,7% e R 3 = 7,5%. (L.C.)

  20. Single-crystal neutron diffraction study of ammonium nitrate phase III

    International Nuclear Information System (INIS)

    Choi, C.S.; Prask, H.J.

    1982-01-01

    The crystal structure of ammonium nitrate phase III has been studied at room temperature by neutron diffraction using a single crystal containing 5% KNO 3 in solid-solution form. The space group is Pnma, with a = 7.6772 (4), b = 5.8208 (4), c = 7.1396 (5) A, Z = 4. The final residual after full-matrix least-squares refinement was R = 0.042 for 348 observed reflections. The ammonium ions are thermally disordered into two orientations, displaced by an angle of approximately 42 0 about an axis parallel to the c axis. (Auth.)

  1. Neutron-Diffraction Study of the Phase Transition in Stannous Chloride Dihydrate

    DEFF Research Database (Denmark)

    Youngblood, R.; Kjems, Jørgen

    1979-01-01

    of the system does not change. We present neutron-diffraction results which show that the temperature dependence of the hydrogen-site occupancies is also highly symmetric around the phase-transition temperature. These results are discussed in terms of a lattice statistical model which was proposed and solved......The order-disorder phase transition in two-dimensional hydrogen-bonded layers of water molecules in SnCl2·2D2O is remarkable in several respects. It has been shown that the peak in the specific heat is highly symmetric around the phase-transition temperature, and that the crystallographic symmetry...

  2. On the atomic structure of liquid Ni-Si alloys: a neutron diffraction study

    Science.gov (United States)

    Gruner, S.; Marczinke, J.; Hennet, L.; Hoyer, W.; Cuello, G. J.

    2009-09-01

    The atomic structure of the liquid NiSi and NiSi2 alloys is investigated by means of neutron diffraction experiments with isotopic substitution. From experimental data-sets obtained using four Ni isotopes, partial structure factors and pair correlation functions are obtained by applying a reverse Monte Carlo modelling approach. Both alloys were found to exhibit a strong tendency to hetero-coordination within the first coordination shell. In particular, covalent Si-Si bonds with somewhat greater distances seem to influence the structure of the liquid NiSi alloy.

  3. On the atomic structure of liquid Ni-Si alloys: a neutron diffraction study

    Energy Technology Data Exchange (ETDEWEB)

    Gruner, S; Marczinke, J; Hoyer, W [Institute of Physics, Chemnitz University of Technology, D-09107 Chemnitz (Germany); Hennet, L [CNRS-CEMHTI, University of Orleans, F-45071 Orleans (France); Cuello, G J, E-mail: sascha.gruner@physik.tu-chemnitz.d [Institute Laue-Langevin, PO Box 156, F-38042 Grenoble (France)

    2009-09-23

    The atomic structure of the liquid NiSi and NiSi{sub 2} alloys is investigated by means of neutron diffraction experiments with isotopic substitution. From experimental data-sets obtained using four Ni isotopes, partial structure factors and pair correlation functions are obtained by applying a reverse Monte Carlo modelling approach. Both alloys were found to exhibit a strong tendency to hetero-coordination within the first coordination shell. In particular, covalent Si-Si bonds with somewhat greater distances seem to influence the structure of the liquid NiSi alloy.

  4. Structures of high and low density amorphous ice by neutron diffraction

    International Nuclear Information System (INIS)

    Finney, J.L.; Hallbrucker, A.; Kohl, I.; Soper, A.K.; Bowron, D.T.

    2002-01-01

    Neutron diffraction with isotope substitution is used to determine the structures of high (HDA) and low (LDA) density amorphous ice. Both 'phases' are fully hydrogen bonded, tetrahedral networks, with local order similarities between LDA and ice Ih, and HDA and liquid water. Moving from HDA, through liquid water and LDA to ice Ih, the second shell radial order increases at the expense of spatial order. This is linked to a fifth first neighbor 'interstitial' that restricts the orientations of first shell waters. This 'lynch pin' molecule which keeps the HDA structure intact has implications for the nature of the HDA-LDA transition that bear on the current metastable water debate

  5. High resolution neutron diffraction crystallographic investigation of Oxide Dispersion Strengthened steels of interest for fusion technology

    International Nuclear Information System (INIS)

    Coppola, R.; Rodriguez-Carvajal, J.; Wang, M.; Zhang, G.; Zhou, Z.

    2014-01-01

    High resolution neutron diffraction measurements have been carried out to characterize the crystallographic phases present in different Oxide Dispersion Strengthened (ODS) steels of interest for fusion technology. The different lattice structures, Im3m for the ferritic ODS and Fm3m for the austenitic ODS, are resolved showing line anisotropy effects possibly correlated with differences in dislocation densities and texture. Many contributions from minority phases are detected well above the background noise; none of the expected crystallographic phases, such as M 23 C 6 and including Y 2 O 3 , fits them, but the TiN phase is identified in accordance with results of other microstructural techniques

  6. Neutron diffraction structure investigations for expanded liquid selenium up to 14000C and 300 bar

    International Nuclear Information System (INIS)

    Edeling, M.

    1980-01-01

    The static structure factor of the expanded liquid Selenium is measured by means of the neutron diffraction for temperatures between 600 0 C and 1400 0 C and for pressures up to 300 bar. From the structure factors the pair distribution functions show that the bond length of the Selenium atoms is constant 2.37 A to 2.38 A for the whole concentration range. For temperatures above 1200 0 C the calculated intermolecular coordination number shows that the intermolecular interaction increases. (BHO)

  7. Residual stress in sprayed Ni+5%Al coatings determined by neutron diffraction

    CERN Document Server

    Matejicek, J; Gnaeupel-Herold, T; Prask, H J

    2002-01-01

    Coatings of nickel-based alloys are used in numerous high-performance applications. Their properties and lifetimes are influenced by factors such as residual stress. Neutron diffraction is a powerful tool for nondestructive residual stress determination. In this study, through-thickness residual stress profiles in Ni+5%Al coatings on steel substrates were determined. Two examples of significantly different spraying techniques - plasma spraying and cold spraying - are highlighted. Different stress-generation mechanisms are discussed with respect to process parameters and material properties. (orig.)

  8. Hydride reorientation in Zircaloy-4 examined by in situ synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Weekes, H.E. [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom); Jones, N.G. [Department of Materials Science and Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS (United Kingdom); Lindley, T.C. [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom); Dye, D., E-mail: david.dye@imperial.ac.uk [Department of Materials, Royal School of Mines, Imperial College London, Prince Consort Road, London SW7 2BP (United Kingdom)

    2016-09-15

    The phenomenon of stress-reorientation has been investigated using in situ X-ray diffraction during the thermomechanical cycling of hydrided Zircaloy-4 tensile specimens. Results have shown that loading along a sample’s transverse direction (TD) leads to a greater degree of hydride reorientation when compared to rolling direction (RD)-aligned samples. The elastic lattice micro-strains associated with radially oriented hydrides have been revealed to be greater than those oriented circumferentially, a consequence of strain accommodation. Evidence of hydride redistribution after cycling, to α-Zr grains oriented in a more favourable orientation when under an applied stress, has also been observed and its behaviour has been found to be highly dependent on the loading axis. Finally, thermomechanical loading across multiple cycles has been shown to reduce the difference in terminal solid solubility of hydrogen during dissolution (TSS{sub D,H}) and precipitation (TSS{sub P,H}).

  9. In situ x-ray diffraction study on AgI nanowire arrays

    International Nuclear Information System (INIS)

    Wang Yinhai; Ye Changhui; Wang Guozhong; Zhang Lide; Liu Yanmei; Zhao Zhongyan

    2003-01-01

    The AgI nanowire arrays were prepared in the ordered porous alumina membrane by an electrochemical method. Transmission electron microscopy observation shows that the AgI nanowires are located in the channels of the alumina membrane. In situ x-ray diffractions show that the nanowire arrays possess hexagonal close-packed structure (β-AgI) at 293 K, orienting along the (002) plane, whereas at 473 K, the nanowire arrays possess a body-centered cubic structure (α-AgI), orienting along the (110) plane. The AgI nanowire arrays exhibit a negative thermal expansion property from 293 to 433 K, and a higher transition temperature from the β to α phase. We ascribe the negative thermal expansion behavior to the phase transition from the β to α phase, and the elevated transition temperature to the radial restriction by the channels of alumina membrane

  10. Atoms in Action: Observing Atomic Motion with Dynamic in situ X-ray Diffraction

    Science.gov (United States)

    Cox, Jordan Michael

    Metal-organic framework (MOF) materials are rich in both structural diversity and application. These materials are comprised of metal atoms or clusters which are connected in a three-dimensional polymer-like network by bridging organic linker molecules. One of the major attractive features in MOFs is their permanent pore space which can potentially be used to adsorb or exchange foreign molecules from/with the surrounding environment. While MOFs are an active area of scientific interest, MOF materials are still relatively new, only 20 years old. As such, there is still much that needs to be understood about these materials before they can be effectively applied to widespread chemical problems like CO2 sequestration or low-pressure hydrogen fuel storage. One of the most important facets of MOF chemistry to understand in order to rationally design MOF materials with tailor-made properties is the relationship between the structural features in a MOF and the chemical and physical properties of that material. By examining in detail the atomic structure of a MOF with known properties under a variety of conditions, scientists can begin to unravel the guiding principles which govern these relationships. X-ray diffraction remains one of the most effective tools for determining the structure of a crystalline material with atomic resolution, and has been applied to the determination of MOF structures for years. Typically these experiments have been carried out using powder X-ray diffraction, but this technique lacks the high-resolution structural information found in single-crystal methods. Some studies have been reported which use specialized devices, sometimes called Environmental Control Cells, to study single crystalline MOFs under non-ambient chemical conditions in situ . However, these in situ studies are performed under static conditions. Even in cases where the ECC provides continued access to the local chemical environment during diffraction data collections, the

  11. In Situ X-ray Diffraction Studies of (De)lithiation Mechanism in Silicon Nanowire Anodes

    KAUST Repository

    Misra, Sumohan

    2012-06-26

    Figure Persented: Silicon is a promising anode material for Li-ion batteries due to its high theoretical specific capacity. From previous work, silicon nanowires (SiNWs) are known to undergo amorphorization during lithiation, and no crystalline Li-Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li 15Si 4 phase forms, and we show that avoiding the formation of this phase, by modifying the SiNW growth temperature, improves the cycling performance of SiNW anodes. Our results provide insight on the (de)lithiation mechanism and a correlation between phase evolution and electrochemical performance for SiNW anodes. © 2012 American Chemical Society.

  12. Evaluation of neutron sources for ISAGE-in-situ-NAA for a future lunar mission

    International Nuclear Information System (INIS)

    Li, X.; Breitkreutz, H.; Burfeindt, J.; Bernhardt, H.-G.; Trieloff, M.; Hopp, J.; Jessberger, E.K.; Schwarz, W.H.; Hofmann, P.; Hiesinger, H.

    2011-01-01

    For a future Moon landing, a concept for an in-situ NAA involving age determination using the 40 Ar- 39 Ar method is developed. A neutron source 252 Cf is chosen for sample irradiation on the Moon. A special sample-in-source irradiation geometry is designed to provide a homogeneous distribution of neutron flux at the irradiation position. Using reflector, the neutron flux is likely to increase by almost 200%. Sample age of 1 Ga could be determined. Elemental analysis using INAA is discussed. - Highlights: → We developed a concept for an in-situ age determination on the Moon. → 252 Cf is chosen as the neutron source for the 40 Ar- 39 Ar-method. → A sample-in-source geometry is designed to provide homogeneous neutron flux. → Determination of U, Th, K and Ir using NAA on the Moon is possible.

  13. Evaluation of neutron sources for ISAGE-in-situ-NAA for a future lunar mission

    Energy Technology Data Exchange (ETDEWEB)

    Li, X., E-mail: xiaosong.li@frm2.tum.de [Forschungs-Neutronenquelle Heinz Maier-Leibnitz, FRM II, Technische Universitaet Muenchen, Lichtenbergstr. 1, D-85747 Garching (Germany); Breitkreutz, H. [Forschungs-Neutronenquelle Heinz Maier-Leibnitz, FRM II, Technische Universitaet Muenchen, Lichtenbergstr. 1, D-85747 Garching (Germany); Burfeindt, J.; Bernhardt, H.-G. [Kayser-Threde GmbH, Wolfratshauser Str. 48, D-81379 Muenchen (Germany); Trieloff, M.; Hopp, J. [Institut fuer Geowissenschaften, Ruprecht-Karls-Universitaet Heidelberg, D-69120 Heidelberg (Germany); Jessberger, E.K. [Institut fuer Planetologie, Westfaelische Wilhelms-Universitaet Muenster, D-48149 Muenster (Germany); Schwarz, W.H. [Institut fuer Geowissenschaften, Ruprecht-Karls-Universitaet Heidelberg, D-69120 Heidelberg (Germany); Hofmann, P. [Kayser-Threde GmbH, Wolfratshauser Str. 48, D-81379 Muenchen (Germany); Hiesinger, H. [Institut fuer Planetologie, Westfaelische Wilhelms-Universitaet Muenster, D-48149 Muenster (Germany)

    2011-11-15

    For a future Moon landing, a concept for an in-situ NAA involving age determination using the {sup 40}Ar-{sup 39}Ar method is developed. A neutron source {sup 252}Cf is chosen for sample irradiation on the Moon. A special sample-in-source irradiation geometry is designed to provide a homogeneous distribution of neutron flux at the irradiation position. Using reflector, the neutron flux is likely to increase by almost 200%. Sample age of 1 Ga could be determined. Elemental analysis using INAA is discussed. - Highlights: > We developed a concept for an in-situ age determination on the Moon. > {sup 252}Cf is chosen as the neutron source for the {sup 40}Ar-{sup 39}Ar-method. > A sample-in-source geometry is designed to provide homogeneous neutron flux. > Determination of U, Th, K and Ir using NAA on the Moon is possible.

  14. In-situ X-ray diffraction system using sources and detectors at fixed angular positions

    Science.gov (United States)

    Gibson, David M [Voorheesville, NY; Gibson, Walter M [Voorheesville, NY; Huang, Huapeng [Latham, NY

    2007-06-26

    An x-ray diffraction technique for measuring a known characteristic of a sample of a material in an in-situ state. The technique includes using an x-ray source for emitting substantially divergent x-ray radiation--with a collimating optic disposed with respect to the fixed source for producing a substantially parallel beam of x-ray radiation by receiving and redirecting the divergent paths of the divergent x-ray radiation. A first x-ray detector collects radiation diffracted from the sample; wherein the source and detector are fixed, during operation thereof, in position relative to each other and in at least one dimension relative to the sample according to a-priori knowledge about the known characteristic of the sample. A second x-ray detector may be fixed relative to the first x-ray detector according to the a-priori knowledge about the known characteristic of the sample, especially in a phase monitoring embodiment of the present invention.

  15. In situ electron backscatter diffraction investigation of recrystallization in a copper wire.

    Science.gov (United States)

    Brisset, François; Helbert, Anne-Laure; Baudin, Thierry

    2013-08-01

    The microstructural evolution of a cold drawn copper wire (reduction area of 38%) during primary recrystallization and grain growth was observed in situ by electron backscatter diffraction. Two thermal treatments were performed, and successive scans were acquired on samples undergoing heating from ambient temperature to a steady state of 200°C or 215°C. During a third in situ annealing, the temperature was continuously increased up to 600°C. Nuclei were observed to grow at the expense of the deformed microstructure. This growth was enhanced by the high stored energy difference between the nuclei and their neighbors (driving energy in recrystallization) and by the presence of high-angle grain boundaries of high mobility. In the early stages of growth, the nuclei twin and the newly created orientations continue to grow to the detriment of the strained copper. At high temperatures, the disappearance of some twins was evidenced by the migration of the incoherent twin boundaries. Thermal grooving of grain boundaries is observed at these high temperatures and affects the high mobile boundaries but tends to preserve the twin boundaries of lower energy. Thus, grooving may contribute to the twin vanishing.

  16. Rapid thermal processing chamber for in-situ x-ray diffraction

    International Nuclear Information System (INIS)

    Ahmad, Md. Imteyaz; Van Campen, Douglas G.; Yu, Jiafan; Pool, Vanessa L.; Van Hest, Maikel F. A. M.; Toney, Michael F.; Fields, Jeremy D.; Parilla, Philip A.; Ginley, David S.

    2015-01-01

    Rapid thermal processing (RTP) is widely used for processing a variety of materials, including electronics and photovoltaics. Presently, optimization of RTP is done primarily based on ex-situ studies. As a consequence, the precise reaction pathways and phase progression during the RTP remain unclear. More awareness of the reaction pathways would better enable process optimization and foster increased adoption of RTP, which offers numerous advantages for synthesis of a broad range of materials systems. To achieve this, we have designed and developed a RTP instrument that enables real-time collection of X-ray diffraction data with intervals as short as 100 ms, while heating with ramp rates up to 100 °Cs −1 , and with a maximum operating temperature of 1200 °C. The system is portable and can be installed on a synchrotron beamline. The unique capabilities of this instrument are demonstrated with in-situ characterization of a Bi 2 O 3 -SiO 2 glass frit obtained during heating with ramp rates 5 °C s −1 and 100 °C s −1 , revealing numerous phase changes

  17. Rapid thermal processing chamber for in-situ x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad, Md. Imteyaz; Van Campen, Douglas G.; Yu, Jiafan; Pool, Vanessa L.; Van Hest, Maikel F. A. M.; Toney, Michael F., E-mail: mftoney@slac.stanford.edu [SSRL, SLAC National Accelerator Laboratory, 2575, Sand Hill Road, Menlo Park, California 94025 (United States); Fields, Jeremy D.; Parilla, Philip A.; Ginley, David S. [National Renewable Energy Laboratory, Golden, Colorado 80401 (United States)

    2015-01-15

    Rapid thermal processing (RTP) is widely used for processing a variety of materials, including electronics and photovoltaics. Presently, optimization of RTP is done primarily based on ex-situ studies. As a consequence, the precise reaction pathways and phase progression during the RTP remain unclear. More awareness of the reaction pathways would better enable process optimization and foster increased adoption of RTP, which offers numerous advantages for synthesis of a broad range of materials systems. To achieve this, we have designed and developed a RTP instrument that enables real-time collection of X-ray diffraction data with intervals as short as 100 ms, while heating with ramp rates up to 100 °Cs{sup −1}, and with a maximum operating temperature of 1200 °C. The system is portable and can be installed on a synchrotron beamline. The unique capabilities of this instrument are demonstrated with in-situ characterization of a Bi{sub 2}O{sub 3}-SiO{sub 2} glass frit obtained during heating with ramp rates 5 °C s{sup −1} and 100 °C s{sup −1}, revealing numerous phase changes.

  18. In situ 2D diffraction as a tool to characterize ferroelectric and piezoelectric thin films

    Science.gov (United States)

    Khamidy, N. I.; Kovacova, V.; Bernasconi, A.; Le Rhun, G.; Vaxelaire, N.

    2017-08-01

    In this paper the application of 2D x-ray diffraction (XRD2) as a technique to characterize in situ during electrical cycling the properties of a ferroelectric and piezoelectric thin film is discussed. XRD2 is one type of XRD on which a 2D detector is used instead of a point detector. This technique enables simultaneous recording of many sample information in a much shorter time compared to conventional XRD. The discussion is focused especially on the data processing technique of the huge data acquired. The methodology to calculate an effective piezoelectric coefficient, analyze the phase and texture, and estimate the domain size and shape is described in this paper. This methodology is then applied to a lead zirconate titanate (PZT) thin film at the morphotropic phase boundary (MPB) composition (i.e. Pb[Zr0.52Ti0.48]O3) with a preferred orientation of (1 0 0). The in situ XRD2 characterization was conducted in the European synchrotron radiation facility (ESRF) in Grenoble, France. Since a high-energy beam with vertical resolution as small as 100 nm was used, a cross-sectional scan of the sample was performed over the entire thickness of the film. From these experimental results, a better understanding on the piezoelectricity phenomena in PZT thin film at MPB composition were achieved, providing original feedback between the elaboration processes and functional properties of the film.

  19. Shock Melting of Iron Silicide as Determined by In Situ X-ray Diffraction.

    Science.gov (United States)

    Newman, M.; Kraus, R. G.; Wicks, J. K.; Smith, R.; Duffy, T. S.

    2016-12-01

    The equation of state of core alloys at pressures and temperatures near the solid-liquid coexistence curve is important for understanding the dynamics at the inner core boundary of the Earth and super-Earths. Here, we present a series of laser driven shock experiments on textured polycrystalline Fe-15Si. These experiments were conducted at the Omega and Omega EP laser facilities. Particle velocities in the Fe-15Si samples were measured using a line VISAR and were used to infer the thermodynamic state of the shocked samples. In situ x-ray diffraction measurements were used to probe the melting transition and investigate the potential decomposition of Fe-15Si in to hcp and B2 structures. This work examines the kinetic effects of decomposition due to the short time scale of dynamic compression experiments. In addition, the thermodynamic data collected in these experiments adds to a limited body of information regarding the equation of state of Fe-15Si, which is a candidate for the composition in Earth's outer core. Our experimental results show a highly textured solid phase upon shock compression to pressures ranging from 170 to 300 GPa. Below 320 GPa, we observe diffraction peaks consistent with decomposition of the D03 starting material in to an hcp and a cubic (potentially B2) structure. Upon shock compression above 320 GPa, the intense and textured solid diffraction peaks give way to diffuse scattering and loss of texture, consistent with melting along the Hugoniot. When comparing these results to that of pure iron, we can ascertain that addition of 15 wt% silicon increases the equilibrium melting temperature significantly, or that the addition of silicon significantly increases the metastability of the solid phase, relative to the liquid. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

  20. Phase separation and magnetic ordering studied by high resolution neutron diffraction

    International Nuclear Information System (INIS)

    Caspi, E.N.; Melamud, M.; Pinto, H.; Shaked, H.; Chmaissem, O.; Jorgensen, J.D.; Short, S.

    1999-01-01

    Complete text of publication follows. In a previous work on the (U 1-x Nd x )Co 2 Ge 2 system, two magnetic transitions were observed in the temperature dependencies of the magnetic susceptibility and in the intensity of the magnetic reflections in neutron diffraction [1]. Because of insufficient resolution, it was not clear whether this is due to clustering or phase separation. In both cases the U-rich regions are expected to order magnetically at higher temperature than the U-poor ones, resulting in two magnetic transitions. In order to resolve this question a temperature dependent TOF neutron diffraction of the x = 0.25 compound has been performed on the SEPD at Argonne's IPNS [2]. The temperature dependent diffractograms were refined by the Rietveld method. It was found that the compound separates into two phases: x = 0.4 (55 wt%) and x = 0.1 (45 wt%). The temperature dependence of the magnetic moment was obtained for each phase, with the transition temperatures: T N (x=0.4) = 130 K, and T N (x=0.1) = 165 K. (author) [1] E. Caspi et al., Phys. Rev. B, 57 (198) 449.; [2] J.D. Jorgensen et al., J. Appl. Cryst. 22 (1989) 321

  1. The chemical reactivity and structure of collagen studied by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Wess, T.J.; Wess, L.; Miller, A. [Univ. of Stirling (United Kingdom)

    1994-12-31

    The chemical reactivity of collagen can be studied using neutron diffraction (a non-destructive technique), for certain reaction types. Collagen contains a number of lysine and hydroxylysine side chains that can react with aldehydes and ketones, or these side chains can themselves be converted to aldehydes by lysyl oxidase. The reactivity of these groups not only has an important role in the maintenance of mechanical strength in collagen fibrils, but can also manifest pathologically in the cases of aging, diabetes (reactivity with a variety of sugars) and alcoholism (reactivity with acetaldehyde). The reactivity of reducing groups with collagen can be studied by neutron diffraction, since the crosslink formed in the adduction process is initially of a Schiff base or keto-imine nature. The nature of this crosslink allows it to be deuterated, and the position of this relatively heavy scattering atom can be used in a process of phase determination by multiple isomorphous replacement. This process was used to study the following: the position of natural crosslinks in collagen; the position of adducts in tendon from diabetic rats in vivo and the in vitro position of acetaidehyde adducts in tendon.

  2. Single-crystal neutron diffraction at the Australian Replacement Research Reactor

    International Nuclear Information System (INIS)

    Klooster, W.T.

    2001-01-01

    The purpose of the workshop was to: identify the future needs and opportunities for single-crystal neutron diffraction, and specify instrument requirements. important number of experiments. The conclusion of the workshop deliberation was that Australia has a diverse community of users of single-crystal neutron diffraction. A (quasi)-Laue image-plate diffractometer allows the fastest throughput by far, but would exclude an important number of experiments. Most of these could be covered by the additional possibility to locate the image-plate detector on a monochromatic beam. Therefore it was recommend both a white thermal beam and a monochromatic beam (λ= 1 to 2.4 Angstroms) for an image-plate detector. At little additional cost the existing 2TanA instrument could be located semi-permanently on the same monochromatic beam, thus offering three quite different types of single-crystal instruments. Small improvements could be made to the 2TanA instrument to cater for the remaining experiments not suited to an image-plate diffractometer: exchange of the Eulerian cradle for an automated tilt goniometer for extremely bulky sample environment (cryomagnets, large pressure cells), optional larger area detector, analyser crystal. It was recommended that an Instrument Advisory Team will be assembled, and will help in specifying, designing and commissioning the instrument

  3. Neutron-diffraction measurement of residual stresses in Al-Cu cold-cut welding

    Science.gov (United States)

    Fiori, F.; Marcantoni, M.

    Usually, when it is necessary to join different materials with a large difference in their melting points, welding should be avoided. To overcome this problem we designed and built a device to obtain cold-cut welding, which is able to strongly decrease oxidation problems of the surfaces to be welded. Thanks to this device it is possible to achieve good joining between different pairs of materials (Al-Ti, Cu-Al, Cu-Al alloys) without reaching the material melting point. The mechanical and microstructural characterisation of the joining and the validation of its quality were obtained using several experimental methods. In particular, in this work neutron-diffraction experiments for the evaluation of residual stresses in Cu-Al junctions are described, carried out at the G5.2 diffractometer of LLB, Saclay. Neutron-diffraction results are presented and related to other experimental tests such as microstructural characterisation (through optical and scanning electron microscopy) and mechanical characterisation (tensile-strength tests) of the welded interface.

  4. Diffraction des neutrons : principe, dispositifs expérimentaux et applications

    Science.gov (United States)

    Muller, C.

    2003-02-01

    La diffraction de neutrons, sur monocristal ou sur échantillon polycristallin (ou poudre), est une technique très largement utilisée, en science des matériaux comme en biologie, lorsque l'on souhaite déterminer la structure cristalline d'un composé ou d'une molécule. Toutefois, le degré de précision de la détermination structurale est très corrélé au choix de l'instrument utilisé. Il s'en suit que la question “comment choisir l'instrument le mieux adapté au composé et à la problématique ?" apparaît comme fondamentale. L'objectif de ce cours est de tenter de répondre à cette question en décrivant brièvement les caractéristiques instrumentales de différents diffractomètres, en exposant les avantages spécifiques des expériences de diffraction de neutrons et en donnant quelques exemples d'application.

  5. Neutron diffraction study of single crystalline ErCo10Mo2

    International Nuclear Information System (INIS)

    Janssen, Y.; De Boer, F.R.; Brueck, E.; Tegus, O.; Ma, L.; Buschow, K.H.J.; Reehuis, M.

    1999-01-01

    Complete text of publication follows. The ferrimagnetic intermetallic compound ErCo 10 Mo 2 (Tc = 600 K) crystallizes in the tetragonal ThMn 12 -type structure (space group 14/mmm). The Co and Mo atoms may share three crystallographic sites (8f, 8i and 8j). Earlier neutron powder diffraction experiments show that Mo has a strong preference for the 8i-site and that the magnetic ordering at low temperature is planar. Furthermore ErCo 10 Mo 2 has been reported to show one [2] or more [3] spin-reorientation transitions from planar to axial magnetic ordering. Recently we succeeded in growing a single-crystalline sample of ErCo 10 Mo 2 . Magnetic measurements in 1T show one spin-reorientation transition at about 135 K. Neutron diffraction experiments were performed to investigate a possible link between the magnetic properties and the site occupation by Mo. Our results show that our sample has the Mo atoms exclusively occupying half the 8i-sites. There is no evidence for a crystallographic superstructure. Furthermore, below 150 K some reflections strongly increase due to the growing Er magnetic moment. (author)

  6. Neutron-diffraction studies of the nuclear magnetic phase diagram of copper

    DEFF Research Database (Denmark)

    Annila, A.J.; Clausen, Kurt Nørgaard; Oja, A.S.

    1992-01-01

    We have studied the spontaneous antiferromagnetic (AF) order in the nuclear spin system of copper by use of neutron-diffraction experiments at nanokelvin temperatures. Copper is an ideal model system as a nearest-neighbor-dominated spin-3/2 fcc antiferromagnet. The phase diagram has been investig......We have studied the spontaneous antiferromagnetic (AF) order in the nuclear spin system of copper by use of neutron-diffraction experiments at nanokelvin temperatures. Copper is an ideal model system as a nearest-neighbor-dominated spin-3/2 fcc antiferromagnet. The phase diagram has been...... investigated by measuring the magnetic-field dependence of the (100) reflection, characteristic of a type-I AF structure, and of a Bragg peak at (0 2/3 2/3). The results suggest the presence of high-field (100) phases at 0.12 less-than-or-equal-to B less-than-or-equal-to B(c) almost-equal-to 0.26 mT, for B...... compared with results of earlier susceptibility measurements in order to identify the translational periods of the three previously found antiferromagnetic phases for B parallel-to [100]. Recent theoretical work has yielded results in agreement with our experimental data....

  7. The chemical reactivity and structure of collagen studied by neutron diffraction

    International Nuclear Information System (INIS)

    Wess, T.J.; Wess, L.; Miller, A.

    1994-01-01

    The chemical reactivity of collagen can be studied using neutron diffraction (a non-destructive technique), for certain reaction types. Collagen contains a number of lysine and hydroxylysine side chains that can react with aldehydes and ketones, or these side chains can themselves be converted to aldehydes by lysyl oxidase. The reactivity of these groups not only has an important role in the maintenance of mechanical strength in collagen fibrils, but can also manifest pathologically in the cases of aging, diabetes (reactivity with a variety of sugars) and alcoholism (reactivity with acetaldehyde). The reactivity of reducing groups with collagen can be studied by neutron diffraction, since the crosslink formed in the adduction process is initially of a Schiff base or keto-imine nature. The nature of this crosslink allows it to be deuterated, and the position of this relatively heavy scattering atom can be used in a process of phase determination by multiple isomorphous replacement. This process was used to study the following: the position of natural crosslinks in collagen; the position of adducts in tendon from diabetic rats in vivo and the in vitro position of acetaidehyde adducts in tendon

  8. Structure, magnetic properties, polarized neutron diffraction, and theoretical study of a copper(II) cubane.

    Science.gov (United States)

    Aronica, Christophe; Chumakov, Yurii; Jeanneau, Erwann; Luneau, Dominique; Neugebauer, Petr; Barra, Anne-Laure; Gillon, Béatrice; Goujon, Antoine; Cousson, Alain; Tercero, Javier; Ruiz, Eliseo

    2008-01-01

    The paper reports the synthesis, X-ray and neutron diffraction crystal structures, magnetic properties, high field-high frequency EPR (HF-EPR), spin density and theoretical description of the tetranuclear CuII complex [Cu4L4] with cubane-like structure (LH2=1,1,1-trifluoro-7-hydroxy-4-methyl-5-aza-hept-3-en-2-one). The simulation of the magnetic behavior gives a predominant ferromagnetic interaction J1 (+30.5 cm(-1)) and a weak antiferromagnetic interaction J2 (-5.5 cm(-1)), which correspond to short and long Cu-Cu distances, respectively, as evidence from the crystal structure [see formulate in text]. It is in agreement with DFT calculations and with the saturation magnetization value of an S=2 ground spin state. HF-EPR measurements at low temperatures (5 to 30 K) provide evidence for a negative axial zero-field splitting parameter D (-0.25+/-0.01 cm(-1)) plus a small rhombic term E (0.025+/-0.001 cm(-1), E/D = 0.1). The experimental spin distribution from polarized neutron diffraction is mainly located in the basal plane of the CuII ion with a distortion of yz-type for one CuII ion. Delocalization on the ligand (L) is observed but to a smaller extent than expected from DFT calculations.

  9. Determination of the Magnetic Structure of Complex anti-Perovskite Fluorides by Neutron Diffraction

    Science.gov (United States)

    Felder, Justin; Yeon, Jeongho; Zur Loye, Hans-Conrad

    An unusual family of anti-perovskite fluorides consisting of complex ions as the A, B, and X building units has been synthesized as single crystals. This family of anti-perovskites provides a unique framework to probe the magnetic properties of transition metals. Presented here is the Fe endmember of the family: [Cu(H2O)4]3[FeF6]2. The iron member exhibits complex magnetic behavior at low temperatures, which has been probed by magnetometry and neutron diffraction experiments. Presented here are the results from the anisotropic magnetometry study as well as the magnetic spin structure as determined by neutron diffraction experiments. The materials presented here represent an interesting class of perovskites that are as-yet unexplored. Given the wide range of properties possible in perovskites and related structures, it is reasonable to expect that further exploration of these materials will reveal many interesting attributes; both chemical and physical. United States Department of Energy, Office of Basic Energy Sciences, Division of Materials Sciences and Engineering, Award DE-SC0008664.

  10. In Situ X-ray Diffraction Studies of Cathode Materials in Lithium Batteries

    International Nuclear Information System (INIS)

    Yang, X. Q.; Sun, X.; McBreen, J.; Mukerjee, S.; Gao, Yuan; Yakovleva, M. V.; Xing, X. K.; Daroux, M. L.

    1998-01-01

    There is an increasing interest in lithiated transition metal oxides because of their use as cathodes in lithium batteries. LiCoO 2 , LiNiO 2 and LiMn 2 O 4 are the three most widely used and studied materials, At present, although it is relative expensive and toxic, LiCoO 2 is the material of choice in commercial lithium ion batteries because of its ease of manufacture, better thermal stability and cycle life. However, the potential use of lithium ion batteries with larger capacity for power tools and electric vehicles in the future will demand new cathode materials with higher energy density, lower cost and better thermal stability. LiNiO 2 is isostructural with LiCoO 2 . It offers lower cost and high energy density than LiCoO 2 . However, it has much poorer thermal stability than LiCoO 2 , in the charged (delithiated) state. Co, Al, and other elements have been used to partially replace Ni in LiNiO 2 system in order to increase the thermal stability. LiMn 2 O 4 has the highest thermal stability and lowest cost and toxicity. However, the low energy density and poor cycle life at elevated temperature are the major obstacles for this material. In order to develop safer, cheaper, and better performance cathode materials, the in-depth understanding of the relationships between the thermal stability and structure, performance and structure are very important. The performance here includes energy density and cycle life of the cathode materials. X-ray diffraction (XRD) is one of the most powerful tools to study these relationships. The pioneer ex situ XRD work on cathode materials for lithium batteries was done by Ohzuku. His XRD studies on LiMn 2 O 4 , LiCoO 2 , LiNiO 2 , LiNi 0.5 Co 0.5 O 2 , and LiAl x Ni 1-x O 2 cathodes at different states of charge have provided important guidelines for the development of these new materials. However, the kinetic nature of the battery system definitely requires an in situ XRD technique to study the detail structural changes of the

  11. In Situ X-ray Diffraction Study of Cesium Exchange in Synthetic Umbite

    International Nuclear Information System (INIS)

    Fewox, C.; Clearfield, A.; Celestian, A.

    2011-01-01

    The exchange of Cs + into H 1.22 K 0.84 ZrSi 3 O 9 · 2.16H 2 O (umbite-(HK)) was followed in situ using time-resolved X-ray diffraction at the National Synchrotron Light Source. The umbite framework (space group P2 1 /c with cell dimensions of a = 7.2814(3) (angstrom), b = 10.4201(4) (angstrom), c = 13.4529(7) (angstrom), and β = 90.53(1) o ) consists of wollastonite-like silicate chains linked by isolated zirconia octahedra. Within umbite-(HK) there are two unique ion exchange sites in the tunnels running parallel to the a-axis. Exchange Site 1 is marked by 8 member-ring (MR) windows in the bc-plane and contains K + cations. Exchange Site 2 is marked by a larger 8-MR channel parallel to [100], and contains H 2 O molecules. The occupancy of the Cs + cations through these channels was modeled by Rietveld structure refinements of the diffraction data and demonstrated that there is a two-step exchange process. The incoming Cs + ions populated the larger 8-MR channel (Exchange Site 2) first and then migrated into the smaller 8-MR channel. During the exchange process a structural change occurs, transforming the exchanger from monoclinic P2 1 /c to orthorhombic P2 1 2 1 2 1 . This structural change occurs when Cs + occupancy in the small cavity becomes greater than 0.50. The final in situ ion exchange diffraction pattern was refined to yield umbite-(CsK) with the molecular formula H 0.18 K 0.45 Cs 1.37 ZrSi 3 O 9 · 0.98H 2 O and possessing an orthorhombic unit cell with dimensions a = 10.6668(8) (angstrom), b = 13.5821(11) (angstrom), c = 7.3946(6) (angstrom). Solid state 133 Cs MAS NMR showed there is only a slight difference between the two cavities electronically. Valence bond sums for the completely occupied Exchange Site 1 demonstrate that Cs-O bonds of up to 3.8 (angstrom) contribute to the coordination of the Cs + cation.

  12. Real time neutron diffraction and NMR of the Empress II glass-ceramic system.

    Science.gov (United States)

    O'Donnell, M D; Hill, R G; Karpukhina, N; Law, R V

    2011-10-01

    This study reports real time neutron diffraction on the Empress II glass-ceramic system. The commercial glass-ceramics was characterized by real time neutron diffraction, ³¹P and ²⁹Si solid-state MAS-NMR, DSC and XRD. On heating, the as-received glass ceramic contained lithium disilicate (Li₂Si₂O₅), which melted with increasing temperature. This was revealed by neutron diffraction which showed the Bragg peaks for this phase had disappeared by 958°C in agreement with thermal analysis. On cooling lithium metasilicate (Li₂SiO₃) started to form at around 916°C and a minor phase of cristobalite at around 852°C. The unit cell volume of both Li-silicate phases increased linearly with temperature at a rate of +17×10⁻³ ų.°C⁻¹. Room temperature powder X-ray diffraction (XRD) of the material after cooling confirms presence of the lithium metasilicate and cristobalite as the main phases and shows, in addition, small amount of lithium disilicate and orthophosphate. ³¹P MAS-NMR reveals presence of the lithiorthophosphate (Li₃PO₄) before and after heat treatment. The melting of lithium disilicate on heating and crystallisation of lithium metasilicate on cooling agree with endothermic and exotermic features respectively observed by DSC. ²⁹Si MAS-NMR shows presence of lithium disilicate phase in the as-received glass-ceramic, though not in the major proportion, and lithium metasilicate in the material after heat treatment. Both phases have significantly long T₁ relaxation time, especially the lithium metasilicate, therefore, a quantitative analysis of the ²⁹Si MAS-NMR spectra was not attempted. Significance. The findings of the present work demonstrate importance of the commercially designed processing parameters in order to preserve desired characteristics of the material. Processing the Empress II at a rate slower than recommended 60°C min⁻¹ or long isothermal hold at the maximal processing temperature 920°C can cause

  13. Determination of crystalline texture in aluminium - uranium alloys by neutron diffraction

    International Nuclear Information System (INIS)

    Azevedo, A.M.V. de.

    1978-01-01

    Textures of hot-rolled aluminum-uranium alloys and of aluminum were determined by neutron diffraction. Sheets of alloys containing 8.0, 21.5 and 23.7 wt pct U, as well as pure aluminum, were obtained in a stepped rolling process, 15% reduction each step, 75% total reduction. During the rolling the temperature was 600 0 C. Alloys with low uranium contents are two phase systems in which an intermetallic compound UAl 4 , orthorhombic, is dispersed in a pure aluminum matrix. The addition of a few percent of Si in such alloys leads to the formation of UAl 3 , simple cubic, instead of UAl 4 . The Al -- 23.7 wt pct U alloy was prepared with 2,2 wt pct of Si. The results indicate that the texture of the matrix is more dependent on the uranium concentration than on the texture of the intermetallic phases. An improvement in the technique applied to texture measurements by using a sample fully bathed in the neutron beam is also presented. The method takes advantage of the low neutron absorption of the studied materials as well as of the neglibible variation in the multiple scattering which occurs in a conveniently shaped sample having a weakly developed texture. (Author) [pt

  14. The structure of liquid water by polarized neutron diffraction and reverse Monte Carlo modelling.

    Science.gov (United States)

    Temleitner, László; Pusztai, László; Schweika, Werner

    2007-08-22

    The coherent static structure factor of water has been investigated by polarized neutron diffraction. Polarization analysis allows us to separate the huge incoherent scattering background from hydrogen and to obtain high quality data of the coherent scattering from four different mixtures of liquid H(2)O and D(2)O. The information obtained by the variation of the scattering contrast confines the configurational space of water and is used by the reverse Monte Carlo technique to model the total structure factors. Structural characteristics have been calculated directly from the resulting sets of particle coordinates. Consistency with existing partial pair correlation functions, derived without the application of polarized neutrons, was checked by incorporating them into our reverse Monte Carlo calculations. We also performed Monte Carlo simulations of a hard sphere system, which provides an accurate estimate of the information content of the measured data. It is shown that the present combination of polarized neutron scattering and reverse Monte Carlo structural modelling is a promising approach towards a detailed understanding of the microscopic structure of water.

  15. Application of neutron diffraction in characterization of texture evolution during high-temperature creep in magnesium alloys

    International Nuclear Information System (INIS)

    Sediako, A.; Shook, S.; Vogel, S.; Sediako, D.

    2010-01-01

    A good combination of room-temperature and elevated temperature strength and ductility, good salt-spray corrosion resistance and excellent diecastability are frequently among the main considerations in development of a new magnesium alloy for automotive industry. Unfortunately, there has been much lesser effort in development of wrought-stock alloys for high temperature applications. Extrudability and high temperature performance of wrought material become important factors in an effort to develop new wrought alloys and processing technologies. This paper shows some results received in creep testing and studies of in-creep texture evolution for several wrought magnesium alloys developed for use in elevated- temperature applications. Along with others 'traditional' characterization techniques of metals' performance in high- temperature creep, neutron diffraction was employed in this study to analyze evolution of crystallographic texture during creep deformation. The paper compares two methods of texture analysis in neutron diffraction studies: based on monochromatic (reactor-source) beam and white neutron beam (time-of-flight method, synchrotron). The time-of-flight (TOF) spectrometer illuminates the sample with a non-filtered beam of neutrons and captures the readings with an encircled detector array. This provides a very fast and detailed picture of the crystallographic texture for the bulk of the sample. As the white beam retains all neutron wavelengths, it takes much less time to collect statistically-valid dataset for the diffraction pattern. On the other hand, the monochromatic beam setup includes a monochromatic crystal that filters out a specific wavelength. The diffracted beam is then captured by a much simpler neutron detector. This setup is more flexible, allowing for choosing various wavelengths (depending on the sample material) but obviously requiring more time for statistically viable data collection. These studies were performed using E3 neutron

  16. Neutron diffraction instruments at the BR2 reactor and their use in the study of crystal and magnetic structures

    International Nuclear Information System (INIS)

    Legrand, E.

    1977-01-01

    The study of structural properties of condensed matted is frequently performed by means of methods based on X-ray, electron or neutron scattering. In many particular cases, the latter technique offers definite advantages which are mainly based on the following characteristics of neutron-matter interaction: The large penetration depth for neutrons in matter (with the exception of a few elements), which allow the study of large samples and the use of wavelengths from 0.5 to 5A, and even to 10 A; the absence of an atomic form factor; the irregular dependence of the scattering length for the different elements as a function of their atomic number; the large cross section for magnetic scattering; the energy of thermal neutrons which allows the direct measuremtment of the enrgy exchange between the neutrons and the scatterer. Three of the four neutron diffraction instruments for solid state research, installed at the BR2 reactor, are described in detail. (author)

  17. A comparison of texture results obtained using precession electron diffraction and neutron diffraction methods at diminishing length scales in ordered bimetallic nanolamellar composites

    International Nuclear Information System (INIS)

    Carpenter, J.S.; Liu, X.; Darbal, A.; Nuhfer, N.T.; McCabe, R.J.; Vogel, S.C.; LeDonne, J.E.; Rollett, A.D.; Barmak, K.; Beyerlein, I.J.; Mara, N.A.

    2012-01-01

    Precession electron diffraction (PED) is used to acquire orientation information in Cu–Nb nanolamellar composites fabricated by accumulative roll bonding (ARB). The resulting maps quantify the grain size, shape, orientation distributions and interface planes in the vicinity of nanometer-thick deformation twins. The PED-based texture results compare favorably with bulk textures provided by neutron diffraction measurements, indicating uniformity in the ARB Cu–Nb texture. Additionally, {1 1 2} Cu ||{1 1 2} Nb interfaces are present, suggesting that ARB techniques can lead to stable interfaces with a special crystallography.

  18. Neutron diffraction studies of a double-crystal ( plus n,-m) setting containing a fully asymmetric diffraction geometry (FAD) of a bent perfect crystal (BPC)

    Czech Academy of Sciences Publication Activity Database

    Mikula, Pavol; Vrána, Miroslav; Šaroun, Jan; Em, V.

    2017-01-01

    Roč. 32, Supl-1 (2017), s. 13-18 ISSN 0885-7156 R&D Projects: GA ČR GC16-08803J; GA MŠk LM2015048 Institutional support: RVO:61389005 Keywords : neutron diffraction * monochromator * bent perfect crystal Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 0.674, year: 2016

  19. In situ synchrotron diffraction of lead-zirconate-titanate at its morphotropic phase boundary

    International Nuclear Information System (INIS)

    Schoenau, K.A.

    2008-01-01

    Ferroelectric lead zirconate titanate ceramics (PZT,Pb(Zr x Ti 1-x )O 3 ) find in industry intensifiedly applications as piezoactors. Their largest macroscopic strain under electric field they show in the region of the morphotropic phase boundary (MPB), the transition region between the Ti rich tetragonal and the Zr rich structure. The structure of PZT at the MPB was controversially discussed since the detection of a monoclinic intermediate phase by Noheda et al. [Appl. Phys. Lett.,74(14), 2059(1999)], whereby into the considerations the domain structure of the material not entered, which however is essentially responsible for the reaction under electric field. In order to understand the domain structure of PZT under electric field and to study possible causes for the fatigue behaviour of the material under bipolar cycling a bridge must be built between macroscopic and local structure. For this at the measuring place B2 of the Hasylab, Hamburg, synchrotron X-ray powder diffractometry was in situ performed under different sample environments in transmission geometry, which was correlated with transmission-electron-microscopical studies and electron spin resonance. Samples with compositions over the whole MPB were beside temperature-dependent measurements measured at room temperature in high resolution and under applied electric field. Furthermore for studies under electric field at elevated temperatures a special E-field furnace was constructed. It could be shown the large piezoelectric reaction of PZT at its MPB is strongly correlated with a diminishment of the domain structure, which simulates in X-ray diffraction a lower symmetric phase. The stability range of the nanodomains with temperature and electric field reflects in the switching behaviour of the matter and by the detection of a relaxor behavior of the nanodomain structure for the first time a direct comparison with relaxoceramics is possible. The varying stress conditions within the sample influence

  20. Application of neutron-induced gamma ray spectrometry for in situ assessment of coal quality

    International Nuclear Information System (INIS)

    Chrusciel, E.; Leutsoa Makhabane, J.

    1990-01-01

    The physical principles of the spectrometric neutron capture borehole logging method and spectrometric neutron activation borehole logging method are presented. Nuclear parameters of major elemental constituents of coal are given. Statistical multiple correlation results of coal core samples assessment are presented for coal quality parameters. The results of in situ spectrometric measurements in a coal field are also given. 7 figs., 11 tabs., 15 refs. (author)

  1. X-Ray Diffraction for In-Situ Mineralogical Analysis of Planetesimals.

    Science.gov (United States)

    Sarrazin, P.; Blake, D. F.; Dera, P.; Downs, R. T.; Taylor, J.

    2017-12-01

    X-ray diffraction (XRD) is a general purpose technique for definitive, quantitative mineralogical analysis. When combined with XRF data for sample chemistry, XRD analyses yield as complete a characterization as is possible by any spacecraft-capable techniques. The MSL CheMin instrument, the first XRD instrument flown in space, has been used to establish the quantitative mineralogy of the Mars global soil, to discover the first habitable environment on another planet, and to provide the first in-situ evidence of silicic volcanism on Mars. CheMin is now used to characterize the depositional and diagenetic environments associated with the mudstone sediments of lower strata of Mt. Sharp. Conventional powder XRD requires samples comprised of small grains presented in random orientations. In CheMin, sample cells are vibrated to cause loose powder to flow within the cell, driven by granular convection, which relaxes the requirement for fine grained samples. Nevertheless, CheMin still requires mechanisms to collect, crush, sieve and deliver samples before analysis. XTRA (Extraterrestrial Regolith Analyzer) is an evolution of CheMin intended to analyze fines in as-delivered surface regolith, without sample preparation. Fine-grained regolith coats the surfaces of most airless bodies in the solar system, and because this fraction is typically comminuted from the rocky regolith, it can often be used as a proxy for the surface as a whole. HXRD (Hybrid-XRD) is concept under development to analyze rocks or soils without sample preparation. Like in CheMin, the diffracted signal is collected with direct illumination CCD's. If the material is sufficiently fine-grained, a powder XRD pattern of the characteristic X-ray tube emission is obtained, similar to CheMin or XTRA. With coarse grained crystals, the white bremsstrahlung radiation of the tube is diffracted into Laue patterns. Unlike typical Laue applications, HXRD uses the CCD's capability to distinguish energy and analyze the

  2. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    Energy Technology Data Exchange (ETDEWEB)

    Cui, J., E-mail: jun.cui@pnnl.gov; Choi, J. P.; Li, G.; Polikarpov, E.; Darsell, J. [Energy and Environment Directorate, Pacific Northwest National Laboratory, Richland, Washington 99354 (United States); Kramer, M. J.; Zarkevich, N. A.; Wang, L. L.; Johnson, D. D. [Materials Sciences and Engineering Division, Ames Laboratory, Ames, Iowa 50011 (United States); Marinescu, M. [Electron Energy Corporation, Landisville, Pennsylvania 17538 (United States); Huang, Q. Z.; Wu, H. [NIST Center for Neutron Research, National Institute of Standards and Technology, Gaithersburg, Maryland 20899-6102 (United States); Vuong, N. V.; Liu, J. P. [Department of Physics, University of Texas at Arlington, Arlington, Texas 76019 (United States)

    2014-05-07

    MnBi attracts great attention in recent years for its great potential as permanent magnet materials. MnBi phase is difficult to obtain because of the rather drastic peritectic reaction between Mn and Bi. In this paper, we report our effort on synthesizing high purity MnBi compound using conventional powder metallurgical approaches. Neutron diffraction was carried out to investigate the crystal and nuclear structure of the obtained powder. The result shows that the purity of the obtained powder is about 91 wt. % at 300 K, and the magnetic moment of the Mn atom in MnBi lattice is 4.424 and 4.013 μ{sub B} at 50 K and 300 K, respectively.

  3. Neutron diffraction study of dense-Kondo compound CeNi2Al5

    International Nuclear Information System (INIS)

    Munoz, A.; Givord, F.; Boucherie, J.X.; Flouquet, J.; Isikawa, Y.; Mizushima, T.; Sakurai, J.; Mori, K.; Oliveira, I.S.

    1993-01-01

    Intermetallic CeNi 2 Al 5 is a dense-Kondo compound with a magnetic transition temperature at 2.6 K. We have carried out a neutron diffraction measurement to study a magnetic structure of CeNi 2 Al 5 using a powder sample and a single crystalline sample. It is found that the magnetic structure is an incommensurate sinusoidal one with a propagation vector k = (0.5, 0.405, 0.083) and that the amplitude of magnetic moment is 1.54 μ Β and the direction of magnetic moment is declined 8 deg. from the b-axis toward the a-axis. (authors). 3 refs., 2 figs

  4. Residual stresses in a composite steel tube measured by neutron diffraction

    International Nuclear Information System (INIS)

    Taran, Yu.V.; Balagurov, A.M.; Zlokazov, V.B.; Schreiber, J.; Stuhr, U.; Kockelmann, H.

    2006-01-01

    The triaxial residual stresses in a composite tube from an austenitic stainless steel with a welded ferritic steel cladding were measured by the time-of-flight neutron diffraction method on the POLDI instrument at the PSI SINQ facility. The POLDI results are compared to the results obtained by the destructive turning out method and theoretical predictions of calculations by the finite element method. Only for the tangential component of the stress tensor the semiquantitative agreement of all used methods was observed. There is a clear discrepancy between the results of the different methods in the axial component. For the radial component all methods reveal quite small stresses, however, with some distinct differences in their distributions

  5. Neutron diffraction studies on GdB{sub 6} and TbB{sub 6} powders

    Energy Technology Data Exchange (ETDEWEB)

    Luca, S.E.; Amara, M.; Galera, R.M.; Givord, F.; Granovsky, S.; Isnard, O.; Beneu, B

    2004-07-15

    We report here the first powder neutron diffraction study of GdB{sub 6} and TbB{sub 6}. GdB{sub 6} and TbB{sub 6} order antiferromagnetically at 15 and 21 K, respectively. In both compounds the transition at T{sub N} is of the first order. Moreover GdB{sub 6} presents a second spontaneous magnetic transition at T{sup *}=8 K. The present study shows that, in both compounds, the magnetic propagation vectors belong to the <((1)/(4)) ((1)/(4)) ((1)/(2))> star and that the direction of the magnetic moment is perpendicular to the ((1)/(2)) component of the wave-vector in GdB{sub 6}, while in TbB{sub 6} the moment is parallel to it. The deduced low-temperature values of the magnetic moments agree with those of the respective rare-earth trivalent ions.

  6. Neutron diffraction studies on GdB6 and TbB6 powders

    International Nuclear Information System (INIS)

    Luca, S.E.; Amara, M.; Galera, R.M.; Givord, F.; Granovsky, S.; Isnard, O.; Beneu, B.

    2004-01-01

    We report here the first powder neutron diffraction study of GdB 6 and TbB 6 . GdB 6 and TbB 6 order antiferromagnetically at 15 and 21 K, respectively. In both compounds the transition at T N is of the first order. Moreover GdB 6 presents a second spontaneous magnetic transition at T * =8 K. The present study shows that, in both compounds, the magnetic propagation vectors belong to the star and that the direction of the magnetic moment is perpendicular to the ((1)/(2)) component of the wave-vector in GdB 6 , while in TbB 6 the moment is parallel to it. The deduced low-temperature values of the magnetic moments agree with those of the respective rare-earth trivalent ions

  7. Phase transitions in Rb2UBr6 observed by neutron powder diffraction

    International Nuclear Information System (INIS)

    Maletka, K.; Ressouche, E.; Tellgren, R.; Delaplane, R.; Szczepaniak, W.; Rycerz, L.; Zablocka-Malecka, M.

    1997-01-01

    The behaviour of the Rb 2 UBr 6 ionic conductor is studied as a function of the temperature by neutron powder diffraction. The low- room and high temperature structures have been determined. At low temperature range 4.2-80 K the compound crystallizes in a monoclinic unit cell with P2 1 /c space group. Among 80 and 853 K the compound crystallizes in a tetragonal unit cell with space group P4/mnc. At 300 K the lattice constants are; a = b 7,745(1), c = 11.064(1) A. At the temperature range 853-960 K is observed the trigonal phase with P-3m1 space group. Above the phase transitions occurring at 960 K the compound crystallizes in the cubic unit cell with Fm3m space group. (author)

  8. Neutron diffraction measurements for the determination of residual stresses in MMC tensile and fatigue specimens

    DEFF Research Database (Denmark)

    Fiori, F.; Girardin, E.; Giuliani, A.

    2000-01-01

    have been performed at RISO (Roskilde, DK) and HMI-BENSC (Berlin, D), for the determination of residual stress in AA2124 + 17% SiCp and AA359 + 20% SiCp specimens, submitted to tensile and fatigue tests. For each of the investigated samples, the macrostress has been separated from the elastic......, residual stresses are present in both the matrix and the particles microstructure, prior to any macroscopic loading. They vary with the temperature and with the type and level of loading imposed to the material, having a strong influence on the mechanical behaviour of MMCs. Neutron diffraction measurements...... and thermal mismatch microstresses. The results show that, in general, the main contribution to the stress state of both matrix and reinforcement is given by the thermal microstresses, already existing due to heat treatment prior to mechanical tests. (C) 2000 Elsevier Science B.V. All rights reserved....

  9. A re-analysis of neutron diffraction data from UO2

    International Nuclear Information System (INIS)

    Cooper, M.J.; Sakata, M.

    1979-04-01

    The results of a re-analysis of recent single crystal and powder neutron diffraction data from UO2 are presented and discussed. It is shown that apparent inconsistencies in the results of previous analyses of these data arose from differences between the values assumed for some of the parameters and that the various sets of data are in fact extremely consistent. These data also provide a more accurate value for the ratio of the scattering amplitudes, i.e. bU/bO = 1.451(2), which gives a value for bU = 0.842(2) x 10(-12) cm on the assumption of a value for b0 = 0.5805(11) x 10(-12) cm. The temperature factors for the atoms at room temperature are determined to be BU = 0.23(1)Angstrom and BO = 0.44(1)Angstrom(2). (author)

  10. Neutron-diffraction measurement of the evolution of strain for non-uniform plastic deformation

    CERN Document Server

    Rogge, R B; Boyce, D

    2002-01-01

    Neutrons are particularly adept for the validation of modeling predictions of stress and strain. In recent years, there has been a significant effort to model the evolution of both the macroscopic stresses and the intergranular stress during plastic deformation. These have had broad implications with regard to understanding the evolution of residual stress and to diffraction-based measurements of strain. Generally the modeling and associated measurements have been performed for simple uniaxial tension, leaving questions with regard to plastic deformation under multi-axial stress and non-uniform stress. Extensive measurements of the strain profile across a plastic hinge for each of a series of loading and unloading cycles to progressively higher degrees of plastic deformation are presented. These measurements are used to assess multiple-length-scale finite-element modeling (FEM) of the plastic hinge, in which the elements will range in size from single crystallites (as used in successful simulations of uniaxia...

  11. Refinement of the crystal structure of malachite, Cu2(OH)2CO3, by neutron diffraction

    International Nuclear Information System (INIS)

    Zigan, F.; Joswig, W.; Schuster, H.D.; Mason, S.A.

    1977-01-01

    The crystal structure of malachite is refined (R = 0,021) with the intensity values of 635 independent neutron reflexions from a single crystal, rather free from absorption and extinction. Concerning the structural geometry, no essential deviations occur from the known results of x-ray diffraction. The thermal elongations are generally largest about the normal to the (201) layers, between which the bonding is relatively weak. In both of the (medium, bent) OH...O hydrogen bonds, the anisotropic thermal parameters, converted according to the riding model, are - with certain restrictions - in agreement with the measured infrared spectrum as well as with frequencies and directions of the proton vibration calculated from the bonding geometry on the basis of a theoretical model. (orig.) [de

  12. Residual stress measurements via neutron diffraction of additive manufactured stainless steel 17-4 PH.

    Science.gov (United States)

    Masoomi, Mohammad; Shamsaei, Nima; Winholtz, Robert A; Milner, Justin L; Gnäupel-Herold, Thomas; Elwany, Alaa; Mahmoudi, Mohamad; Thompson, Scott M

    2017-08-01

    Neutron diffraction was employed to measure internal residual stresses at various locations along stainless steel (SS) 17-4 PH specimens additively manufactured via laser-powder bed fusion (L-PBF). Of these specimens, two were rods (diameter=8 mm, length=80 mm) built vertically upward and one a parallelepiped (8×80×9 mm 3 ) built with its longest edge parallel to ground. One rod and the parallelepiped were left in their as-built condition, while the other rod was heat treated. Data presented provide insight into the microstructural characteristics of typical L-PBF SS 17-4 PH specimens and their dependence on build orientation and post-processing procedures such as heat treatment. Data have been deposited in the Data in Brief Dataverse repository (doi:10.7910/DVN/T41S3V).

  13. Neutron diffraction study of Fe-substituted YBa2Cu3O7

    International Nuclear Information System (INIS)

    Balagurov, A.M.; Mironova, G.M.; Pajaczkowska, A.; Piechota, J.; Shimchak, Kh.

    1989-01-01

    Neutron diffraction spectra of YBa 2 (Cu 1-x Fe x )O 7-δ (0 2 planes were determined. It is significant that the doped iron atoms occupy both of the copper site. The substitution of Fe for Cu in (2q) site is proportional to the concentration of iron in the sample. For small x there are a considerable amount of vacancies (10%) in the Cu1 site, which disappear quickly if x increases. Therefore, a joint effect of Cu substitution and the filling in vacancies by Fe occures for the Cu1 site. The amount of oxygen in samples increases with x up to 7.06 for x=0.12. Any visible effect of location of Fe at the Ba site is absent, but we can not exclude it completely. 20 refs.; 4 figs.; 1 tab

  14. Neutron diffraction analysis of HRh[P(C6H5)3]4

    International Nuclear Information System (INIS)

    Bau, R.; Stevens, R.C.; McLean, M.; Koetzle, T.F.

    1987-01-01

    We have collected neutron diffraction data on a large single crystal of the title compound. The most surprising result is an extremely short Rh-H distance of 1.31(8) A, presumably caused by steric interactions involving the bulky triphenyl phosphine ligands. Crystallographic details: HRh[P(C 6 H 5 ) 3 ] 4 . 1 / 2 C 6 H 6 crystallizes in the space group Pa3, with a = b = c = 22.776(3) A, Z = 8. Data were collected at the Brookhaven High Flux Beam reactor at a temperature of -23 0 C, λ = 1.15882(7) A -1 . Least-squares refinement (in which the phenyl rings were treated as rigid groups) resulted in an R factor [based on data with f > 4σ(F)] of 0.12 for 914 reflections and 95 parameters. 10 refs

  15. Heat treatment of bovine bone preceding spatially resolved texture investigation by neutron diffraction

    International Nuclear Information System (INIS)

    Benmarouane, Abdelilah; Hansen, Thomas; Lodini, Alain

    2004-01-01

    Bone is a composite material of collagen and porous hydroxyapatite crystallites, aligned parallel to each other, with the c-axis parallel to the long axis of the fibre. Its texture and crystallinity has been investigated by means of neutron diffraction, using the high intensity 2-axis diffractometer D20 at ILL in particular. We show spatially resolved pole figures on a composite sample of two bone pieces of different preferred orientation. We have selected the (1 1 1) reflection, which is nearly not affected by texture to characterise the crystallinity index, and (0 0 2) to show the texture because the c-axes of hydroxyapatite crystallites is directed along the axis of the bone

  16. Different Conditions of Formation Experienced by Iron Meteorites as Suggested by Neutron Diffraction Investigation

    Directory of Open Access Journals (Sweden)

    Francesco Grazzi

    2018-01-01

    Full Text Available In this communication, we report the results of a preliminary neutron diffraction investigation of iron meteorites. These planetary materials are mainly constituted by metallic iron with variable nickel contents, and, owing to their peculiar genesis, are considered to offer the best constrains on the early stages of planetary accretion. Nine different iron meteorites, representative of different chemical and structural groups, thought to have been formed in very different pressure and temperature conditions, were investigated, evidencing variances in crystallites size, texturing, and residual strain. The variability of these parameters and their relationship, were discussed in respect to possible diverse range of petrological conditions, mainly pressure and cooling rate, experienced by these materials during the crystallization stage and/or as consequence of post accretion events.

  17. Experimental determination of residual stress by neutron diffraction in a boiling water reactor core shroud

    International Nuclear Information System (INIS)

    Payzant, A.; Spooner, S.; Zhu, Xiaojing; Hubbard, C.R.

    1996-01-01

    Residual strains in a 51 mm (2-inch) thick 304L stainless steel plate have been measured by neutron diffraction and interpreted in terms of residual stress. The plate, measuring (300 mm) in area, was removed from a 6m (20-ft.) diameter unirradiated boiling water reactor core shroud, and included a multiple-pass horizontal weld which joined two of the cylindrical shells which comprise the core shroud. Residual stress mapping was undertaken in the heat affected zone, concentrating on the outside half of the plate thickness. Variations in residual stresses with location appeared consistent with trends expected from finite element calculations, considering that a large fraction of the residual hoop stress was released upon removal of the plate from the core shroud cylinder

  18. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    Energy Technology Data Exchange (ETDEWEB)

    Cui, J; Choi, JP; Li, G; Polikarpov, E; Darsell, J; Kramer, MJ; Zarkevich, NA; Wang, LL; Johnson, DD; Marinescu, M; Huang, QZ; Wu, H; Vuong, NV; Liu, JP

    2014-05-07

    MnBi attracts great attention in recent years for its great potential as permanent magnet materials. MnBi phase is difficult to obtain because of the rather drastic peritectic reaction between Mn and Bi. In this paper, we report our effort on synthesizing high purity MnBi compound using conventional powder metallurgical approaches. Neutron diffraction was carried out to investigate the crystal and nuclear structure of the obtained powder. The result shows that the purity of the obtained powder is about 91 wt. % at 300 K, and the magnetic moment of the Mn atom in MnBi lattice is 4.424 and 4.013 mu(B) at 50 K and 300 K, respectively. (C) 2014 AIP Publishing LLC.

  19. Neutron diffraction and thermal studies of amorphous CS2 realised by low-temperature vapour deposition

    International Nuclear Information System (INIS)

    Yamamuro, O.; Matsuo, T.; Onoda-Yamamuro, N.; Takeda, K.; Munemura, H.; Tanaka, S.; Misawa, M.

    2003-01-01

    We have succeeded in preparing amorphous carbon disulphide (CS 2 ) by depositing its vapour on a cold substrate at 10 K. Complete formation of the amorphous state has been confirmed by neutron diffraction and differential thermal analysis (DTA). The amorphous sample crystallized at ca. 70 K, which is lower than the hypothetical glass transition temperature (92 K) estimated from the DTA data of the (CS 2 ) x (S 2 Cl 2 ) 1-x binary mixture. CS 2 , a symmetric linear tri-atomic molecule, is the simplest of the amorphized molecular substances whose structural and thermal information has been reported so far. Comparison of the static structure factors S(Q) has shown that the orientational correlation of CS 2 molecules may be much stronger in the amorphous state than in the liquid state at higher temperature. (authors)

  20. Structure analysis of K3H(SO4)2 by neutron powder diffraction

    International Nuclear Information System (INIS)

    Murakami, Satoshi; Kuroiwa, Yoshihiro; Noda, Yukio; Nakai, Yusuke; Kamiyama, Takashi; Asano, Hajime.

    1993-01-01

    Neutron powder diffraction experiments of K 3 H(SO 4 ) 2 were carried out at KENS-HRP station in order to obtain the positional parameters of hydrogen nuclei. The data was taken at six different temperatures from room temperature to 20K. Even though K 3 H(SO 4 ) 2 contained a hydrogen atom, the structural analysis was successfully performed by using a program RIETAN. Concerning the hydrogen position, four different models give almost the same R-factor so that the state of the hydrogen nucleus is not uniquely determined. The result based on the assumption that a hydrogen nucleus occupies two sites shows that the distance of split hydrogen nuclei is shorter than the distance of hydrogen electron clouds. This result suggests that a large polarizability exists in a hydrogen atom. (author)

  1. Neutron diffraction stress determination in W-laminates for structural divertor applications

    Directory of Open Access Journals (Sweden)

    R. Coppola

    2015-07-01

    Full Text Available Neutron diffraction measurements have been carried out to develop a non-destructive experimental tool for characterizing the crystallographic structure and the internal stress field in W foil laminates for structural divertor applications in future fusion reactors. The model sample selected for this study had been prepared by brazing, at 1085 °C, 13 W foils with 12 Cu foils. A complete strain distribution measurement through the brazed multilayered specimen and determination of the corresponding stresses has been obtained, assuming zero stress in the through-thickness direction. The average stress determined from the technique across the specimen (over both ‘phases’ of W and Cu is close to zero at −17 ± 32 MPa, in accordance with the expectations.

  2. Residual stress measurements via neutron diffraction of additive manufactured stainless steel 17-4 PH

    Directory of Open Access Journals (Sweden)

    Mohammad Masoomi

    2017-08-01

    Full Text Available Neutron diffraction was employed to measure internal residual stresses at various locations along stainless steel (SS 17-4 PH specimens additively manufactured via laser-powder bed fusion (L-PBF. Of these specimens, two were rods (diameter=8 mm, length=80 mm built vertically upward and one a parallelepiped (8×80×9 mm3 built with its longest edge parallel to ground. One rod and the parallelepiped were left in their as-built condition, while the other rod was heat treated. Data presented provide insight into the microstructural characteristics of typical L-PBF SS 17-4 PH specimens and their dependence on build orientation and post-processing procedures such as heat treatment. Data have been deposited in the Data in Brief Dataverse repository (doi:10.7910/DVN/T41S3V.

  3. Temperature-induced itinerant-electron metamagnetism in ErCo3 studied by neutron diffraction

    International Nuclear Information System (INIS)

    Gratz, E.; Markosyan, A.S.; Gaidukova, I.Yu.; Rodimin, V.E.; Paul-Boncour, V.; Hoser, A.; Stuesser, N.

    2002-01-01

    Powder neutron diffraction studies in the temperature range from 2 K to 450 K of the ferrimagnetic ErCo 3 compound (T C =401 K) revealed an increase of the unit-cell volume at 100 K (T m ) when cooling down (ΔV/V∼4 x 10 -3 ). This is referred to as a temperature-induced change in the Co sublattice magnetization from a low-magnetic state (T>T m ) to a high-magnetic state (T m ). From the temperature variation of the sublattice magnetization (ErI (3a sites), ErII (6c), CoI (3b), CoII (6c) and CoIII (18h)) it was found that the Co moments at the 6c and 18h sites change near 100 K, giving rise to the volume anomaly at T m . A qualitative discussion of the mechanism behind this phenomenon is given. (orig.)

  4. Type I and type II residual stress in iron meteorites determined by neutron diffraction measurements

    Science.gov (United States)

    Caporali, Stefano; Pratesi, Giovanni; Kabra, Saurabh; Grazzi, Francesco

    2018-04-01

    In this work we present a preliminary investigation by means of neutron diffraction experiment to determine the residual stress state in three different iron meteorites (Chinga, Sikhote Alin and Nantan). Because of the very peculiar microstructural characteristic of this class of samples, all the systematic effects related to the measuring procedure - such as crystallite size and composition - were taken into account and a clear differentiation in the statistical distribution of residual stress in coarse and fine grained meteorites were highlighted. Moreover, the residual stress state was statistically analysed in three orthogonal directions finding evidence of the existence of both type I and type II residual stress components. Finally, the application of von Mises approach allowed to determine the distribution of type II stress.

  5. The structure of para-toluidine by X-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Bertinotti, A.L.

    1965-12-01

    The crystal and molecular structure of para-toluidine has been solved by X-ray and neutron diffraction counter techniques. The molecules are arranged in the form of infinite chains in the crystal, each molecule being linked to two neighbours by hydrogen bonds. The presence of the H bonds makes clear the difference in the melting points between para-toluidine and benzene hydrocarbons of related symmetry and molecular weight. Their direction accounts for the (001) cleavage and the growth anisotropy of crystals from supersaturated vapour phase. A structure-seeking method by computer has been elaborated, using lattice energy calculations applied to molecules treated as rigid bodies and making use of a simplex method for function minimization without calculation of derivatives. The way the available information is handled allows to increase the range of convergence, as shown in the case of para-toluidine. (author) [fr

  6. A powder neutron diffraction study of stoichiometric silver beta alumina at 4.2 K

    International Nuclear Information System (INIS)

    Newsam, J.M.; Tofield, B.C.

    1980-10-01

    The low-temperature structure of stoichiometric silver beta alumina, AgAl 11 O 17 , is described for the first time. A powder neutron diffraction study at 4.2 K reveals that there is a single three-fold silver location of unit occupancy in each mirror plane. The silver site lies between the mid-oxygen and Beevers-Ross positions where the Ag-O contact distances can be minimised. The Ag-O interactions, in particular the cooperative movement of the spacer oxygens, are responsible for the superlattice which has been described previously. The Beevers-Ross, anti-Beevers-Ross and interstitial aluminium sites are vacant and the c-axis constant is expanded relative to the non-stoichiometric parent. (author)

  7. Neutron diffraction study of high temperature phase of K2SeO4

    International Nuclear Information System (INIS)

    Iwata, Yutaka; Koyano, Nobumitsu; Shibuya, Iwao; Hidaka, Masanori; Okazaki, Atsushi.

    1984-01-01

    The crystal structure of high-temperature phase of K 2 SeO 4 has been determined by means of single crystal neutron diffraction. The space group is P6 3 /mmc of hexagonal system with two formula units per unit cell. The structure is characterized by an averaged dispositions of SeO 4 tetrahedra with one of its Se-O bonds pointing parallel and antiparallel to the hexagonal c-axis in addition to the split distribution of potassium atoms. Heavily distorted distribution of oxygen atoms in SeO 4 is observed in Fourier maps corrersponding to split positions and reorientational motion of tetrahedra. This disordered arrangement is found to have close relation with the room temperature orthorhombic structure. The hexagonal-orthorhombic phase transition of K 2 SeO 4 at 472 0 C is grouped to an order-disorder type. (author)

  8. A neutron diffraction study on deuterated Rochelle salt structure at - 195degC paraelectric phase

    International Nuclear Information System (INIS)

    Iwata, Yutaka; Mitani, Shigeshi; Fukui, Susumu; Shibuya, Iwao

    1989-01-01

    Neutron diffraction study on the low temperature paraelectric phase of Rochelle salt was performed using deuterated single crystal specimen. Large anisotropic thermal motions of atoms are found to be prevailing in the lower paraelectric phase. This indicates the disordering of atoms and the analysis by two-site split-atom method showed that a split atom model holds equally well with an ordinary non-split model. By connecting split positions selectively, a disordered paraelectric structure, which is composed of half-occupied units, was obtained. These units can be regarded as ones in the ferroelectric phase according to a deduction from an order-disorder phase transition scheme. A possibility of existence of the 'local disorder' of O(5)-H group in the tartrate molecule was examined by Fourier method and a result proved to be negative. Present disordered model gives better understanding to the phase transition scheme of Rochelle salt than the local disorder model case. (author)

  9. Characterisation of polycrystal deformation by numerical modelling and neutron diffraction measurements

    International Nuclear Information System (INIS)

    Clausen, B.

    1997-09-01

    The deformation of polycrystals are modelled using three micron mechanic models; the Taylor model, the Sachs model and Hutchinson's self-consistent (SC) model. The predictions of the rigid plastic Taylor and Sachs models are compared with the predictions of the SC model. As expected, the results of the SC model is about half-way between the upper- and lower-bound models. The influence of the elastic anisotropy is investigated by comparing the SC predictions for aluminium, copper and a hypothetical material (Hybrid) with the elastic anisotropy of copper and the Young's modulus and hardening behaviour of aluminium. It is concluded that the effect of the elastic anisotropy is limited to the very early stages of plasticity, as the deformation pattern is almost identical for the three materials at higher strains. The predictions of the three models are evaluated by neutron diffraction measurements of elastic lattice strains in grain sub-sets within the polycrystal. The two rigid plastic models do not include any material parameters and therefore the predictions of the SC model is more accurate and more detailed than the predictions of the Taylor and Sachs models. The SC model is used to determine the most suitable reflection for technological applications of neutron diffraction, where focus is on the volume average stress state in engineering components. To be able to successfully to convert the measured elastic lattice strains for a specific reflection into overall volume average stresses, there must be a linear relation between the lattice strain of the reflection and the overall stress. According to the model predictions the 311-reflection is the most suitable reflection as it shows the smallest deviations from linearity and thereby also the smallest build-up of residual strains. The model predictions have pin pointed that the selection of the reflection is crucial for the validity of stresses calculated from the measured elastic lattice strains. (au) 14 tabs., 41

  10. Neutron diffraction studies of magnetic ordering in Ni-doped LaCoO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Rajeevan, N.E. [Department of Physics, Z.G. College, Calicut 673014, Kerala (India); Kumar, Vinod; Kumar, Rajesh [Department of Physics, National Institute of Technology, Hamirpur 177005, Himachal Pradesh (India); Kumar, Ravi [Beant College of Engineering and Technology, Gurudaspur 143521, Punjab (India); Kaushik, S.D. [UGC-DAE CSR Mumbai Centre, R-5 Shed, BARC, Mumbai 400085, Maharashtra (India)

    2015-11-01

    Research in rare earth cobaltite has recently been intensified due to its fascinating magnetic properties. LaCoO{sub 3}, an important cobaltite, exhibits two prominent susceptibility features at ~90 K and 500 K in low field measurement. The magnetic behavior below 100 K is predominantly antiferromagnetic (AFM), but absence of pure AFM ordering and emergence of ferromagnetic coupling on further decreasing temperature made situation more intricate. The present work of studying the effect of Ni substitution at Co site in polycrystalline LaCo{sub 1−x}Ni{sub x}O{sub 3} (0≤x≤0.3) is motivated by the interesting changes in magnetic and electronic properties. For lucid understanding, temperature dependent neutron diffraction (ND) study was carried out. ND patterns fitted with rhombohedral structure in perovskite form with R-3c space group, elucidated information on phase purity. Further temperature dependent cell parameter, Co–O bond-length and Co–O–Co bond angle were calculated for the series of Ni doped LaCoO{sub 3}. The results are explained in terms of decrease in the crystal field energy which led to the transition of cobalt from low Spin (LS) state to intermediate spin state (IS). - Highlights: • Temperature dependent neutron diffraction (ND) on Ni doped LaCoO{sub 3} are studied. • Microscopic parameters (cell, bond length, bond angle etc.) are determined by ND. • Increase in Co–O bond length and decrease in Co–O–Co bond angle on Ni substitution. • Ionic radii of Co{sup +3} in IS state (0.56 Å) is larger than in LS state (0.54 Å). • Lattice expansion induced increase in Co–O length stabilizes Co{sup +3} in magnetic state.

  11. Application of in situ diffraction in high-throughput structure determination platforms.

    Science.gov (United States)

    Aller, Pierre; Sanchez-Weatherby, Juan; Foadi, James; Winter, Graeme; Lobley, Carina M C; Axford, Danny; Ashton, Alun W; Bellini, Domenico; Brandao-Neto, Jose; Culurgioni, Simone; Douangamath, Alice; Duman, Ramona; Evans, Gwyndaf; Fisher, Stuart; Flaig, Ralf; Hall, David R; Lukacik, Petra; Mazzorana, Marco; McAuley, Katherine E; Mykhaylyk, Vitaliy; Owen, Robin L; Paterson, Neil G; Romano, Pierpaolo; Sandy, James; Sorensen, Thomas; von Delft, Frank; Wagner, Armin; Warren, Anna; Williams, Mark; Stuart, David I; Walsh, Martin A

    2015-01-01

    Macromolecular crystallography (MX) is the most powerful technique available to structural biologists to visualize in atomic detail the macromolecular machinery of the cell. Since the emergence of structural genomics initiatives, significant advances have been made in all key steps of the structure determination process. In particular, third-generation synchrotron sources and the application of highly automated approaches to data acquisition and analysis at these facilities have been the major factors in the rate of increase of macromolecular structures determined annually. A plethora of tools are now available to users of synchrotron beamlines to enable rapid and efficient evaluation of samples, collection of the best data, and in favorable cases structure solution in near real time. Here, we provide a short overview of the emerging use of collecting X-ray diffraction data directly from the crystallization experiment. These in situ experiments are now routinely available to users at a number of synchrotron MX beamlines. A practical guide to the use of the method on the MX suite of beamlines at Diamond Light Source is given.

  12. Optimizing structure in nanodiamonds using in-situ strain-sensitive Bragg coherent diffraction imaging.

    Science.gov (United States)

    Hruszkewycz, Stephan; Cha, Wonsuk; Ulvestad, Andrew; Fuoss, Paul; Heremans, F. Joseph; Harder, Ross; Andrich, Paolo; Anderson, Christopher; Awschalom, David

    The nitrogen-vacancy center in diamond has attracted considerable attention for nanoscale sensing due to unique optical and spin properties. Many of these applications require diamond nanoparticles which contain large amounts of residual strain due to the detonation or milling process used in their fabrication. Here, we present experimental, in-situ observations of changes in morphology and internal strain state of commercial nanodiamonds during high-temperature annealing using Bragg coherent diffraction imaging to reconstruct a strain-sensitive 3D image of individual sub-micron-sized crystals. We find minimal structural changes to the nanodiamonds at temperatures less than 650 C, and that at higher temperatures up to 750 C, the diamond-structured volume fraction of nanocrystals tend to shrink. The degree of internal lattice distortions within nanodiamond particles also decreases during the anneal. Our findings potentially enable the design of efficient processing of commercial nanodiamonds into viable materials suitable for device design. We acknowledge support from U.S. DOE, Office of Science, BES, MSE.

  13. Pyrophosphate-Inhibition of Apatite Formation Studied by In Situ X-Ray Diffraction

    Directory of Open Access Journals (Sweden)

    Casper Jon Steenberg Ibsen

    2018-02-01

    Full Text Available The pathways to crystals are still under debate, especially for materials relevant to biomineralization, such as calcium phosphate apatite known from bone and teeth. Pyrophosphate is widely used in biology to control apatite formation since it is a potent inhibitor of apatite crystallization. The impacts of pyrophosphate on apatite formation and crystallization kinetics are, however, not fully understood. Therefore, we studied apatite crystallization in water by synchrotron in situ X-ray diffraction. Crystallization was conducted from calcium chloride (0.2 M and sodium phosphate (0.12 M at pH 12 where hydrogen phosphate is the dominant phosphate species and at 60 °C to allow the synchrotron measurements to be conducted in a timely fashion. Following the formation of an initial amorphous phase, needle shaped crystals formed that had an octacalcium phosphate-like composition, but were too small to display the full 3D periodic structure of octacalcium phosphate. At later growth stages the crystals became apatitic, as revealed by changes in the lattice constant and calcium content. Pyrophosphate strongly inhibited nucleation of apatite and increased the onset of crystallization from minute to hour time scales. Pyrophosphate also reduced the rate of growth. Furthermore, when the pyrophosphate concentration exceeded ~1% of the calcium concentration, the resultant crystals had reduced size anisotropy suggesting that pyrophosphate interacts in a site-specific manner with the formation of apatite crystals.

  14. Uranium oxidation kinetics monitored by in-situ X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Zalkind, S., E-mail: shimonzl@nrcn.org.il; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

    2017-03-15

    The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90–150 °C was studied by means of in-situ X-ray diffraction (XRD). A “breakaway” in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO{sub 2}(111) is the prominent one. As the oxide thickens, the growth rate of UO{sub 2}(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Q{sub parabolic} = 17.5 kcal/mol and Q{sub linear} = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

  15. In situ synchrotron X-ray diffraction study of hydrides in Zircaloy-4 during thermomechanical cycling

    Energy Technology Data Exchange (ETDEWEB)

    Cinbiz, Mahmut N., E-mail: cinbizmn@ornl.gov [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Koss, Donald A., E-mail: koss@ems.psu.edu [Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Motta, Arthur T., E-mail: atm2@psu.edu [Department of Mechanical and Nuclear Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA, 16802 (United States); Park, Jun-Sang, E-mail: parkjs@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States); Almer, Jonathan D., E-mail: almer@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL, 60439 (United States)

    2017-04-15

    The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. These experimental results can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix. - Highlights: •The δ{111} d-spacings aligned with the hydride plate edges exhibit a bi-linear thermal expansion. •Stress state reversal is predicted with the onset of hydride dissolution. •During dissolution, the δ{111} planes oriented parallel to the hydride plate face initially contract upon heating. •Hydride d-spacings indicate that both in-plane (circumferential) and out-of-plane (radial) hydrides are in the same strain-state and likely in the same stress state as well.

  16. Chloride influence on the formation of lanthanum hexaboride: An in-situ diffraction study

    Science.gov (United States)

    Mattox, Tracy M.; Groome, Chloe; Doran, Andrew; Beavers, Christine M.; Urban, Jeffrey J.

    2018-03-01

    LaB6 has been a material of interest for decades due to its thermionic emission, plasmonic properties, and low work function, and researchers continue to discover new properties even now. In order to meet growing interest in customizing these properties, it is important to gain better control over the system and a better understanding of the fundamental mechanism of LaB6 crystal growth and formation. Traditional synthetic methods require very high temperatures, at which point crystallization happens too quickly to be readily studied. Our discovery that LaB6 may be made using lower temperatures has made it possible to slow down crystal formation enough for lattice growth to be observed. We report here an in situ diffraction study of the reaction between LaCl3 and NaBH4. In observing the evolution of the (1 1 1), (1 1 0), and (2 0 0) lattice planes of LaB6, we have discovered that the Cl of LaCl3 has a strong influence on crystal formation, and that excess Cl, temperature and heating rate may all be used as tools to control the LaB6 final product.

  17. Neutron diffraction as a tool in the study of reinforced concrete. Compilation of some cases

    International Nuclear Information System (INIS)

    Castellote, M

    2014-01-01

    Cementitious materials are much more complex than it seems at a first sight. On one hand, due to the excess of water needed to make the mix workable, a network of pores is generated, that puts in contact the material with the environment and allows their attack by aggressive agents that can be physical of chemical agents, producing the deterioration of the concrete itself and corrosion of the rebars. Then, it is necessary to study the transport properties and the chemical and physical interaction of aggressive agents with the solid and liquid phases of the cement paste the corrosion of the rebars, and the reparation processes. This is an approach concerning the service life of structures, however, we cannot forget an important chapter which is gaining much relevance in the last time: that of the special uses of concrete, for which, tailored concretes have to be designed. In order to undertake these problems, we need new analysis tools, different that the traditionally ones applied to study concrete, that allows the understanding of the mechanisms regulating the processes. One of these analysis tools is neutron diffraction that gives us the possibility of study the bulk of materials using a quite big specimen. In this work, 4 different problems undertaken with the help of neutrons in experiments carried out by the group of the author at the ILL, at the D1B and D20 instruments are presented

  18. FEM Analysis and Measurement of Residual Stress by Neutron Diffraction on the Dissimilar Overlay Weld Pipe

    International Nuclear Information System (INIS)

    Kim, Kang Soo; Lee, Ho Jin; Woo, Wan Chuck; Seong, Baek Seok; Byeon, Jin Gwi; Park, Kwang Soo; Jung, In Chul

    2010-01-01

    Much research has been done to estimate the residual stress on a dissimilar metal weld. There are many methods to estimate the weld residual stress and FEM (Finite Element Method) is generally used due to the advantage of the parametric study. And the X-ray method and a Hole Drilling technique for an experimental method are also usually used. The aim of this paper is to develop the appropriate FEM model to estimate the residual stresses of the dissimilar overlay weld pipe. For this, firstly, the specimen of the dissimilar overlay weld pipe was manufactured. The SA 508 Gr3 nozzle, the SA 182 safe end and SA376 pipe were welded by the Alloy 182. And the overlay weld by the Alloy 52M was performed. The residual stress of this specimen was measured by using the Neutron Diffraction device in the HANARO (High-flux Advanced Neutron Application ReactOr) research reactor, KAERI (Korea Atomic Energy Research Institute). Secondly, FEM Model on the dissimilar overlay weld pipe was made and analyzed by the ABAQUS Code (ABAQUS, 2004). Thermal analysis and stress analysis were performed, and the residual stress was calculated. Thirdly, the results of the FEM analysis were compared with those of the experimental methods

  19. First steps of ion beam mixing: study by X-ray reflectometry and neutron diffraction

    International Nuclear Information System (INIS)

    Le Boite, M.G.

    1987-12-01

    There are several processes involved in ion beam mixing: ballistic processes, chemical driving forces and radiation enhanced diffusion. Experiments usually performed on bilayers irradiated with heavy elements and characterized by Rutherford backscattering (R.B.S.), have shown that the measured mixing rate is always higher than the calculated one, taking into account ballistic effects only. Besides classical R.B.S. experiments on NiAu and NiPt bilayers irradiated with Xe, we have used another technique of characterization: X-ray reflectometry and neutron diffraction, performed on multilayers irradiated with He. The systems are NiAu, NiPt, NiPd and NiAg, which behave similarly from the ballistic point of view, but have very different heats of mixing. In these experiments, the range of deposited energy density is very low, in contrast to heavy ions irradiation: this has allowed us to reach very low diffusion coefficient, never observed before. The dependence of the diffusion coefficient on the heat of mixing is in agreement with the one theoretically calculated. For the NiAg system, which has a positive heat of mixing, the measured diffusion coefficient is smaller than the ballistic one: a decrease of the ballistic mixing rate is seen for the first time. In this work, we have shown the interest of the reflectometry techniques (X-ray and neutrons); we have used a simple model to analyze the ion beam mixing, when elementary processes are involved

  20. Neutron diffraction study of δ-alloy Pu{sup 242}–Ga aging

    Energy Technology Data Exchange (ETDEWEB)

    Somenkov, V.A. [National Research Center “Kurchatov Institute”, Moscow (Russian Federation); Blanter, M.S., E-mail: mike.blanter@gmail.com [Moscow State University of Instrumental Engineering and Information Science, Moscow (Russian Federation); Glazkov, V.P. [National Research Center “Kurchatov Institute”, Moscow (Russian Federation); Laushkin, A.V.; Orlov, V.K. [JSC VNIINM n.a. A.A. Bochvar, Moscow (Russian Federation)

    2014-09-15

    In this paper, we report on a continuing neutron diffraction study of the mean-square atom displacements occurring during the long-term self-irradiation of a Pu–Ga alloy. The measurements were performed at room temperature using the sample based on the isotope Pu{sup 242} with low neutron absorption cross-section to which the short-lived isotope Pu{sup 238} (1.4 wt.%) was added to accelerate self-irradiation. We obtain the maximum self-irradiation equivalent time of 35.5 years, 12 years longer than in our previous papers. In the entire range of self-irradiation time a single fcc phase is preserved. It was found that after the two stages of change in the mean-square displacements we observed earlier (rapid growth up to ∼5–6 equivalent years and a slow decline in the range of ∼6–25 years), comes a stage of stabilization (after ∼25 years). The stabilization can be explained by the emergence of a balance between the formation of point defects and their absorption by helium bubbles and dislocation loops which accumulated over time.

  1. Neutron-diffraction localization of deuterium in Ti6OD0,45 alloy

    International Nuclear Information System (INIS)

    Sumin, V.V.; Fadeev, N.V.; Morozov, S.I.

    1987-01-01

    Attemp to localize hydrogen in TiO alloy octahedral internodes was made by independent method. To do this, deuterium and hydrogen interstitial solid solutions in titanium were studied by neutron-diffraction method. Deuterium localization in crystal lattice is considerably more reliable, than hydrogen localization due to low noncoherent cross-section of neutron scattering by deuterium. Phase analysis of TiO samples with different deuterium content has shown, that alloys remain singlephase, at least, up to D/O≤1/2 composition. Second phase presence in a sample was determined with accuracy of up to ∼1%, that was proved by phase mixing-in method. Deuterium distribution analysis was conducted for Ti 6 O alloy. It is shown, that presence of oxigen atoms within titanium matrix provides conditions for hydrogen and deuturium localization in octacell layers, which are partially filled with oxygen atoms. Here, hydrogen (Deuterium) forms with oxygen O-H pairs (D), placed in plane parallel to basis HCP of titanium lattice. The most possible characteristic distance between oxygen and hydrogen atoms constitutes a 0 =2,96A (a o -HCP parameter of Ti lattice in Ti 6 O alloy)

  2. X-ray and neutron diffraction study of alums. Pt. 2 and 3

    International Nuclear Information System (INIS)

    Abdeen, A.M.; Will, G.; Schaefer, W.; Kirfel, A.; Bargouth, M.O.; Recker, K.; Weiss, A.

    1981-01-01

    The crystal structure of the alums, (NH 3 CH 3 )Al(SO 4 ) 2 x 12 H 2 0 and (NH 4 )AL(SO 4 ) 2 x 12 H 2 0, has been determined and refined from X-ray and neutron diffraction data. The compounds crystallize cubic in space group Pa3 (Z = 4). The positional and thermal parameters of all atoms including hydrogens have been refined by full matrix least-sqares analysis resulting in Rsub(w) values from the X-ray and neutron data of 0.030 and 0.029 respectively for the methylammonium alum and of 0.024 and 0.014 respectively for the ammonium alum. The atoms of the cation groups (NH 3 CH 3 ) + and (NH 4 ) + are distributed on 8(c) and 24(d) positions in two orientations of equal probability on and around the [111] direction related to each other by an inversion centre. The disorder in the cation groups is explained by a quantized rotation. Disorder in the sulfate groups has been determined to 4.2% for the methylammonium alum and to about 17% for the ammonium alum. The disordered sulfate tetrahedra are distorted and in a reversed orientation along the threefold axis. The system of the hydrogen bonds is discussed. (orig.)

  3. The structure of phosphate glass biomaterials from neutron diffraction and 31P nuclear magnetic resonance data

    International Nuclear Information System (INIS)

    Pickup, D M; Ahmed, I; Guerry, P; Knowles, J C; Smith, M E; Newport, R J

    2007-01-01

    Neutron diffraction and 31 P nuclear magnetic resonance spectroscopy were used to probe the structure of phosphate glass biomaterials of general composition (CaO) 0.5-x (Na 2 O) x (P 2 O 5 ) 0.5 (x = 0, 0.1 and 0.5). The results suggest that all three glasses have structures based on chains of Q 2 phosphate groups. Clear structural differences are observed between the glasses containing Na 2 O and CaO. The P-O bonds to bridging and non-bridging oxygens are less well resolved in the neutron data from the samples containing CaO, suggesting a change in the nature of the bonding as the field strength of the cation increases Na + → Ca 2+ . In the (CaO) 0.5 (P 2 O 5 ) 0.5 glass most of the Ca 2+ ions are present in isolated CaO x polyhedra whereas in the (Na 2 O) 0.5 (P 2 O 5 ) 0.5 glass the NaO x polyhedra share edges leading to a Na-Na correlation. The results of the structural study are related to the properties of the (CaO) 0.4 (Na 2 O) 0.1 (P 2 O 5 ) 0.5 biomaterial

  4. Evaluation of neutron sources for ISAGE-in-situ-NAA for a future lunar mission.

    Science.gov (United States)

    Li, X; Breitkreutz, H; Burfeindt, J; Bernhardt, H-G; Trieloff, M; Hopp, J; Jessberger, E K; Schwarz, W H; Hofmann, P; Hiesinger, H

    2011-11-01

    For a future Moon landing, a concept for an in-situ NAA involving age determination using the (40)Ar-(39)Ar method is developed. A neutron source (252)Cf is chosen for sample irradiation on the Moon. A special sample-in-source irradiation geometry is designed to provide a homogeneous distribution of neutron flux at the irradiation position. Using reflector, the neutron flux is likely to increase by almost 200%. Sample age of 1Ga could be determined. Elemental analysis using INAA is discussed. Copyright © 2011 Elsevier Ltd. All rights reserved.

  5. Structure of zinc and niobium tellurite glasses by neutron and x-ray diffraction

    International Nuclear Information System (INIS)

    Hoppe, U; Yousef, E; Ruessel, C; Neuefeind, J; Hannon, A C

    2004-01-01

    Neutron and x-ray diffraction experiments of high resolving power with neutrons from a spallation source and high-energy photons from a synchrotron have been performed on compositional series of binary Zn, Nb and on mixed Zn/Nb tellurite glasses. The Te-O, Zn-O and Nb-O coordination numbers are determined by Gaussian fitting of the first-neighbour peaks in the neutron and x-ray data simultaneously. The transition of TeO 4 to TeO 3 units with increasing fraction of a second component is indicated by decreasing total Te-O coordination numbers. This transition appears different for glasses with ZnO or Nb 2 O 5 additions. Details of the Te-O peaks suggest there are two species of Te-O bonds with lengths of ∼ 0.19 and ∼ 0.21 nm. The change of their fractions shows excellent agreement with the existence of TeO 4 trigonal bipyramids and TeO 3 trigonal pyramids. All oxygen atoms from ZnO and Nb 2 O 5 are used for rupture of Te-O-Te bridges, which is accompanied with a change of nearly all participating TeO 4 to TeO 3 groups. The tendency for a TeO 4 → TeO 3 change decreases for glasses of higher second component content which is accompanied by the occurrence of TeO 4 groups with non-bridging oxygens. The Nb tellurite glasses show transition to network-forming behaviour with the formation of Nb-O-Nb bridges. The fractions of TeO 3 units of ternary Zn/Nb tellurite glasses agree with an additivity behaviour of the modifying effects of ZnO and Nb 2 O 5 additions

  6. Implementation of neutron diffraction technique at Nuclear Center of National Institute of Nuclear Research for study of materials

    International Nuclear Information System (INIS)

    Macias Betanzos, L.R.

    1993-01-01

    The Neutron Diffraction technique, it's a helpful tool for the study of materials. The purpose, was to verify that such technique works with the Neutron Diffractometer of National Institute of Nuclear Research. The scope, is to study crystalline materials by the Neutron Diffraction Method, that means it completion with Bragg's Law. There exist a lot of diffraction techniques that depend on the kind of study to do. In this case the study was to measure known samples to have a correlation between parameters such a extinction factor and dislocation density. Known copper deformed samples were measured to observe the extinction effect and it could be observed. We had to calibrate the Neutron Diffractometer, the detection system and to have an optimal movement control of diffractometer devices by mean of a microcomputer. Also, was necessary to control the Reactor TRIGA operation to minimize the neutron flux oscillation. It was not possible the quantification of dislocation density in the samples because the relation signal/background was about one and it gives high inaccuracy. To correct this problem, it's necessary to have a better shielding to minimize the contribution of the background. The conclusion is that the Neutron Diffractometer is in conditions to carry out investigation on the material field, today it can be lattice constants, crystalline phases and measurements of metallic textures. For such studies, it's necessary to have samples with 2 cm 3 or higher to increase the relation signal/background. At present, we have the process software to give the interpretation of the Neutron Diffraction process. (Author). 12 refs, 16 figs

  7. Residual Stress Measurement of SiC tile/Al7075 Hybrid Composites by Neutron Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Park, Jong Bok; Lee, Jun Ho; Hong, Soon Hyung; Ryu, Ho Jin [KAIST, Daejeon (Korea, Republic of); Lee, Sang Bok; Lee, Sang Kwan [Korea Institute of Materials Science, Changwon (Korea, Republic of); Muslihd, M. Rifai [Center for Advanced Materials Science and Technology, Tangerang (India)

    2016-05-15

    In this research, SiC which has low density, high compressive strength, and high elastic modulus was used to fabricate the armor plate. In addition, Al which has low density and high toughness was used for a metal matrix of the composites. If two materials are combined, the composite can be effective materials for light weight armor applications. However, the existence of a large difference in coefficients of thermal expansion (CTE) between SiC and Al matrix, SiC/Al composites can have residual stresses while cooled in the fabrication process. Previous research reported that residual stresses in the composites or microstructures have an effect on the fatigue life and their mechanical properties. Some researchers reported about the residual stresses in the SiCp/Al metal matrix composites by numerical simulation systems, X-ray diffraction, and destructive methods. In order to analyze the residual stress of SiC/Al composites, the neutron diffraction as the non-destructive method was performed in this research. The 50 vol.% SiC{sub p}/Al7075 composites and SiC tile inserted 50 vol.% SiC{sub p}/Al7075 hybrid composites were measured to analyze the residual stress of Al (111) and SiC (111). Both samples had the tensile residual stresses in the Al (111) and the compressive residual stresses in the SiC (111) due to the difference in CTE.

  8. Thermodynamic and neutron diffraction studies on multiferroic NdMn{sub 2}O{sub 5}

    Energy Technology Data Exchange (ETDEWEB)

    Chattopadhyay, S.; Balédent, V.; Auban-Senzier, P.; Pasquier, C.; Doubrovsky, C. [Laboratoire de Physique des Solides, Université Paris-Sud, CNRS-UMR 8502, 91405 Orsay (France); Greenblatt, M. [Department of Chemistry and Chemical Biology, Rutgers, The State University of New Jersey, Piscataway, NJ 08854 (United States); Foury-Leylekian, P., E-mail: pascale.foury@u-psud.fr [Laboratoire de Physique des Solides, Université Paris-Sud, CNRS-UMR 8502, 91405 Orsay (France)

    2015-03-01

    Magnetically frustrated RMn{sub 2}O{sub 5} oxides have attracted considerable attention in recent years, because most of the members of this family show spin ordering induced dielectric polarization along with strong magneto-electric coupling. Although the true origin of the ferroelectricity is still a matter of debate, it has been observed that the magneto-electric phase diagram can be substantially tuned with the variation of rare earth elements. In this work, we have chosen NdMn{sub 2}O{sub 5} as the compound of our interest since it lies exactly in between the ferroelectric and non-ferroelectric members of this family and also, because there are few investigations performed on RMn{sub 2}O{sub 5} systems with large rare earth atoms . With the combination of heat capacity, magnetic susceptibility, dielectric permittivity, powder X-ray diffraction, and powder neutron diffraction measurements, it has been found that NdMn{sub 2}O{sub 5} undergoes an incommensurate magnetic ordering around 30 K followed by a possible ferroelectric-like transition at ∼26 K. Another lock-in kind of magnetic transition appears when the temperature is decreased to ∼15 K. With further lowering of temperature, an antiferromagnetic ordering, which is presumably associated with the Nd{sup 3+}, is achieved near 4 K. This study thus sheds light on a new compound of the RMn{sub 2}O{sub 5} series presenting different multiferroic properties.

  9. Potassium Disorder in the Defect Pyrochlore KSbTeO6: A Neutron Diffraction Study

    Directory of Open Access Journals (Sweden)

    José Antonio Alonso

    2017-01-01

    Full Text Available KSbTeO6 defect pyrochlore has been prepared from K2C2O4, Sb2O3, and 15% excess TeO2 by solid-state reaction at 850 °C. Direct methods implemented in the software EXPO2013 allowed establishing the basic structural framework. This was followed by a combined Rietveld refinement from X-ray powder diffraction (XRD and neutron powder diffraction (NPD data, which unveiled additional structural features. KSbTeO6 is cubic, a = 10.1226(7 Å, space group F d 3 ¯ m , Z = 8 and it is made of a mainly covalent framework of corner-sharing (Sb,TeO6 octahedra, with weakly bonded K+ ions located within large cages. The large K-O distances, 3.05(3–3.07(3 Å, and quite large anisotropic atomic displacement parameters account for the easiness of K+ exchange for other cations of technological importance.

  10. Texture analysis of a friction stir processed 6061-T6 aluminum alloy using neutron diffraction

    International Nuclear Information System (INIS)

    Woo, W.; Choo, H.; Brown, D.W.; Vogel, S.C.; Liaw, P.K.; Feng, Z.

    2006-01-01

    Time-of-flight neutron diffraction was used to investigate the texture changes in friction stir-processed (FSP) 6061-T6 aluminum alloy plates. Two different specimens were prepared with the purpose of separating the effects of frictional heating and severe plastic deformation on the changes of the preferred orientation in the as-received rolled plates: a plate processed with both stirring pin and tool shoulder, i.e., a regular FSP plate subjected to both severe plastic deformation and frictional heating (Case 1); and a plate processed only with the tool shoulder, i.e., subjected mainly to frictional heating (Case 2). The diffraction peak intensities provide insights into the texture variations at various locations across the centerline and through the thickness of the FSP plates. Comparison of the texture variations between Cases 1 and 2 clearly shows that the severe plastic deformation from the stirring pin affects the preferred orientation during the FSP, while heating alone from the tool shoulder has little effect

  11. Crystal structure investigations on cation-substituted alums by X-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Abdeen, A.M.

    1980-04-01

    The crystal structures of the three alums: NH 4 Al(SO 4 ) 2 .12H 2 O, (NH 3 CH 3 )Al(SO 4 ) 2 .12H 2 O and (NH 3 OH)Al(SO 4 ) 2 .12H 2 O have been determined from three-dimensional neutron diffraction data enhanced by X-ray diffraction when necessary. These compounds crystallize cubic in space group Pa3. The structures of the three alums exhibit partial occupancies of crystallographic sites for the NH 4 , (NH 3 CH 3 ) and (NH 3 OH) group atoms. This can be explained by a quantized rotation of the three groups around an axis perpendicular to the [111] direction. Some of the (SO 4 ) 2- groups in the NH 4 -alum are disordered with about 17% of the sulfate tetrahedra being in a reversed orientation around the sulfur atom. The disorder in (NH 3 CH 3 ) and (NH 3 OH)-alums is only 4,3% and 3.0% respectively. The atoms in the alum structures are held together by a system of hydrogen bonds between the water molecules and between the water molecules and the sulfate oxygen atoms. In these three structures there is a strong indication that shorter hydrogen bonds tend to be nearly linear. (orig.)

  12. An investigation of the structure of disordered materials by using neutron diffraction

    International Nuclear Information System (INIS)

    Petri, I.

    1999-01-01

    The structure of several semiconducting, metallic and ionic disordered materials was investigated using neutron diffraction and the results were compared with those obtained from recent ab initio molecular dynamics methods. The method of isotopic substitution was applied to measure the full set of partial structure factors, S αβ (Q), for the liquid semiconductor GeSe and the covalent network glass GeSe 2 . Their short range ordering and for GeSe 2 also the intermediate range ordering were identified and a substantial number of 'defects' such as homopolar bonds were detected in both systems. Further, the structure of liquid GeSe 2 with increasing temperature was studied at the total structure factor level. Also, changes in the topology of Ge x Se 1-x glasses in the range 0 ≤ x ≤ 0.4 were observed and investigated by measuring the total structure factors. As far as possible our results were compared with those from molecular dynamics studies. The Ge-Se system was found to serve as a sensitive test-system for these studies, giving an insight into the strengths and limitations of them. For instance, problems are found in the region of the homopolar bonds for g GeGe (r) and for the first sharp diffraction peak in the Bhatia-Thornton concentration-concentration structure factor that could not be reproduced. The structure of liquid lithium was measured and particular attention was paid to the inelasticity and resolution function corrections. The ion-ion and ion-valence electron partial structure factors were obtained and found to be in good agreement with ab initio molecular dynamics studies. The method of first order difference functions in neutron diffraction in combination with H/D substitution was applied to 2 molal solutions of Cu(ClO 4 ) 2 in perchloric acid to measure the Cu-H and, to a first order approximation, the Cu-O partial structure factor. A (4 + 1) distortion of the hydration shell around the Cu 2+ ion was measured. (author)

  13. Neutron diffraction as a precise and reliable method for obtaining structural properties of bulk quantities of graphene

    Czech Academy of Sciences Publication Activity Database

    Sofer, Z.; Šimek, P.; Jankovský, O.; Sedmidubský, D.; Beran, Přemysl; Pumera, M.

    2014-01-01

    Roč. 6, č. 21 (2014), s. 13082-13089 ISSN 2040-3364 R&D Projects: GA MŠk(XE) LM2011019 Institutional support: RVO:61389005 Keywords : graphen * graphit oxide * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 7.394, year: 2014

  14. Neutron diffraction studies on Ca1− xBaxZr4P6O24 solid solutions

    Indian Academy of Sciences (India)

    P6O24 compositions from combined Rietveld refinements of powder X-ray and neutron diffraction data. All the studied compositions crystallize in rhombohedral lattice (space group R-3 No. 148). A continuous solid solution is concluded from ...

  15. Hydrogen bond nature of ferroelectric material studied by X-ray and neutron diffraction. Electric dipole moment and proton tunneling

    International Nuclear Information System (INIS)

    Noda, Yukio; Kiyanagi, Ryoji; Mochida, Tomoyuki; Sugawara, Tadashi

    2006-01-01

    Hydrogen bond nature of MeHPLN and BrHPLN is studied using x-ray and neutron diffraction technique. We found that electric dipole moment of hydrogen atom plays an important role for the phase transition, and proton tunneling model is confirmed on this isolated hydrogen bond system. (author)

  16. Lattice-preferred orientations of late-Variscan granitoids derived from neutron diffraction data: implications for magma emplacement mechanisms

    Czech Academy of Sciences Publication Activity Database

    Müller, A.; Leiss, B.; Ullemeyer, K.; Breiter, Karel

    2011-01-01

    Roč. 100, č. 7 (2011), s. 1515-1532 ISSN 1437-3254 Institutional research plan: CEZ:AV0Z30130516 Keywords : neutron diffraction * lattice-preferred orientation * shape-preferred orientation * magma tic flow * Podlesí granite * Meissen massif Subject RIV: DB - Geology ; Mineralogy Impact factor: 2.342, year: 2011

  17. Stress-induced martensite variant reorientation in magnetic shape memory Ni–Mn–Ga single crystal studied by neutron diffraction

    Czech Academy of Sciences Publication Activity Database

    Molnár, Peter; Šittner, Petr; Lukáš, Petr; Hannula, S.-P.; Heczko, Oleg

    2008-01-01

    Roč. 17, č. 3 (2008), 035014/1-035014/4 ISSN 0964-1726 Institutional research plan: CEZ:AV0Z10100520; CEZ:AV0Z10480505 Keywords : NiMnGa single crystal * neutron diffraction * stress induced martensite reorientation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.743, year: 2008

  18. Twinning processes in Cu-Al-Ni martensite single crystals investigated by neutron single crystal diffraction method

    Czech Academy of Sciences Publication Activity Database

    Molnar, P.; Šittner, P.; Novák, V.; Lukáš, Petr

    2008-01-01

    Roč. 481, Sp.Iss.SI (2008), s. 513-517 ISSN 0921-5093 R&D Projects: GA AV ČR IAA100480704 Institutional research plan: CEZ:AV0Z10480505 Keywords : Cu-Al-Ni * single crystals * neutron diffraction Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 1.806, year: 2008

  19. Examples of neutron diffraction texture analysis on one and the same chalcopyrite sample before and after experimental deformation

    International Nuclear Information System (INIS)

    Jansen, E.M.; Brokmeier, H.G.; Siemes, H.

    1994-01-01

    Natural chalcopyrite specimens from Mt. Isa, Australia were investigated by neutron diffraction texture analysis. The preferred orientation of the specimens consists of 3 main orientation components. After axial shortening at a temperature of 25 C the initial orientation components became weaker, a new component was detected. (orig.)

  20. Anisotropic thermal expansion of MgSiN2 from 10 to 300 K as measured by neutron diffraction

    NARCIS (Netherlands)

    Bruls, R.J.; Hintzen, H.T.J.M.; Metselaar, R.; Loong, C.K.

    2000-01-01

    The lattice parameters of orthorhombic MgSiN2 as a function of the temperature have been determined from time-of-flight neutron powder diffraction. The results indicate that MgSiN2, just like several other adamantine-type crystals, exhibits a relatively small thermal expansion coefficient at low

  1. Non-destructive Quantitative Phase Analysis and Microstructural Characterization of Zirconium Coated U-10Mo Fuel Foils via Neutron Diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cummins, Dustin Ray [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Vogel, Sven C. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Hollis, Kendall Jon [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Donald William [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Dombrowski, David E. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2016-10-18

    This report uses neutron diffraction to investigate the crystal phase composition of uranium-molybdenum alloy foils (U-10Mo) for the CONVERT MP-1 Reactor Conversion Project, and determines the effect on alpha-uranium contamination following the deposition of a Zr metal diffusion layer by various methods: plasma spray deposition of Zr powders at LANL and hot co-rolling with Zr foils at BWXT. In summary, there is minimal decomposition of the gamma phase U-10Mo foil to alpha phase contamination following both plasma spraying and hot co-rolling. The average unit cell volume, i.e. lattice spacing, of the Zr layer can be mathematically extracted from the diffraction data; co-rolled Zr matches well with literature values of bulk Zr, while plasma sprayed Zr shows a slight increase in the lattice spacing, indicative of interstitial oxygen in the lattice. Neutron diffraction is a beneficial alternative to conventional methods of phase composition, i.e. x ray diffraction (XRD) and destructive metallography. XRD has minimal penetration depth in high atomic number materials, particularly uranium, and can only probe the first few microns of the fuel plate; neutrons pass completely through the foil, allowing for bulk analysis of the foil composition and no issues with addition of cladding layers, as in the final, aluminum-clad reactor fuel plates. Destructive metallography requires skilled technicians, cutting of the foil into small sections, hazardous etching conditions, long polishing and microscopy times, etc.; the neutron diffraction system has an automated sample loader and can fit larger foils, so there is minimal analysis preparation; the total spectrum acquisition time is ~ 1 hour per sample. The neutron diffraction results are limited by spectra refinement/calculation times and the availability of the neutron beam source. In the case of LANSCE at Los Alamos, the beam operates ~50% of the year. Following the lessons learned from these preliminary results, optimizations to

  2. Non-destructive Quantitative Phase Analysis and Microstructural Characterization of Zirconium Coated U-10Mo Fuel Foils via Neutron Diffraction

    International Nuclear Information System (INIS)

    Cummins, Dustin Ray; Vogel, Sven C.; Hollis, Kendall Jon; Brown, Donald William; Dombrowski, David E.

    2016-01-01

    This report uses neutron diffraction to investigate the crystal phase composition of uranium-molybdenum alloy foils (U-10Mo) for the CONVERT MP-1 Reactor Conversion Project, and determines the effect on alpha-uranium contamination following the deposition of a Zr metal diffusion layer by various methods: plasma spray deposition of Zr powders at LANL and hot co-rolling with Zr foils at BWXT. In summary, there is minimal decomposition of the gamma phase U-10Mo foil to alpha phase contamination following both plasma spraying and hot co-rolling. The average unit cell volume, i.e. lattice spacing, of the Zr layer can be mathematically extracted from the diffraction data; co-rolled Zr matches well with literature values of bulk Zr, while plasma sprayed Zr shows a slight increase in the lattice spacing, indicative of interstitial oxygen in the lattice. Neutron diffraction is a beneficial alternative to conventional methods of phase composition, i.e. x ray diffraction (XRD) and destructive metallography. XRD has minimal penetration depth in high atomic number materials, particularly uranium, and can only probe the first few microns of the fuel plate; neutrons pass completely through the foil, allowing for bulk analysis of the foil composition and no issues with addition of cladding layers, as in the final, aluminum-clad reactor fuel plates. Destructive metallography requires skilled technicians, cutting of the foil into small sections, hazardous etching conditions, long polishing and microscopy times, etc.; the neutron diffraction system has an automated sample loader and can fit larger foils, so there is minimal analysis preparation; the total spectrum acquisition time is ~ 1 hour per sample. The neutron diffraction results are limited by spectra refinement/calculation times and the availability of the neutron beam source. In the case of LANSCE at Los Alamos, the beam operates ~50% of the year. Following the lessons learned from these preliminary results, optimizations to

  3. In-situ elemental analysis of coal by neutron activation

    International Nuclear Information System (INIS)

    Mikesell, J.L.; Senftle, F.E.; Tanner, A.B.

    1986-01-01

    The U.S. Geological Survey (USGS) has worked to develop neutron techniques for the borehole measurement of the elemental composition of ores since 1969, and first demonstrated a borehole ultimate analysis of coal in 1977. Borehole measurements such as these permit real-time evaluation of coal quality without the expense of coring or the delays associated with laboratory analyses. Two technological innovations make such measurements possible: the availability, from Savannah River Operations Office, DOE, of small californium-252 (/sup 252/Cf) fission neutron sources, and the development, by USGS and Princeton Gamma-Techn, of the melting-cryogen-cooled high-purity germanium borehole gamma-ray detector. A technique of relating mass fractions to measured gamma-ray intensities, which eliminates the need for detailed knowledge of the geometry of the neutron distribution, is used to calculate elemental compositions without resorting to the test pits or computer borehole modeling. In coal, all of the major constituents (C, H, N, S, Si, Al, Fe, Ti) except oxygen can be determined quantitatively by thermal neutron capture gamma-ray spectroscopy

  4. Neutron irradiation effects on in situ Nb3Sn superconducting wires

    International Nuclear Information System (INIS)

    Hirano, Y.; Fukumoto, M.; Kodaka, H.; Nishijima, S.; Okada, T.; Yoshida, H.

    1985-01-01

    Three types of ''in situ'' Nb 3 Sn conductors have been studied to determine the detrimental effects of neutron irradiation on critical temperature, critical current and AC losses. It was found that at fluences of 10 18 n/cm 2 , the critical temperature is degraded by approximately 10%. Degradation of AC loss is discussed in comparison with that of critical current density

  5. In situ neutron depth profiling: A powerful method to probe lithium transport in micro-batteries

    NARCIS (Netherlands)

    Oudenhoven, J.F.M.; Labohm, F.; Mulder, M.; Niessen, R.A.H.; Mulder, F.M.; Notten, P.H.L.

    2011-01-01

    In situ neutron depth profiling (NDP) offers the possibility to observe lithium transport inside micro-batteries during battery operation. It is demonstrated that NDP results are consistent with the results of electrochemical measurements, and that the use of an enriched6LiCoO2 cathode offers more

  6. The Oxford-Diamond In Situ Cell for studying chemical reactions using time-resolved X-ray diffraction

    Science.gov (United States)

    Moorhouse, Saul J.; Vranješ, Nenad; Jupe, Andrew; Drakopoulos, Michael; O'Hare, Dermot

    2012-08-01

    A versatile, infrared-heated, chemical reaction cell has been assembled and commissioned for the in situ study of a range of chemical syntheses using time-resolved energy-dispersive X-ray diffraction (EDXRD) on Beamline I12 at the Diamond Light Source. Specialized reactor configurations have been constructed to enable in situ EDXRD investigation of samples under non-ambient conditions. Chemical reactions can be studied using a range of sample vessels such as alumina crucibles, steel hydrothermal autoclaves, and glassy carbon tubes, at temperatures up to 1200 °C.

  7. Neutron Production from In-situ Heavy Ice Coated Targets at Vulcan

    Science.gov (United States)

    Morrison, John; Krygier, A. G.; Kar, S.; Ahmed, H.; Alejo, A.; Clarke, R.; Fuchs, J.; Green, A.; Jung, D.; Kleinschmidt, A.; Najmudin, Z.; Nakamura, H.; Norreys, P.; Notley, M.; Oliver, M.; Roth, M.; Vassura, L.; Zepf, M.; Borghesi, M.; Freeman, R. R.

    2015-05-01

    Laser based neutron production experiments have been performed utilizing ultra-high intensity laser accelerated ions impinging upon a secondary target. The neutron yield from such experiments may be improved if the accelerated ions were primarily deuterons taking advantage of the d-d cross section. Recent experiments have demonstrated that selective deuteron acceleration from in-situ heavy ice coating of targets can produce ion spectra where deuterons comprise > 99 % of the measured ions. Results will be presented from integrated neutron production experiments from heavy ice targets coated in-situ recently performed on the Vulcan laser at Rutherford Appleton Laboratory. We are grateful for the Staff at RAL and acknowledge funding from the US DoE. AFOSR, European Social Fund, and the Czech Republic.

  8. Neutron diffraction studies on structural and magnetic properties of RE2NiGe3 (RE=La, Ce)

    International Nuclear Information System (INIS)

    Kalsi, Deepti; Rayaprol, S.; Siruguri, V.; Peter, Sebastian C.

    2014-01-01

    We report the crystallographic properties of RE 2 NiGe 3 (RE=La, Ce) synthesized by arc melting. Rietveld refinement on the powder neutron diffraction (ND) data suggest both compounds are isostructural and crystallize in the non-centrosymmetric Er 2 RhSi 3 type structure having hexagonal space group P6 ¯ 2c. In the crystal structure of RE 2 NiGe 3 , two dimensional arrangements of nickel and germanium atoms lead to the formation of hexagonal layers with rare earth atoms sandwiched between them. Magnetic susceptibility measurements performed in low fields exhibit antiferromagnetic ordering in cerium compound around (T o =) 3.2 K. Neutron diffraction measurements at 2.8 K (i.e., at Tdiffraction lines nor indicate the appearance of any new diffraction lines in the Q-range of 0.47–7.34 Å −1 , thus ruling out any long-range magnetic order. - Graphical abstract: The compounds La 2 NiGe 3 and Ce 2 NiGe 3 crystallize in the Er 2 RhSi 3 type. Magnetic susceptibility show antiferromagnetic ordering for Ce 2 NiGe 3 at 3.2 K and neutron diffraction confirms the absence of long range ordering. - Highlights: RE 2 NiGe 3 (RE=La, Ce) crystallize in the ordered superstructure of the AlB 2 type. Magnetic susceptibility measurements exhibit antiferromagnetic ordering in Ce 2 NiGe 3 . Structure and magnetism of RE 2 NiGe 3 (RE=La, Ce) are studied by neutron diffraction

  9. Investigation of digestion Kinetics in commercial starches using in-situ small-angle neutron scattering

    International Nuclear Information System (INIS)

    Blazek, Jaroslav; Gilbert, Elliot Paul

    2009-01-01

    Full text: The digestion of starch has been the subject of many investigations, mostly involving in vitro measurement of the susceptibility of starches to attack by different enzymes, rather than measuring actual digestibility in vivo. The rate and extent of amylolytic hydrolysis of granular starches is known to vary according to botanical origin. Granule characteristics considered to influence susceptibility to attack by alpha-amylase include crystallinity, granule size and available specific surface, amylose content, porosity, structural inhomogeneities and degree of integrity. Most in-vitro studies of granular starch digestion have been limited to samples for which aliquots have been removed from the reaction mixture at various time intervals and freeze-dried to be subsequently characterized using a range of techniques. It remains unclear whether sample preparation creates artefacts in the samples. In this study, we have studied the kinetics of starch digestion of several commercial granular starches by time-resolved small-angle neutron scattering using an in-situ digestion chamber allowing, for the first time, to follow structural changes of starch in the course of digestion directly in the digestion mixture. Additionally, samples before and after digestion were studied by x-ray diffraction, small-angle x-ray scattering, differential scanning calorimetry and microscopy. Microscopy revealed that studied starches, which varied in their amylose content and digestion kinetics, followed different modes of attack The multidisciplinary approach allowed the nanostructural changes detected by small-angle scattering in the course of enzymic breakdown to be correlated with changes in crystallinity and functional properties.

  10. In situ measurement of ash content by neutron activation analysis

    International Nuclear Information System (INIS)

    Chrusciel, E.; Palka, K.; Makhabane, J.L.

    1991-01-01

    The paper presents the results of spectrometric neutron activation logging. A scintillation spectrometer with the source-to-detector spacing of 1.5 m, together with a Po-Be neutron source, with the yield of about 10 7 n/s, were used to measure the intensity of gamma rays in two energy windows during continuous logging. The first energy window of 300 keV width was centered at the 843 keV energy and the second - of 500 keV width at 1779 keV. For ash content varying between 5-35 wt % the mean standard deviation was 2.5 wt %. (author). 22 refs, 6 figs, 1 tab

  11. Evaluation of material properties of SiC particle reinforced aluminum alloy composite using neutron and X-ray diffraction

    International Nuclear Information System (INIS)

    Akiniwa, Yoshiaki; Machiya, Shutaro; Kimura, Hidehiko; Tanaka, Keisuke; Minakawa, Nobuaki; Morii, Yukio; Kamiyama, Takashi

    2006-01-01

    The phase stresses under loading in a monolithic aluminum alloy and an aluminum alloy reinforced with silicon carbide particles were measured by the neutron diffraction method. Under uniaxial loading, the longitudinal and transverse strains in each constituent phase were measured. The diffraction elastic constants for each diffraction plane were investigated as a function of the diffraction intensity by TOF. Single peak analysis was carried out for each diffraction profile. The measured results were compared with the theoretical micromechanical models such as the self-consistent and Mori-Tanaka method using the Eshelby theory (MTE). The accuracy of the elastic constant strongly depends on the diffraction intensity. In order to confirm the rule of mixture, the phase stress was measured by the X-ray method. The macrostress calculated by the rule of mixture agreed very well with the applied stress. Finally, fatigue damage was evaluated by the neutron method. The change of the full width at half maximum in the aluminum phase during fatigue is small. On the other hand, the value in the SiC phase increased steeply just before fracture

  12. High-pressure cells for study of condensed matter by diffraction and inelastic neutron scattering at low temperatures and in strong magnetic fields

    Science.gov (United States)

    Sadykov, R. A.; Strassle, Th; Podlesnyak, A.; Keller, L.; Fak, B.; Mesot, J.

    2017-12-01

    We have developed and implemented series of new original clamp high-pressure cells for neutron diffraction and inelastic neutron scattering at low temperatures. The cells design allows one to place them in the standard cryostats or cryomagnets used on neutron sources. Some results obtained for ZnCr2Se4 are demonstrated as an example.

  13. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    International Nuclear Information System (INIS)

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

    2016-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  14. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Storm, Mie Møller, E-mail: mmst@dtu.dk; Johnsen, Rune E.; Norby, Poul

    2016-08-15

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  15. In situ X-ray diffraction study of the electrochemical reaction on lead electrodes in sulphate electrolytes

    International Nuclear Information System (INIS)

    Angerer, P.; Mann, R.; Gavrilovic, A.; Nauer, G.E.

    2009-01-01

    The anodic oxidation of pure lead in two acidic sulphate electrolytes with identical ionic strength (pH ∼ 0 and pH ∼ -0.1) was studied by in situ grazing incidence X-ray diffraction method (GIXD). Crystalline products such as lead sulphate (anglesite, PbSO 4 , orthorhombic), α- and β-lead dioxide (α-PbO 2 , orthorhombic, and β-PbO 2 , tetragonal), and tribasic lead sulphate hydrate with the stoichiometric composition 3PbO.PbSO 4 .H 2 O (triclinic) were detected at defined potentials. A method for the semi-quantitative determination of the thickness of the deposited layer from diffraction data is described. After the in situ measurement, the washed and dried working electrodes were additionally characterized ex situ by GIXD measurements at different angles of incidence. The phase litharge (lead oxide, t-PbO, tetragonal) and lead sulphate were observed at the surface of the lead substrate. The quantitative evaluation of the diffraction intensity of this measurement series enables the modelling of a qualitative depth profile of the layer generated during the electrochemical treatment. The anglesite phase is located in the uppermost layer, while the litharge phase was detected closer to the lead substrate

  16. Using neutron diffraction to examine the onset of mechanical twinning in calcite rocks

    Science.gov (United States)

    Covey-Crump, S. J.; Schofield, P. F.; Oliver, E. C.

    2017-07-01

    Experimental calibration of the calcite twin piezometer is complicated by the difficulty of establishing the stresses at which the twins observed in the final deformation microstructures actually formed. In principle, this difficulty may be circumvented if the deformation experiments are performed in a polychromatic neutron beam-line because this allows the elastic strain (and hence stress) in differently oriented grains to be simultaneously monitored from diffraction patterns collected as the experiment is proceeding. To test this idea small strain (marble (grain size 150 μm) and Solnhofen limestone (5 μm) at temperatures of 20°-600 °C using the ENGIN-X instrument at the ISIS neutron facility, UK. At the lowest temperatures (25 °C Carrara; 200 °C Solnhofen) the deformation response was purely elastic up to the greatest stresses applied (60 MPa Carrara; 175 MPa Solnhofen). The sign of the calcite elastic stiffness component c14 is confirmed to be positive when the obverse setting of the calcite rhombohedral lattice in hexagonal axes is used. In the Carrara marble samples deformed at higher temperatures, elastic twinning was initiated at small stresses (<15 MPa) in grains oriented such that the Schmid factor for twinning was positive on more than one e-twin system. At greater stresses (65 MPa at 200 °C decreasing to 41 MPa at 500 °C) there was an abrupt onset of permanent twinning in grains with large Schmid factors for twinning on any one e-twin system. No twinning was observed in the Solnhofen limestone samples deformed at 200° or 400 °C at applied stresses of <180 MPa. These results highlight the potential of this approach for detecting the onset of twinning and provide, through experiments on samples with different microstructures, a strategy for systematically investigating the effects of microstructural variables on crystallographically-controlled inelastic processes.

  17. Determination of low-field critical parameters of superconducting niobium by small-angle neutron diffraction

    International Nuclear Information System (INIS)

    Christen, D.K.; Spooner, S.; Thorel, P.; Kerchner, H.R.

    1977-01-01

    The perfect double-crystal small-angle diffraction technique enables measurement of scattering angles to within 0.3 arc sec. accuracy. At a wavelength of 2.55 A, this provides a resolution of 3 x 10 -6 A -1 in the scattering vector. This technique has been used to study the anisotropic behavior of the critical parameters B 0 and H/sub c1/, characteristic of the first-order magnetic phase transition which occurs in low-kappa type-II superconductors. Magnetic fields were applied parallel to several crystal axes of a large single-crystal sphere of pure niobium, resulting in well-defined flux-line lattices (FLL). Measurement of the FLL cell area in the intermediate mixed state field region gives the equilibrium flux density B 0 , which results from an attractive interaction between fluxoids. In addition, field variation of the scattered neutron intensity allows measurement of the transition field between the mixed state and intermediate mixed state. This transition field is related to the lower critical field H/sub c1/ and enables its determination to a precision 0.2%. Data at T = 4.3 K display a small anisotropic effect of about 2% in B 0 and 1% in H/sub c1/. Although orientation effects of this magnitude are difficult to resolve by bulk measurements, the neutron data are in accord with magnetization data. Observations regarding the temperature dependence of these parameters also will be presented, and comparisons made with current theoretical models

  18. Transformation Heat Treatment of Rapidly Quenched Nb3A1 Precursor Monitored in situ by High Energy Synchrotron Diffraction

    CERN Document Server

    Scheuerlein, C; Di Michiel, M; Jin, X; Takeuchi, T; Kikuchi, A; Tsuchiya, K; Nakagawa, K; Nakamoto, T

    2013-01-01

    Nb3Al superconductors are studied for use in high field magnets. Fine grained Nb3Al with nearly stoichiometric Al content is obtained by a Rapid Heating Quenching and Transformation (RHQT) process. We describe a non destructive in situ study of the transformation process step of a RHQ Nb3Al precursor wire with ramp rates of either 120 °C/h or 800 °C/h. High energy synchrotron x-ray diffraction measurements show the transformation from a Nb(Al)SS supersaturated solid solution into Nb3Al. When heating with a ramp rate of 120 °C/h a strong reduction of the Nb(Al)SS (110) diffraction peak component is observed when the temperature exceeds 660 °C. Additional diffraction peaks are detectable in the approximate temperature interval 610 °C - 750 °C and significant Nb3Al growth is observed above 730 °C.

  19. Measurement of the neutron lifetime using a magneto-gravitational trap and in situ detection.

    Science.gov (United States)

    Pattie, R W; Callahan, N B; Cude-Woods, C; Adamek, E R; Broussard, L J; Clayton, S M; Currie, S A; Dees, E B; Ding, X; Engel, E M; Fellers, D E; Fox, W; Geltenbort, P; Hickerson, K P; Hoffbauer, M A; Holley, A T; Komives, A; Liu, C-Y; MacDonald, S W T; Makela, M; Morris, C L; Ortiz, J D; Ramsey, J; Salvat, D J; Saunders, A; Seestrom, S J; Sharapov, E I; Sjue, S K; Tang, Z; Vanderwerp, J; Vogelaar, B; Walstrom, P L; Wang, Z; Wei, W; Weaver, H L; Wexler, J W; Womack, T L; Young, A R; Zeck, B A

    2018-05-11

    The precise value of the mean neutron lifetime, τ n , plays an important role in nuclear and particle physics and cosmology. It is used to predict the ratio of protons to helium atoms in the primordial universe and to search for physics beyond the Standard Model of particle physics. We eliminated loss mechanisms present in previous trap experiments by levitating polarized ultracold neutrons above the surface of an asymmetric storage trap using a repulsive magnetic field gradient so that the stored neutrons do not interact with material trap walls. As a result of this approach and the use of an in situ neutron detector, the lifetime reported here [877.7 ± 0.7 (stat) +0.4/-0.2 (sys) seconds] does not require corrections larger than the quoted uncertainties. Copyright © 2018 The Authors, some rights reserved; exclusive licensee American Association for the Advancement of Science. No claim to original U.S. Government Works.

  20. Structure solution from powder neutron and x-ray diffraction data: getting the best of both worlds

    International Nuclear Information System (INIS)

    Hunter, B.A.

    2000-01-01

    Full text: Powder diffraction methods have traditionally been used in three main areas: phase identification and quantification, lattice parameter determination and structure refinement. Until recently structure solution has been the almost exclusive domain of single crystal diffraction methods, predominantly using x-rays. The increasing use of synchrotron and neutron sources, and the unrelenting advances in computing hardware and software means that powder methods are challenging single crystal methods as a practical method for structure solution, especially when single crystal method can not be applied. It is known that structural refinements from a known starting structure using combined X-ray and neutron data sets are capable of providing highly accurate structures. Likewise, using combined x-ray and neutron powder diffraction data in the structure solution process should also be a powerful technique, although to date no one is pursuing this methodology. This paper present examples of solutions to the problem. Namely we are using high resolution powder X-ray and neutron methods to solve the structures of molecular materials and minerals, then refining the structures using both sets of data. In this way we exploit the advantages of both methods while minimising the disadvantages. We present our solution for a small amino acid structure, a metalorganic and a mineral structure